Cocour Lasegar - PRAJAB 3
Cocour Lasegar - PRAJAB 3
Cocour Lasegar - PRAJAB 3
Feb. 2009
Read the instruction manual thoroughly before you use the product.
Keep this instruction manual for future reference.
This page is intentionally left blank.
Introduction
Thank you for purchasing this product. This manual describes the operation, hardware validation, usage
cautions, accessories and options for this product. Read this manual thoroughly before using the product and
operate the product in accordance with the instructions in this manual.
IMPORTANT
• If the user or usage location changes, ensure that this Instruction Manual is always kept together with the
product.
• If this manual or a product warning label is lost or damaged, immediately contact your Shimadzu
representative to request a replacement.
• To ensure safe operation, read all Safety Instructions before using the product.
• To ensure safe operation, contact your Shimadzu representative if product installation, adjustment, or
re-installation (after the product is moved) is required.
Notice • Information in this manual is subject to change without notice and does not
represent a commitment on the part of the vendor.
• Any errors or omissions which may have occurred in this manual despite the
utmost care taken in its production will be corrected as soon as possible,
although not necessarily immediately after detection.
• All rights are reserved, including those to reproduce this manual or parts
thereof in any form without permission in writing from Shimadzu Corporation.
• Microsoft and Windows are registered trademarks of Microsoft Corporation in
the United States and/or other countries. Other company names and product
names mentioned in this manual are trademarks or registered trademarks of
their respective companies.
The TM and ® symbols are omitted in this manual.
AA-7000 i
Safety Instructions
• To ensure safe operation of the instrument, read these Safety Instructions carefully before use.
• Observe all of the WARNINGS and CAUTIONS described in this section. They are extremely important for
safety.
• In this manual, warnings and cautions are indicated using the following conventions;
Application Precautions
WARNING
This instrument is an atomic absorption spectrophotometer.
Use this instrument ONLY for the intended purpose.
Using this instrument for any other purpose could cause accidents.
WARNING
• This product is not an explosion-proof product.
It ignites and causes a fire.
Provide fire extinguishers for use in case of fire.
• Be sure to provide a duct made of metal for the expulsion of combustible gas above the atomic
absorption spectrophotometer.
If you use a duct made of plastic it will burn due to the heat of the flame.
• The weight of the body of the product is 72 kg. Take the weight of the entire analysis system into
account when installing the product.
Install this product on a desk or stand that can easily bear the weight of the entire analysis system and
is flat and stable.
If these conditions are not met, accidents in which the product topples over or falls may occur.
CAUTION
• Avoid installing the product in locations that are exposed to corrosive gases, organic solvents,
halogenated substances, gases containing polysiloxanes, oil mist, or a lot of dirt and dust.
This may make it impossible to maintain the product's performance or shorten the life of the instrument.
• Do NOT use the instrument in an environment where dew may condense on it.
This may prevent its normal operation.
ii AA-7000
Installation Precautions
WARNING
• To ensure safe operation, contact your Shimadzu representative if product installation,
adjustment, or re-installation (after the product is moved) is required.
• Take measures to prevent the instrument from falling in the event of an earthquake or other
disaster.
Strong vibrations could cause the instrument to fall over, resulting in injury.
• The power supply voltage of the instrument is indicated on the label on the right side of the
instrument. Connect the instrument only to a power supply of the voltage indicated;
otherwise, fire or electric shock could result. Check that the power supply voltage is stable and that its
current capacity is sufficient to operate all the components of the system. If not, the instrument will not
operate at its rated performance.
• Do NOT allow the grounding conductor of the adaptor to set in or contact the power outlet.
This could cause fire or electric shock.
• Do NOT place heavy objects on the power cord, and keep any hot items away.
The cord could be damaged, resulting in fire, electrical shock or malfunction. If the cord becomes
damaged, contact your Shimadzu representative immediately.
• Do NOT modify the cord in any way. Do NOT bend it excessively or pull on it.
The cord could be damaged, resulting in fire, electrical shock or malfunction. If the cord becomes
damaged, contact your Shimadzu representative immediately.
• Please insert the power cord in the power outlet at an easily accessible position.
The power cord must be unplugged from the power outlet in case of emergency.
CAUTION
• When installing the instrument, be careful not to pinch your fingers between the system
components, as this could result in injury.
• When opening the doors to the hollow cathode lamps, be careful not to pinch your fingers as
this could result in injury.
• Ground the PC and the optional device with equal potential grounds.
Otherwise communications between devices may be interrupted and equipment failures could occur.
AA-7000 iii
Precautions on Work and Operation
WARNING
• This instrument should be used only by personnel who have undergone special education and
training.
"Special education and training" indicates studies including the following contents:
1. Information relating to high-pressure gas and the handling of this unit
2. Information relating to high-pressure gas supply equipment
WARNING
• Do NOT use flammable sprays (hairspray, spray insecticides, etc.) near this product.
The spray could ignite and cause fire.
• When measuring an inflammable sample, take care about the handling of naked flame.
The material could ignite and cause fire.
Be sure to ventilate the room while using the instrument.
• Use the rubber hose supplied as a standard accessory with the product to supply gas.
Using any part other than this may cause accidents.
• At a frequency of once a month, implement the inspections described in 8.4 "Checking the Pilot
Flame Unit" and 8.5 "Checking for Gas Leaks".
If you do not, safety may be compromised.
• When using a nitrous oxide-acetylene flame, be sure to use the high-temperature burner head
(option).
CAUTION
• If you spill a liquid like water or an organic solvent on the instrument, wipe it off immediately.
It could cause equipment failure.
• Be sure to make a backup copy of the contents of the PC's hard disk.
Important data could be lost as the result of an unforeseen accident.
• The standard analysis conditions incorporated in the software are not the optimum conditions.
Optimize the analysis conditions for each element of each sample to be measured.
The analysis conditions may change according to the characteristics of the sample, the temperature,
humidity and other environmental conditions, replacement of maintenance parts and consumable parts,
and so on.
iv AA-7000
Precautions on Handling Gas
For details on the type and purity of gas to be used with this product, and the gas supply pressure, see 10.6.3
"Gas Requirements".
WARNING
• Do NOT use oxygen gas.
This could cause ignition or equipment failure.
• Install the gas cylinders in an airy location outdoors that is not exposed to direct sunlight. Feed
the high pressure gas indoors using piping.
• Take care that gas cylinders become no hotter than 40 °C, and do NOT allow any flame within
2 meters of the gas cylinders.
• With regard to the use of flammable gases (e.g. acetylene) and gases that increase the
susceptibility of substances to burn (e.g. nitrous oxide), smoking and the use of fire is
prohibited within 5 meters of the equipment that is using these gases. Install a fire extinguisher
to be prepared in the event of an accident.
• Secure gas cylinders with ropes or chains while they are standing up. Liquefied gas cylinders in
particular (acetylene, nitrous oxide, etc.) must never be allowed to fall to a horizontal position.
• Be sure to use oil-free pressure regulators. Also use ones that have no oil adhering to the inside
of the pipes, etc., where high-pressure gas comes into contact.
• Before mounting a pressure regulator on a gas cylinder, be sure to remove dust and other
material adhering to the cylinder's outlet. Dust remaining on the outlet may cause gas leakage.
• If the mounting screw for a cylinder's pressure regulator becomes damaged or thread-stripped,
do NOT attempt to mount the pressure regulator by force but replace the cylinder with a new
one. Mounting the regulator by force in this condition could cause gas leakage.
• Even if the main valve is stiff and difficult to open, do NOT strike the handle or main valve with a
hammer or spanner. This could cause gas leakage from the pressure regulator or cylinder outlet,
or failure of the pressure regulator.
• When using high pressure gas, make sure that there is sufficient ventilation. Carry out leak
inspections on the gas piping and pressure regulators at least once a month.
For details, see 8.5 "Checking for Gas Leaks" and 8.6 "Checking for Leaks of Pressure
Regulators (Optional)".
• Before opening a gas cylinder, check that the stop valve is closed. Turn the secondary pressure
adjusting valve fully to the left (counterclockwise), then open the cylinder using the handle for
that purpose.
• Close the cylinder's main valve immediately after you have finished using gas.
AA-7000 v
• Precautions on handling acetylene gas
Acetylene is a dangerous gas that explodes easily. When handling it, observe the following points in
addition to the "Precautions on Handling Gas" stated above.
• It has a wide range of combustion, and will burn when it is mixed with air in a ratio by volume of
2.5% or greater.
• Even when it is not mixed with air or oxygen, ignition energy can cause explosive
decomposition.
• Contact with copper (including alloys containing 62% or more copper), silver (including alloys),
gold (including alloys) or mercuric materials (including alloys) may trigger explosive
decomposition.
Acetylene gas is fed in to fill a container (cylinder) that incorporates a porous substance impregnated with
acetone, and supplied as dissolved acetylene.
WARNING
• When using acetylene gas, be sure to use a pressure regulator for acetylene gas.
If you use any other kind of regulator, gas will leak and may ignite.
• Do NOT use pipes made of copper (including alloys containing 62% or more copper), silver
(including alloys), gold (including alloys) or mercuric materials (including alloys) to convey
dissolved acetylene gas.
This will lead to the formation of metal acetylides, which could undergo explosive decomposition if
subjected to shock.
• When opening the main valve on a dissolved acetylene cylinder, turn it one turn or more but one
and a half full turn or less from the fully closed state.
If it is opened by less than one full turn, it will not be possible to supply sufficient acetylene gas when
using a nitrous oxide-acetylene flame with the high-temperature burner head (option), causing
flashback and failure of the instrument.
vi AA-7000
CAUTION
• Use dissolved acetylene cylinders that use acetone as the solvent.
Solvents other than acetone can cause the electromagnetic valves used with the unit to fail.
• When opening the main valve on a dissolved acetylene cylinder, turn it one turn or more but one
and a half full turn or less from the fully closed state.
If it is opened more than one and a half turns, the acetone that fills the cylinder will flow out and may
influence measurement.
• Do NOT use a dissolved acetylene cylinder with a primary pressure of less than 0.5 MPa.
The acetone that fills the cylinder will flow out and may influence measurement. When the primary
pressure of a gas cylinder has fallen to 0.5 MPa, exchange it for a new one.
• Do NOT use a cylinder with an acetylene pressure regulator at the secondary pressure of greater
than 0.127 MPa.
The acetone that fills the cylinder will flow out and may influence measurement.
WARNING
• Nitrous oxide gas has anesthetic characteristics.
Be sure to ventilate the room while you are using the instrument.
CAUTION
• Open the cylinder's main valve fully.
If it is not opened sufficiently, the flow rate of the gas may fluctuate during use and this may affect
measurement.
AA-7000 vii
• Precautions on handling of the air compressor (optional)
WARNING
• Handle the air compressor correctly by referring to the instruction manual that is supplied with
it.
Incorrect usage could lead to accidents. It could also lead to equipment failure.
CAUTION
• Provide a device like a drain separator part way along the piping from the air supply source for
dehumidification.
If you use air with a lot of moisture in it, the instrument may fail.
• Before using the air compressor, check the operation by referring to its instruction manual.
Using it without checking its operation first could cause equipment failure.
• When using an oil supply type compressor, check that the oil level always remains between the
red lines of the oil level gauge.
• After use, always open the drain cocks and discharge the water and oil inside the tank and the
transformer.
• When supplying air from an existing compressor or compressed air tubing, verify the following:
• That air is supplied at a pressure of 0.35 to 0.4 MPa
• That the pressure does not fluctuate
• That the air supplied does not contain water, oil, or dust
viii AA-7000
Measures for Preventing Static Electricity Accidents
WARNING
• Take thorough measures to prevent buildup of static electricity.
Static electricity could result in fire or explosion.
CAUTION
• The best way to prevent static electricity accidents is simply to prevent the occurrence and
accumulation of electro-static charges.
• It is important to combine multiple preventive measures.
• If large amounts of flammable solvents are collected in a large container, implement preventive
measures 1 to 5 below.
Preventive measure 1:
Use a metal container for the waste liquid which grounds the container. This will ensure that the electrical
charges of the container and liquids pass to the ground. Accessories for this measure:
• Be sure to ground the metal waste container properly. If the grounding wire is not properly
attached or connected to the ground, static electricity can build up in the metal container.
• Some metal containers have surfaces that are laminated or oxidized, and therefore do NOT
conduct electricity. After grounding the metal container, use a tester to make sure that electricity
is conducted to the ground.
• If the liquid to be drained into the waste liquid container is virtually non-conductive (10−10 S/m or
less), it will be necessary to add properly conductive (and therefore safe) liquid to the tank (this
conductive liquid may be added beforehand).
Preventive measure 2:
Cover the spaces between the tubing and the sides of the inlet and outlet openings of the waste container
(with caps or the like). This will prevent any sparks generated outside the container from getting inside.
Preventive measure 3:
Keep electro-statically charged objects, including the human body, away from the waste liquid container. To
prevent the electro-static charging of the human body, take the following precautions:
Preventive measure 4:
Use the tubing included in standard accessories for the drain line.
AA-7000 ix
Preventive measure 5:
If it is not possible to use a conductive waste liquid container, take the following precautions:
• Ensure that the end of the inflow tube is always submerged inside the container. Also, place
some type of grounded metal object (wire connected to the unit, etc.) in the liquid.
The above precautions will be ineffective for liquid of low conductivity (less than 10−10 S/m). For such liquid:
WARNING
• When handling chemicals, wear protective goggles and protective gloves.
If chemicals get into the eyes, there is a risk of loss of sight. If any chemical does get into the eyes,
wash it out immediately and consult a doctor.
• When handling a sample that is toxic or where there is a risk of biological infection, wear
protective gloves.
• When copper, silver, gold or mercury mixes with acetylene inside the chamber, deposits called
metal acetylides are formed. After measuring a sample that contains any of these metals,
periodically clean out the deposits from inside the chamber.
If metal acetylides are left inside the chamber, it will cause flashback due to a decomposition reaction.
x AA-7000
Precautions for Instrument Inspection, Maintenance, Adjustment and Care
WARNING
• Unplug the instrument before inspection, maintenance, or parts replacement.
Otherwise, electrical shock or short-circuit accidents could occur.
• If the power cord plug gets dusty, remove the plug from the power outlet and wipe away the dust
with a dry cloth.
If dust is allowed to accumulate, fire could result.
• Check that there is no cracking of the rubber hose for gas supply or deterioration due to
adhesion of chemicals, every time you use the instrument. If there is any cracking or
deterioration, replace the hose with a new one.
Note that cracking will cause gas leakage or fire.
• When replacing a part, use the part described in the instruction manual.
If you use any other part, that part may be damaged, meaning that it cannot be used normally.
• Do NOT attempt to perform any measurement other than those described in the instruction
manual.
CAUTION
• Do NOT leave this product wet with water, or wipe it over with alcohol or thinner based solvents.
This will cause rusting or discoloration.
• Deal with waste liquids appropriately in accordance with the regulations and directions of the
relevant authorities.
CAUTION
• Do NOT modify or disassemble the product without permission.
This can result in accidents due to electric shock or short circuits. It can also result in injuries and
equipment failure.
AA-7000 xi
Precautions on Use
In order to use the atomic absorption spectrophotometer safely, observe the following warnings and
precautions.
If you fail to observe them, the safety of the instrument may be compromised.
WARNING
• At ignition, do NOT put your face or hand inside the burner module (burner compartment). Do
NOT look in from above the burner compartment or hold your hand over it.
The nitrous oxide-acetylene flame reaches a height of 40 cm above the top face of the instrument. To
prevent accidents that might result from carelessness, always fit the chimney and close the flame shield
(chimney door) before ignition.
• Do NOT remove the nebulizer, drain tube or burner head during combustion.
• Do NOT touch the chimney or burner head for 30 minutes after the flame has been extinguished.
You could be burned.
• Do NOT touch the tip of the cleaning wire for the nebulizer capillary tube.
The wire may stick into your finger.
xii AA-7000
CAUTION
• Do NOT use the flame for any purpose other than analysis.
• When using the atomic absorption spectrophotometer in the flame method, do NOT remove the
chimney.
If you remove it, the heat of the flame will transfer inside the instrument and the reliability of the
measurement may be lost.
• Only open the chimney door when necessary, and do NOT leave it open during combustion.
If the door is left open, the nitrous oxide flame will shift backward and come into contact with the
chimney, and this will greatly speed up the rate of deterioration of the chimney.
• Do NOT use the standard burner head (10 cm slot burner) with the key for the high temperature
burner head (option) left in the key slot of the burner selection keyswitch (BURNER SELECT).
• Do NOT allow foreign material to get into the key slot of the burner selection keyswitch
(BURNER SELECT).
• Do NOT insert your fingers or hand into the holes of the lamp turret, igniter, flame monitor, etc.
AA-7000 xiii
Emergency Action
In an Emergency
Take the following actions in case of emergency or when an abnormality occurs in the atomic absorption
spectrophotometer.
Inspect the equipment before using it again and contact your Shimadzu representative if necessary.
• Emergency Action
1. Turn OFF the power switch of the atomic absorption spectrophotometer.
Even if measurement is in progress, the burner flame can be safely extinguished by turning the power
switch OFF.
2. Turn OFF all the power switches of accessories.
3. Close the main valves of the gas supply pipings for acetylene, air and nitrous oxide.
4. Close the main valve of the cooling water and argon supply piping.
5. Shut OFF the power supply.
• Turn OFF the switchboard when the power cable is fixed to the switchboard with screws.
• Disconnect the power cable when the power cable is connected with the plug.
Power cable
Power switch
xiv AA-7000
Measures in the Event of a Power Outage
When a power outage has occurred, take the following measures.
If the instrument does not start up, request your Shimadzu representative to inspect it.
If the instrument does not start up, request your Shimadzu representative to inspect it.
AA-7000 xv
Measures When Gas Leakage Is Detected
Execute [Start Leak Check] on the [Initialize] dialog box or select [Instrument] - [Gas Leak Check] from the
menu, and a gas leak inspection lasting approximately 8 minutes will be performed automatically.
WARNING
• If a gas leak is detected, stop using the instrument immediately.
The leaked gas could be ignited, causing fire.
If a gas leak is detected, the following message is displayed at the moment of detection.
If a gas leak is detected, stop using the instrument immediately and take the following measures.
If no gas leak is detected as the result of the gas leakage inspection, the following message is displayed after
the elapse of approximately 8 minutes, and from this point on it will be possible to ignite the flame.
NOTE
In the following cases the result of the gas leakage inspection is [NG] and it will not be possible to ignite the
flame.
• Gas was not being supplied at the start of the inspection.
• The inspection was stopped part way through.
xvi AA-7000
Measures When Flashback Occurs
The AA-7000 series instruments are equipped with a safety device to prevent flashback, but flashback may still
occur when using the flame method. If flashback occurs, stop using the instrument immediately and implement
the measures in the event of an emergency.
WARNING
• When flashback occurs, the burner head can be thrown 10 cm upward.
NOTE
If the instrument detects flashback, ignition will become impossible.
Before using the instrument again, request your Shimadzu representative to inspect it.
Once the representative has inspected the instrument and confirmed that there is no problem with it, he will
restore it to the condition in which ignition is possible.
AA-7000 xvii
Warning Labels on the Instrument
xviii AA-7000
Types of Corresponding Details of the
Position Where Affixed
Label Model Warning
(Part No.:
206-77429)
(Part No.:
206-77429)
AA-7000 xix
Warranty and After-Sales Service
1. Period: Please contact your Shimadzu representative for information about the period of this
warranty.
2. Description: If a product/part failure occurs for reasons attributable to Shimadzu during the warranty
period, Shimadzu will repair or replace the product/part free of charge. However, in the
case of products which are usually available on the market only for a short time, such as
personal computers and their peripherals/parts, Shimadzu may not be able to provide
identical replacement products.
3. Exceptions: Failures caused by the following are excluded from the warranty, even if they occur during
the warranty period.
1) Improper product handling
2) Repairs or modifications performed by parties other than Shimadzu or Shimadzu
designated companies
3) Product use in combination with hardware or software other than that designated by
Shimadzu
4) Computer viruses leading to device failures and damage to data and software,
including the product's basic software
5) Power failures, including power outages and sudden voltage drops, leading to device
failures and damage to data and software, including the product's basic software
6) Turning OFF the product without following the proper shutdown procedure leading to
device failures and damage to data and software, including the product's basic
software
7) Reasons unrelated to the product itself
8) Product use in harsh environments, such as those subject to high temperatures or
humidity levels, corrosive gases, or strong vibrations
9) Fires, earthquakes, or any other act of nature, contamination by radioactive or
hazardous substances, or any other force majeure event, including wars, riots, and
crimes
10) Product movement or transportation after installation
11) Consumable items
Note: Recording media such as floppy disks and CD-ROMs are considered
consumable items.
* If there is a document such as a warranty provided with the product, or there is a separate contract agreed
upon that includes warranty conditions, the provisions of those documents shall apply.
After-Sales Service
If any problem occurs with this instrument, inspect it and take appropriate corrective action as described in
this manual. If the problem persists, or symptoms not covered in this manual occur, contact your Shimadzu
representative.
xx AA-7000
Software License Agreement
1. LICENSE.
SMZ grants you a non-exclusive and nontransferable license to use the SOFTWARE subject to the
following terms and conditions.
2. LIMITATION OF USE.
Except as specifically authorized by SMZ, you may NOT:
a. Use the SOFTWARE, or permit the SOFTWARE to be used, on more than one PC at any one time.
b. Copy the SOFTWARE except one (1) archival copy of the SOFTWARE.
c. Modify, reverse engineer, decompile, disassemble, or create derivative works based upon the
SOFTWARE.
d. Transfer, rent, lease or grant any rights in the SOFTWARE in any form to anyone else.
4. UPGRADES.
You are entitled to receive all official software upgrades for the SOFTWARE that SMZ will release as
deemed necessary by SMZ. An upgrade means certain supplemental program modules and/or information
for bug fixing and/or updates to the defects and/or failures of the SOFTWARE that are acknowledged or
confirmed by SMZ. An upgrade excludes hardware, network, consulting services, third party products,
operation and general PC system maintenance. All supplemental program module for upgrades and
enhancements furnished to you shall be deemed to be part of the SOFTWARE and subject to the terms
and conditions set forth in this Agreement.
5. LIMITED WARRANTY.
SMZ warrants that for a period of one (1) year from the date of purchase, as evidenced by a copy of the
receipt, the media on which SOFTWARE is furnished will be free of defects in materials and workmanship
under normal use.
Except for the foregoing, SOFTWARE is provided AS IS. Your exclusive remedy and the entire liability of
SMZ and its suppliers under this limited warranty will be, at SMZ's option, repair, replacement, or refund of
the Software if reported (or, upon request, returned) to the party supplying the SOFTWARE to you. In no
event does SMZ warrant that the Software is error free or that you will be able to operate the SOFTWARE
without problems or interruptions.
EXCEPT AS SPECIFIED IN THIS WARRANTY, ALL EXPRESS OR IMPLIED CONDITIONS,
REPRESENTATIONS, AND WARRANTIES INCLUDING, WITHOUT LIMITATION, ANY IMPLIED
WARRANTY OF MERCHANTABILITY, FITNESS FOR A PARTICULAR PURPOSE,
NONINFRINGEMENT, ARISING FROM A COURSE OF DEALING, USAGE, OR TRADE PRACTICE,
ARE HEREBY EXCLUDED TO THE EXTENT ALLOWED BY APPLICABLE LAW.
AA-7000 xxi
6. LIMITATION OF LIABILITY.
IN NO EVENT WILL SMZ BE LIABLE FOR ANY LOST REVENUE, PROFIT OR DATA, OR FOR
SPECIAL, INDIRECT, CONSEQUENTIAL, INCIDENTIAL OR PUNITIVE DAMAGES, HOWEVER
CAUSED REGARDLESS OF THE THEORY OF LIABILITY, ARISING OUT OF OR RELATED TO THE
USE OF OR INABILITY TO USE SOFTWARE, EVEN IF SMZ HAS BEEN ADVISED OF THE
POSSIBILITY OF SUCH DAMAGE. IN NO EVENT WILL SMZ'S LIABILITY TO YOU, WHETHER IN
CONTRACT, TORT (INCLUDING NEGRIGENCE), OR OTHERWISE, EXCEED THE AMOUNT YOU
PAID FOR SOFTWARE.
7. TERMINATION.
This License is effective until terminated. You may terminate this License at any time by destroying all
copies of SOFTWARE including any documentation. This License will terminate immediately without notice
from SMZ if you fail to comply with any provision of this License. Upon termination, you must destroy all
copies of SOFTWARE.
8. GENERAL
a. This Agreement is the entire agreement. If any provision of this agreement is held invalid, the
remainder of this agreement shall continue in full force and effect.
b. This Agreement shall be construed and governed in accordance with the laws of Japan, excluding its
conflict of law rules.
c. The exclusive jurisdiction for any disputes arising out of or in connection with this Agreement shall be
Kyoto District Court of Japan.
d. The invalidity or unenforceability of any provision of this Agreement shall not affect the validity or
enforceability of any other provision.
xxii AA-7000
Handling Waste Liquid
WARNING
• Do NOT use a container made of glass as the waste liquid tank.
In the event of a flashback there is a risk that glass fragments will be scattered.
• Select a waste liquid container made of material that is resistant to the chemicals used.
If you use a container with no chemical resistance, waste liquid will leak and may cause burns or fire.
Waste liquid discharged during measurement or pretreatment should be handled in different ways in
accordance with the solute and solvent contained in that waste liquid. The way of handling waste liquid is
different depending upon the country or region.
Be sure to dispose of waste liquid according to the location of use.
When handling waste liquids, wear protective gloves and safety goggles.
Disposal Precautions
Disposal of lamps
The raw materials used in hollow cathode lamps are metal (the lamp element), quartz glass and plastic. Some
lamps also contain harmful metals (mercury, arsenic, berylium, selenium, etc.) or metals that ignite on contact
with water (calcium, lithium, sodium). Carefully read the notes that accompany the hollow cathode lamp, and, if
any of these metals is contained, ask an industrial waste disposer officially licensed for hazardous waste
disposal.
AA-7000 xxiii
Action for Environment (WEEE)
Contact Shimadzu service representative when the equipment has reached the end of
its life. They will advise you regarding the equipment take-back.
WEEE Mark
With your co-operation we are aiming to reduce contamination from waste electronic and electrical equipment
and preserve natural resource through re-use and recycling.
Do not hesitate to ask Shimadzu service representative, if you require further information.
Regulatory Information
For Europe:
The product complies with the following requirements.
xxiv AA-7000
Electromagnetic Compatibility
WARNING
• Graphite furnace atomizer GFA-7000 is a class A product, designed not for use in residential
environment.
Graphite furnace atomizer GFA-7000, an optional accessory for AA-7000 series, is a class A for
electromagnetic interference (emission).
NOTE
When an electromagnetic disturbance occurs to the instruments being used close to this product, take the
following measures:
• Take an appropriate distance among the instruments and this product in order to eliminate the
disturbance.
• Supply power from a different power source.
AA-7000 xxv
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xxvi AA-7000
Contents
Chapter 1 Overview
1.1 Overview of AA-7000 Series.................................................................................................. 1-2
1.2 Parts Information ................................................................................................................... 1-3
1.2.1 AA-7000F Parts Information ...................................................................................... 1-3
1.2.2 AA-7000G Parts Information ...................................................................................... 1-4
1.3 Installation.............................................................................................................................. 1-5
1.3.1 Installation of AA-7000 Series.................................................................................... 1-5
1.3.2 Installation of PC Software......................................................................................... 1-5
1.4 Name and Function of Each Part........................................................................................... 1-6
1.4.1 Operation Switches/Connectors ................................................................................ 1-6
1.4.2 Burner Compartment ................................................................................................. 1-7
1.4.3 Burner ........................................................................................................................ 1-9
1.4.4 Hollow Cathode Lamp Turret ................................................................................... 1-10
1.4.5 Deuterium Lamp ...................................................................................................... 1-12
1.4.6 Support Gas Flow Meter (When Option Equipped) ................................................. 1-13
1.4.7 Optical System ......................................................................................................... 1-14
1.4.8 Photometric System ................................................................................................. 1-15
1.4.9 Analog Output .......................................................................................................... 1-17
1.4.10 [WizAArd] Launcher ................................................................................................. 1-18
1.4.11 Safety Devices ......................................................................................................... 1-19
AA-7000 xxvii
3.1.7 Optics Parameters ................................................................................................... 3-22
3.1.8 Atomizer/Gas Flow Rate Setup................................................................................ 3-24
3.2 Software Basic Operation (Flame Micro Sampling Method) ................................................ 3-27
3.2.1 Operation Flowchart (Flame Micro Sampling Method)............................................. 3-27
3.2.2 Logging in WizAArd.................................................................................................. 3-27
3.2.3 Wizard Selection ...................................................................................................... 3-28
3.2.4 Element Selection .................................................................................................... 3-29
3.2.4.1 Lamp Setting Procedure ........................................................................... 3-31
3.2.5 Preparation Parameters ........................................................................................... 3-33
3.2.5.1 Calibration Curve Setup ............................................................................ 3-34
3.2.5.2 Sample Group Setup................................................................................. 3-38
3.2.6 Connect to Instrument/Send Parameters................................................................. 3-41
3.2.6.1 Initializing the Instrument .......................................................................... 3-42
3.2.6.2 Instrument Check List for Flame Analysis................................................. 3-48
3.2.7 Optics Parameters ................................................................................................... 3-49
3.2.8 Atomizer/Gas Flow Rate Setup................................................................................ 3-51
3.3 Software Basic Operation (Furnace Method)....................................................................... 3-54
3.3.1 Operation Flowchart (Furnace Method) ................................................................... 3-54
3.3.2 Logging in WizAArd.................................................................................................. 3-54
3.3.3 Wizard Selection ...................................................................................................... 3-55
3.3.4 Element Selection .................................................................................................... 3-56
3.3.4.1 Lamp Setting Procedure ........................................................................... 3-58
3.3.5 Preparation Parameters ........................................................................................... 3-60
3.3.5.1 Calibration Curve Setup ............................................................................ 3-61
3.3.5.2 Sample Group Setup................................................................................. 3-66
3.3.6 Connect to [Instrument/Send Parameters] Page ..................................................... 3-69
3.3.6.1 Initializing the Instrument .......................................................................... 3-70
3.3.6.2 Bypass the Instrument Check List for Flame Analysis .............................. 3-71
3.3.7 Optics Parameters ................................................................................................... 3-72
3.3.8 Furnace Program ..................................................................................................... 3-74
3.3.8.1 Furnace Program Setup............................................................................ 3-75
3.4 Saving the Template ............................................................................................................ 3-77
3.5 Explanation of Main Window................................................................................................ 3-78
3.5.1 Menu Bar.................................................................................................................. 3-79
3.5.2 Standard Tool Bar .................................................................................................... 3-79
3.5.3 Measurement Element Tool Bar .............................................................................. 3-80
3.5.4 Absorbance Digital Display ...................................................................................... 3-80
3.5.5 Real Time Graph (and Furnace Program Graph) .................................................... 3-81
3.5.6 Peak Profile (Latest Four Measurements and Overlay Display) .............................. 3-83
3.5.7 Calibration Curve Display......................................................................................... 3-85
3.5.8 MRT Work Sheet...................................................................................................... 3-87
3.5.9 Function Buttons ...................................................................................................... 3-88
3.5.10 Status Bar ................................................................................................................ 3-89
3.6 Operating the MRT Work Sheet........................................................................................... 3-90
3.6.1 Fields of MRT Work Sheet ....................................................................................... 3-90
3.6.1.1 Drop-down List of [Action] ......................................................................... 3-93
3.6.2 Right Mouse Button Menu........................................................................................ 3-95
3.6.3 Right Mouse Button on Summary Table .................................................................. 3-99
3.6.4 Inserting and Deleting the Measurement Row ......................................................... 3-99
3.6.5 Active Cell Movement by Shortcut Key and Cell Selection ...................................... 3-99
3.6.5.1 Moving an Active Cell................................................................................ 3-99
3.6.5.2 Selecting Cells ........................................................................................ 3-100
xxviii AA-7000
3.6.6 Copy and Paste ..................................................................................................... 3-100
3.6.6.1 Copy........................................................................................................ 3-100
3.6.6.2 Paste....................................................................................................... 3-100
3.6.7 Changing Column Width and Column Header Height of MRT Worksheet ............ 3-101
AA-7000 xxix
5.2.5 Short Time after System Operation Has Been Started ............................................ 5-20
5.2.5.1 Viewing the History of System Administration........................................... 5-20
5.2.5.2 Changing Passwords ................................................................................ 5-21
5.3 Using the Security Support Functions.................................................................................. 5-23
5.3.1 Login Authentication................................................................................................. 5-23
5.3.2 Current User Display................................................................................................ 5-24
5.3.3 Restricting the Operations according to User Rights ............................................... 5-24
5.3.4 Protecting an Analytical Task by Locking the Screen .............................................. 5-25
5.4 Audit Trail............................................................................................................................. 5-26
5.4.1 Referencing a Record in a Data File ........................................................................ 5-27
5.4.2 Viewing the History of System Changes .................................................................. 5-27
5.5 Performing Software Validation ........................................................................................... 5-29
5.5.1 Performing Program Checks.................................................................................... 5-29
5.5.2 Performing the Function Check................................................................................ 5-31
5.6 Data Administration.............................................................................................................. 5-32
5.6.1 Reviewing the Long-Term Storage of Data.............................................................. 5-32
5.6.1.1 Managing the Print Images ....................................................................... 5-32
5.6.1.2 Storing a Data File for a Long Period of Time........................................... 5-32
5.6.1.3 Devising a Data Storage Method .............................................................. 5-33
5.6.1.4 Using a Print Image................................................................................... 5-33
5.7 Other System Management Tools ....................................................................................... 5-34
5.7.1 Performing the Maintenance of System Management Database............................. 5-34
5.7.1.1 Using the Database Maintenance Tool ..................................................... 5-34
5.7.2 Managing the System on the Network ..................................................................... 5-35
5.7.2.1 Using Shimadzu User Authentication Tool on the Network ...................... 5-35
5.7.2.2 Using the Maintenance of Instrument Information Tool ............................ 5-36
xxx AA-7000
7.3.7 Absorbance and Repeatability (In the Case of Furnace Analysis)............................. 7-6
7.3.8 Detection Limit (In the Case of Furnace Analysis) ..................................................... 7-6
7.4 Basic Operation Procedures .................................................................................................. 7-7
7.4.1 Preparation ................................................................................................................ 7-7
7.4.1.1 Preparation of Hollow Cathode Lamp ......................................................... 7-7
7.4.1.2 Sample Preparation .................................................................................... 7-7
7.4.2 Selecting the Test Items ............................................................................................ 7-8
7.4.3 Setting the ASC Parameters .................................................................................... 7-11
7.4.4 Setting the Warm-up Time of Lamps and Stabilization Time for Flame................... 7-12
7.4.5 Starting the Test....................................................................................................... 7-13
7.4.6 Items with Sample Measurement............................................................................. 7-15
7.4.7 Stop the Test............................................................................................................ 7-16
7.4.8 Print the Check Result ............................................................................................. 7-17
7.4.9 Saving and Loading the Data................................................................................... 7-18
7.4.9.1 Saving the Data ........................................................................................ 7-18
7.4.9.2 Loading the Data....................................................................................... 7-18
7.5 Parameter Change .............................................................................................................. 7-19
7.5.1 Entering the Parameter Change Screen .................................................................. 7-19
7.5.2 Setting the Test Parameters .................................................................................... 7-20
7.5.3 Setting the Scale for Graph Display/Output of Each Data ....................................... 7-22
7.5.4 Saving/Loading the Parameters............................................................................... 7-23
7.5.4.1 When Saved as the Individual Validation File........................................... 7-23
7.5.4.2 Loading the Individual Validation File ....................................................... 7-23
7.5.4.3 When Saved as the Auto Load Validation File.......................................... 7-24
7.6 Functions of Operation Menu .............................................................................................. 7-25
7.6.1 Main Screen ............................................................................................................. 7-25
7.6.2 File ........................................................................................................................... 7-26
7.6.2.1 [Print Setup] Dialog Box............................................................................ 7-27
7.6.3 Tests ........................................................................................................................ 7-28
7.6.4 Configuration............................................................................................................ 7-28
7.6.5 Perform .................................................................................................................... 7-29
7.6.6 Graph ....................................................................................................................... 7-29
Chapter 8 Maintenance
8.1 Routine Inspections and Periodic Inspections ....................................................................... 8-2
8.1.1 Routine Inspections ................................................................................................... 8-2
8.1.1.1 Common to All AA-7000 Series Models...................................................... 8-2
8.1.1.2 AA-7000F.................................................................................................... 8-2
8.1.2 Monthly Inspection ..................................................................................................... 8-3
8.1.2.1 Common to All AA-7000 Series Models...................................................... 8-3
8.1.2.2 AA-7000F.................................................................................................... 8-3
8.1.2.3 Equipment and Options .............................................................................. 8-4
8.2 Burner Maintenance (AA-7000F) ........................................................................................... 8-5
8.2.1 Burner Head Maintenance ......................................................................................... 8-6
8.2.2 Nebulizer Maintenance .............................................................................................. 8-7
8.2.2.1 Removing and Mounting the Sampling Tube.............................................. 8-8
8.2.2.2 Removing and Mounting the Shield Cover ................................................. 8-8
8.2.2.3 Cleaning the Capillary................................................................................. 8-8
8.2.2.4 Inspecting and Replacing the Polyethylene Tube....................................... 8-9
8.2.2.5 Inspecting and Cleaning the Tip of the Spray Unit...................................... 8-9
8.2.2.6 Cleaning the Disperser ............................................................................. 8-10
AA-7000 xxxi
8.2.3Chamber Maintenance............................................................................................. 8-11
8.2.3.1 Cleaning the Chamber .............................................................................. 8-11
8.2.3.2 Replacing O-rings ..................................................................................... 8-12
8.2.3.3 Cleaning the Drain Tank and U-Tube ....................................................... 8-13
8.3 Atomizer Positioning Adjustment ......................................................................................... 8-16
8.3.1 Burner Positioning Adjustment................................................................................. 8-16
8.3.1.1 AA-7000F .................................................................................................. 8-16
8.3.1.2 AA-7000F (When Equipped with AAC-7000) ............................................ 8-16
8.3.2 Furnace Position Adjustment ................................................................................... 8-18
8.3.2.1 AA-7000G ................................................................................................. 8-18
8.3.2.2 AA-7000F (When Equipped with AAC-7000) ............................................ 8-18
8.4 Checking the Pilot Flame Unit.............................................................................................. 8-19
8.4.1 Inspection Procedure ............................................................................................... 8-19
8.5 Checking for Gas Leaks....................................................................................................... 8-20
8.6 Checking for Leaks of Pressure Regulators (Optional)........................................................ 8-21
8.7 Replacing the Drain Tube .................................................................................................... 8-23
8.8 Replacing the Deuterium Lamp ........................................................................................... 8-24
8.8.1 Specifications of Deuterium Lamp ........................................................................... 8-24
8.8.2 Replacing Procedures of Deuterium Lamp .............................................................. 8-24
8.8.2.1 Replacing Deuterium Lamp....................................................................... 8-25
8.8.2.2 Adjusting Position of Deuterium Lamp ...................................................... 8-27
8.9 Method for Replacing the Hollow Cathode Lamp ................................................................ 8-28
8.10 Maintenance Parts ............................................................................................................... 8-32
8.10.1 Parts Relating to Safety of Product .......................................................................... 8-32
8.10.2 Parts Relating to Performance of Product................................................................ 8-32
8.11 Repair Parts ......................................................................................................................... 8-33
Chapter 9 Troubleshooting
9.1 Failure to Ignite ...................................................................................................................... 9-2
9.2 Responding to Trouble........................................................................................................... 9-3
9.2.1 Common to All AA-7000 Series Instruments.............................................................. 9-3
9.2.2 AA-7000F ................................................................................................................... 9-6
9.3 When the Buzzer Sounds ...................................................................................................... 9-8
9.3.1 When the Buzzer Sounds Continuously (beep, beep) ............................................... 9-8
9.3.2 When the Buzzer Sounds Continuously (pippip, pippip) ............................................ 9-9
9.3.3 When the Buzzer Sounds Four Times (beep, beep, beep, beep).............................. 9-9
9.4 Error Messages.................................................................................................................... 9-12
xxxii AA-7000
10.4.3 Autosampler........................................................................................................... 10-13
10.4.4 Dual Atomizer System ........................................................................................... 10-13
10.4.5 Hollow Cathode Lamps (Single Element Lamps) .................................................. 10-14
10.4.6 Hollow Cathode Lamps (Single Element Lamps, Usable for SR Method) ............. 10-16
10.4.7 Hollow Cathode Lamp (Multi-Element Lamps) ...................................................... 10-17
10.4.8 Other Parts............................................................................................................. 10-18
10.5 Instrument Placement and Site Requirements .................................................................. 10-19
10.6 Equipment Requirements .................................................................................................. 10-21
10.6.1 Power Requirements ............................................................................................. 10-21
10.6.2 Cooling Water Supply Requirement (GFA Only) ................................................... 10-21
10.6.3 Gas Requirements ................................................................................................. 10-22
10.6.4 Ventilation System ................................................................................................. 10-25
AA-7000 xxxiii
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xxxiv AA-7000
Chapter 1
Overview
CONTENTS
AA-7000 1-1
Chapter 1 Overview
1.1 Overview of AA-7000 Series
The Atomic Absorption Spectrophotometer AA-7000 series incorporates two background correction functions,
the D2 method (Deuterium Lamp method) and the SR method (High-Speed Self-Reversal method), enabling
selection of the appropriate method for the measurement sample.
• The AA-7000 series instruments support the following three measurement modes.
Flame Continuous Method
Flame Micro Sampling Method
Furnace Method (Electrothermal Method)
• Instrument configurations
AA-7000F: Flame unit (can be extended for furnace analysis)
AA-7000G: Furnace unit
The AA-7000F, equipped with the Auto Atomizer Changer AAC-7000 (optional), allows you to change the
measurement mode while automatically setting the proper atomizer for the changed measurement mode on the
optical axis. It also enables quick and easy switching back and forth between flame measurement and furnace
measurement. In addition, wide ranging measurement operations are available, from manual operation to
automatic continuous measurement of multi-elements with the use of an autosampler. This enables selection of
the appropriate combination to match the number of elements and samples to be analyzed as well as the skill of
the operator.
The PC software controlling the AA-7000 series operates on Windows Vista Business / XP Professional, and
using the Wizard for parameter setting enables an operator, even a beginner with the atomic absorption
spectrophotometer, to make measurement conditions easily. In addition, a hardware validation function is
available as standard to allow you to check the performance of the AA-7000 series. This function is applicable
to system suitability management for IQ/OQ or the like.
1-2 AA-7000
1.2 Parts Information
1.2 Parts Information
This instrument consists of the standard parts listed below. Check the parts against this list after unpacking.
2 Accessories 1 206-77534-xx
AA-7000 1-3
Chapter 1 Overview
2 Accessories 1 206-77535-xx
1-4 AA-7000
1.3 Installation
1.3 Installation
AA-7000 1-5
Chapter 1 Overview
1.4 Name and Function of Each Part
4
5
6
7
8
9
0
a@
3 1
2
Fig. 1.1 AA-7000 Series Main Unit
3 BURNER SELECT switch This key switch is for preventing mistaken use of burner heads. When
the high temperature burner head (optional) is to be used with the
nitrous oxide-acetylene flame, a key attached to the burner head is
used to change to the N2O-C2H2 position. If not in this position, the
nitrous oxide flame cannot be ignited.
4 PURGE button When this button is pressed independently, the solenoid valve is
opened to send support gas (air or N2O). When this button and the
IGNITE button are pressed simultaneously, flame is ignited.
5 IGNITE button When this button is pressed independently, nothing happens. When this
button and the PURGE button are pressed simultaneously, gas is fed to
the burner and then flame is ignited with the pilot flame.
0 ANALOG OUT This is the analog voltage output terminal. Connect a pen recorder or
other device here.
a AC power supply (~) inlet Connect the cable set to supply AC power here.
1-6 AA-7000
1.4 Name and Function of Each Part
2 5
6
9
0
7
1 Atomizer position indicator The scale indicates the height of the atomizer.
scale
2 forward/backward When the knob is turned clockwise, the atomizer moves forward.
adjusting knob When the knob is turned counterclockwise, the atomizer moves
backward. (1 mm per rotation)
3 upward/downward When the knob is turned clockwise, the atomizer moves downward.
adjusting knob When the knob is turned counterclockwise, the atomizer moves
upward. (2 mm per rotation)
4 Front panel The front panel serves to stabilize the combustion of the flame. Remove
it when carrying out inspection and maintenance.
For details, see 2.4 "Removing and Mounting the Front Panel".
AA-7000 1-7
Chapter 1 Overview
6 Flame shield The whole of the front of the chimney 5 slides upward.
(chimney door) * Open this door when maintenance of the atomizer is necessary.
7 Burner head * The flame available for the burner head provided as standard is air-
acetylene flame. Be sure to use the high temperature burner head
(optional) when using a nitrous oxide-acetylene flame.
8 Burner head angle This allows the angle of burner slot to be adjusted relative to the light
adjustment lever * path. When measuring high-concentration samples, measurements of
better linearity between concentration and absorbance can be obtained
by angling the slot to decrease sensitivity.
9 Flame monitor * An optical sensor is built in the instrument for monitoring the intensity of
the light emitted by the flame. If the flame goes out and the light
emission is lost, the solenoid valve in the gas control unit is closed by a
signal from the sensor and the flow of raw gas is stopped. In addition,
when switching between an air-acetylene flame and nitrous oxide-
acetylene flame, an increase in the acetylene flow rate will be detected
by an increase in the light emission intensity, and the air and nitrous
oxide will be switched.
0 Pilot flame * When the IGNITE and PURGE buttons located on the front of the
AA-7000 series are pressed simultaneously, the pilot flame is ignited.
NOTE
When the instrument is equipped with AAC-7000 (optional), the atomizer (burner and graphite furnace) is
driven by PC operation. Therefore, there are no positioning knobs for driving the burner module.
1-8 AA-7000
1.4 Name and Function of Each Part
1.4.3 Burner
WARNING
In the event of a flashback, the mixer plays the role of absorbing the shock. Before igniting the flame, check
that the mixer is correctly installed inside the chamber.
If it is damaged or deformed, it must be replaced.
If there is a flashback, it could cause a gas leak that will damage the chamber.
The AA-7000F has a burner head with a 10 cm length slot (standard) mounted in the premixing atomizer
chamber. This burner head can be used with air-acetylene flames. Please specially install a 5 cm high-
temperature head (optional) when using a nitrous oxide-acetylene flame.
3
2
5 4
6 7
AA-7000 1-9
Chapter 1 Overview
NOTE
When an AAC-7000 (optional) and a GFA-7000 (optional) are provided at the same time, adjustment of the
burner head angle is no longer possible.
WARNING
• Do NOT touch the terminals of the lamp sockets while the power is on.
Be sure to turn the lamp OFF before removal or fitting.
If it is not OFF there will be a risk of electric shock.
Six hollow cathode lamps (optional) can be installed in the Lamp Turret, and two of them can be on at one time.
For routine analysis in which the analysis elements are known, it is convenient if all the lamps to be used in
measurement (up to six) are installed in the turret and the lamp current values, lamp numbers (socket numbers)
along with the other measurement parameters are stored beforehand in the instrument memory. This allows the
required lamp to be automatically set in the optical path by just loading the stored parameters.
CAUTION
• To install the lamp, be sure to insert it until it reaches the bottom of the socket, and then secure
it with the lamp securing ring.
If the lamp is not fully inserted, it is not properly positioned and this can cause a failure in lighting the
lamp.
NOTE
Do NOT touch the window section of the lamp with bare hands.
Soiling such as finger grease will adhere to the window and diminish the strength of the lamp, affecting
performance.
1-10 AA-7000
1.4 Name and Function of Each Part
Cap
Window
Securing ring
Lock screw
AA-7000 1-11
Chapter 1 Overview
Adjusting screw
Deuterium lamp
Lamp base
1-12 AA-7000
1.4 Name and Function of Each Part
NOTE
• The flow rate setting ranges for support gas are as follows.
Air: 13.5 to 17.5 L/min
Nitrous oxide: 10.0 to 12.5 L/min
• AA-7000G cannot be equipped with the flow meter kit.
AA-7000 1-13
Chapter 1 Overview
PMT
S2
M G M
S1
D2
CM
M M
M
BS
HCL
1-14 AA-7000
1.4 Name and Function of Each Part
Deuterium
lamp
Analog
circuit
Monochrometer Reference
Chopper mirror
Beam splitter
CPU
PC
Gas controller unit
The following four measurement modes can be selected in the AA-7000 series.
EMISSION Used for flame emission analysis.
mode
NON-BGC Used for atomic absorption analysis that doesn't require background correction.
mode
BGC-D2 mode only available in a wavelength range between 185 and 430 nm.
BGC-SR mode Available at any wavelength. Effective for compensating spectral interference
resulting from nearby lines.
AA-7000 1-15
Chapter 1 Overview
1-16 AA-7000
1.4 Name and Function of Each Part
Item Specification
Output range 5.0, 2.5, 1.25, 0.625 Abs./1 V (4-step switching for each)
In the EMISSION mode, fixed at 1 V F.S
For details on the output cables that are suited to these terminals (optional), see 10.4.8 "Other Parts" under
10.4 "Optional Parts".
AA-7000 1-17
Chapter 1 Overview
NOTE
2
3
NOTE
[Agent Connection Setting] in the [Administration] menu becomes operational when CLASS-Public Agent
(optional) is installed.
1-18 AA-7000
1.4 Name and Function of Each Part
Name Function
Vibration sensor Monitors the vibration imparted to the instrument.
Fan stop sensor Monitors the operation status of the fan in the back of the instrument.
Drain level sensor* Monitors the level in the drain tank.
Support gas pressure monitor* Monitors the supply pressure of support gas (air or nitrous oxide) being
supplied to the instrument.
Fuel gas pressure monitor* Monitors the supply pressure of fuel gas (acetylene) being supplied to the
instrument. During a gas leak inspection, it detects whether the pressure
drop is within the permissible range to judge whether there is a gas leak.
Flame monitor Monitors the luminous strength of the flame.
For details, see 1.4.2 "Burner Compartment" No. 9.
Flashback monitor device* Monitors flashback occurrence. If flashback occurs, implement the
"Measures When Flashback Occurs".
NOTE
1. When a safety device is actuated, the following message is displayed.
2. The status of all the safety devices except the flame monitor can be checked in the [Gas Controller
Status] dialog box.
For details, see 2.7 "Checking the Gas Controller Status (AA-7000F)".
3. When a safety device is actuated, a message is displayed on the screen and the buzzer sounds.
For details, see 9.3 "When the Buzzer Sounds".
AA-7000 1-19
Chapter 1 Overview
1-20 AA-7000
Chapter 2
Basic Operation
CONTENTS
AA-7000 2-1
Chapter 2 Basic Operation
2.1 Power ON/OFF
2.1.1 Activation
(1) When using the Autosampler ASC-7000 or Graphite Furnace Atomizer GFA-7000, set the ASC-7000
power switch or the GFA-7000 power switch to the ON position (" | " position).
ASC-7000
power switch
Power switch
(2) Set the power switch of AA-7000 main unit to the ON position ( " | " position).
Power switch
NOTE
When the power to the instrument is turned on, the buzzer sounds once (pip). Following the buzzer, a self-
diagnosis session starts. When it is completed successfully, the buzzer sounds three times (pip, pip, pip).
2-2 AA-7000
2.1 Power ON/OFF
(3) Maintain the circuit protector on the GFA-7000 in the OFF position, and turn it ON when preparing for
starting the measurement of the furnace.
Power switch
Circuit protector
(6) Select [Operation] in the [WizAArd] launcher, and click the AA-7000 main unit icon.
The WizAArd software for controlling the AA main unit is started up, and the [WizAArd Login] dialog box
(Fig. 3.2) will appear at the center of the screen.
When you log into the wizard, the [Wizard Selection] dialog box (Fig. 3.3) appears.
After the WizAAd software is started up, simply follow the messages displayed on the screen to complete
the settings necessary for measurement (wizard function).
AA-7000 2-3
Chapter 2 Basic Operation
2.1.2 Quitting
(1) Confirm that all necessary WizAArd data has been saved.
(2) Quit WizAArd with the [File] - [Exit] command.
(3) On quitting, shut off all main valves.
When using the GFA-7000, shut off the main valve for the cooling water too.
NOTE
When the ASC-7000 and/or GFA-7000 are used, turn off their respective power switches.
CAUTION
Never turn off the power to the PC or press the PC reset switch while Windows is running.
This may cause Windows to fail to boot afterward.
2-4 AA-7000
2.2 Initialization of the Instrument
2.2 Initialization of the Instrument
This is the procedure for connecting from WizAArd to the AA-7000 main unit and performing initialization.
(1) Check that there is nothing that will obstruct the light path in the burner compartment in the AA-7000 main
unit.
NOTE
If there is anything that will block the light path in the burner compartment, such as a card (accessory), an
NG (fail) result will be recorded for the "wavelength origin detection" inspection during initialization.
NOTE
If as a result of initialization " No Test (Not Connected)" is indicated for the ASC connection or GFA
connection, check that the ASC-7000 or GFA-7000 power switch is ON. If the ASC connection or GFA
connection is indicated as not connected despite the fact that the relevant power switch is ON, or if another
item is flagged up as NG, stop using the instrument and contact your Shimadzu representative.
(4) When using the flame method, the [Instrument Check List for Flame Analysis] screen is displayed.
When using the furnace method, a screen on which you can select whether or not to implement the check
list for the flame analysis is displayed.
For details, see the following sections:
• Flame continuous method: 3.1.6.2 "Instrument Check List for Flame Analysis"
• Flame micro sampling method: 3.2.6.2 "Instrument Check List for Flame Analysis"
• Furnace method: 3.3.6.2 "Bypass the Instrument Check List for Flame Analysis"
AA-7000 2-5
Chapter 2 Basic Operation
2.3 Mounting a Hollow Cathode Lamp (Optional)
WARNING
• Do NOT touch the terminals of the lamp sockets while the power is on.
Be sure to turn the lamp OFF before removal or fitting.
If it is not OFF there will be a risk of electric shock.
CAUTION
• To install the lamp, be sure to insert it until it reaches the bottom of the socket, and then secure
it with the lamp securing ring.
If the lamp is not fully inserted, it is not properly positioned and this can cause a failure in lighting the
lamp.
NOTE
Do NOT touch the window section of the lamp with bare hands.
Soiling such as finger grease will adhere to the window and diminish the strength of the lamp, affecting
performance.
(1) Open the cover on the right side of the main unit.
(2) Remove the cap from the socket where the lamp is installed.
(3) Remove the lamp securing ring from the lamp lock screw.
(4) Insert the hollow cathode lamp into the lamp socket.
(5) Pass the lamp through the lamp securing ring and then firmly tighten it to the lamp lock screw.
2-6 AA-7000
2.3 Mounting a Hollow Cathode Lamp (Optional)
Cap
Window
Securing ring
Lock screw
AA-7000 2-7
Chapter 2 Basic Operation
2.4 Removing and Mounting the Front Panel
WARNING
• Wait at least 30 minutes after the flame has been extinguished before starting maintenance
inside the burner compartment.
Otherwise you risk burns.
(2) While supporting the door that has been slid upward with your hand, pull the upper part of the front panel
out toward you.
The front panel stops when it has tilted about 15 mm toward you.
About 15 mm
2-8 AA-7000
2.4 Removing and Mounting the Front Panel
(3) In this state, pull the front panel approximately 10 mm upward and toward you.
10 mm
AA-7000 2-9
Chapter 2 Basic Operation
(2) While supporting the door that has been slid upward with your hand, insert the lower part of the front panel
into the two catches at the bottom of the front face of the instrument.
(3) Using the bottom of the front panel as the fulcrum, push in the top part of the panel.
2-10 AA-7000
2.5 Removing and Mounting the Chimney (AA-7000F)
2.5 Removing and Mounting the Chimney
(AA-7000F)
WARNING
• Wait at least 30 minutes after the flame has been extinguished before starting maintenance
inside the burner compartment.
Otherwise you risk burns.
AA-7000 2-11
Chapter 2 Basic Operation
(2) Place the chimney on the body of the instrument so that the two pins will coincide with the two holes, as
shown in the figure below.
2-12 AA-7000
2.6 Using "Help"
2.6 Using "Help"
Details of each of the screens in the software are given in the help information. This section explains how to
refer to the help information.
NOTE
There is no help information for [Hardware Validation] and [Program Check] in the validation menu.
For explanations of each of the screens, see Chapter 7 "Hardware Validation" and 5.5 "Performing Software
Validation".
WizAArd software
Click [Search for Help on] in the [Help] menu.
NOTE
To start up the WizAArd, select [Operation] from the [WizAArd] launcher, then click the AA-7000 icon.
[Administration] menu
Click (the help button) on the [WizAArd] launcher.
NOTE
AA-7000 2-13
Chapter 2 Basic Operation
1
2
Search
(1) Use the [Search] tab to display the item that you want to refer to.
1
2
3
4
2-14 AA-7000
2.6 Using "Help"
Key words
(1) Use the [Index] tab to display the item you want to refer to.
NOTE
There is no [Index] screen in the WizAArd software.
1
2
AA-7000 2-15
Chapter 2 Basic Operation
2.7 Checking the Gas Controller Status (AA-7000F)
The [Gas Controller Status] dialog box displays the status of the gas controller safety devices and the
inspection results.
WARNING
• If a gas leak is detected, stop using the instrument immediately.
If leaked gas is ignited it can cause a fire.
2
3
4
5
6
7
8
9
0
a
NOTE
The AA-7000G has no [Gas Controller Status] dialog box.
3 [Support Gas Pressure Indicates the status of the support gas pressure inside the gas
Monitor Level] controller.
4 [Fuel Gas Pressure Indicates the status of the fuel gas pressure inside the gas controller.
Monitor Level]
2-16 AA-7000
2.7 Checking the Gas Controller Status (AA-7000F)
6 [Fan Stop Sensor] Indicates whether or not the fan in the body of the AA instrument has
stopped.
If the indication is [OK], ignition is possible.
If the indication is [NG], ignition is not possible. Check whether or not
the rotation of the fan has been impeded by a foreign body.
7 [Burner Select Sensor Indicates the inspection results when the instrument is initialized.
Check] If the indication is [OK], ignition is possible.
If the indication is [NG] or [No Check], ignition is not possible.
Reconnect to the instrument by selecting [Instrument] - [Connect], then
implement an inspection from the [Initialize] screen.
8 [Drain Level Sensor Indicates the inspection results when the instrument is initialized.
Check] If the indication is [OK], ignition is possible.
If the indication is [NG] or [No Check], ignition is not possible.
Reconnect to the instrument by selecting [Instrument] – [Connect], then
implement an inspection from the [Initialize] screen.
9 [Support Gas Pressure Indicates the inspection results when the instrument is initialized.
Monitor Check (Air)] If the indication is [OK], ignition is possible.
If the indication is [NG] or [No Check], ignition is not possible.
Reconnect to the instrument by selecting [Instrument] - [Connect], then
implement an inspection from the [Initialize] screen.
0 [Support Gas Pressure Indicates the inspection results when the instrument is initialized.
Monitor Check (N2O)] If the indication is [OK], the N2O-C2H2 flame can be used.
If the indication is [NG] or [No Check], the N2O - C2H2 flame cannot be
used.
To use the N2O - C2H2 flame, reconnect to the instrument by selecting
[Instrument] - [Connect], then implement an inspection from the
[Initialize] screen.
a [Fuel Gas Pressure Indicates the inspection results when the instrument is initialized.
Monitor Check] If the indication is [OK], ignition is possible.
If the indication is [NG] or [No Check], ignition is not possible.
Reconnect to the instrument by selecting [Instrument] - [Connect], then
implement an inspection from the [Initialize] screen.
NOTE
When any of the sensors of the gas controller detects an error, the buzzer sounds.
AA-7000 2-17
Chapter 2 Basic Operation
2.8 Supplying Water to the Drain Tank (AA-7000F)
WARNING
• When handling chemicals, wear protective goggles and protective gloves.
If chemicals get into the eyes it can cause loss of sight. If any chemical does get into the eyes, wash it
out immediately and have your eyes examined by a doctor.
(1) Insert the drain tube into the waste liquid container.
Drain tube
NOTE
If the instrument has already been connected, taking the drain sensor out of the drain tank causes the buzzer
to sound continuously - pip-pip...pip-pip... - and the message shown below is displayed. If this happens, click
[OK] when you have finished the operation.
(4) Supply water to the drain tank until it is overflowing from the outlet.
NOTE
• A rinsing bottle (made of polythene) is useful for supplying water.
• If using a solvent other than water, ensure that it is a solvent to which the material of the rinsing bottle
has chemical resistance.
2-18 AA-7000
Chapter 3
Software Operation Flow
and Basic Operation
This chapter describes the simple operating procedures using this wizard for the flame method, the
flame micro sampling method and the furnace method. For a detailed explanation of the display
items, menus and buttons on each screen, refer to the Help for the screen concerned.
CONTENTS
AA-7000 3-1
Chapter 3 Software Operation Flow and Basic Operation
3.1 Software Basic Operation
(Flame Continuous Method)
NOTE
When measuring multiple elements, you cannot set parameters for the elements other than the current
measurement one on the "8. Optics Parameters" and "9. Atomizer/Gas Flow Rate Setup" pages. If you use
the ASC to measure multiple elements automatically and you need to modify the parameters for other
elements than the current measurement one, you can change these parameters by using the [Edit
Parameters] button in the "3. Element Selection" page.
The [WizAArd Login] dialog box will appear at the center of the screen.
3-2 AA-7000
3.1 Software Basic Operation (Flame Continuous Method)
(2) Enter "Admin" to the Login ID box and no password to the Password box to log in for the first use.
NOTE
If a login ID and password are already specified, only the authorized user is permitted to use the WizAArd.
Therefore, correctly enter the items to log in the WizAArd.
The [WizAArd Selection] dialog box will appear at the center of the screen.
NOTE
For [Recent Files] sheet and [Recent Templates] sheet, you can open the recent files or templates quickly by
selecting from the list.
AA-7000 3-3
Chapter 3 Software Operation Flow and Basic Operation
3-4 AA-7000
3.1 Software Basic Operation (Flame Continuous Method)
NOTE
You can use one of the methods below to select the element.
• Enter the element symbol directly in the element field from the keyboard.
• Click on the [T] button at the right of the element field, and select the element from the element symbol
list shown in alphabetical order.
• Click on the [Periodic Table] button and select the element from the periodic table.
4
Fig. 3.5 [Cookbook] Page in [Load Parameters]
1. Next, select [Flame Continuous] for the measurement method by the radio button.
2. Select [Normal Lamp] when using a normal hollow cathode lamp ([SR Lamp] is selected only when
the SR method is used as the background correction method).
3. When using the autosampler, click on [Using ASC] check box.
4. After finishing the settings, click on the [OK] button. If the message on the lamp setup appears,
proceed to the section 3.1.4.1 "Lamp Setting Procedure".
(3) To continue measuring multiple elements, temporarily return to the [Element Selection] page, click on
[Select Elements], and then select the next element. Repeat the sequence of clicking on the [Select
Elements] button, selecting an element and then clicking on the [OK] button, the number of times required.
NOTE
When you return to the [Element Selection] page after completing selecting elements, the selected elements
are displayed in the order of selections. If there is any element you want to delete, click on the appropriate
row to highlight it and then click on the [Delete] button. The [Meas. Element] field in the lower right part of the
screen indicates the element to be measured first.
AA-7000 3-5
Chapter 3 Software Operation Flow and Basic Operation
(4) If you click on the [Edit Parameters] button, the parameters for the element on the highlighted row on the
[Element Selection] page will be displayed. Those parameters may be modified as necessary. First
proceed with the operations without using this function.
(5) Click on [OK].
(6) If you click on the [Next] button, the [Preparation Parameters] page will be displayed.
NOTE
When analyzing plural elements sequentially, the order on the [Element Selection] page becomes the
measurement order. If you need to change the order, click on the element to highlight it and then click on
[Up] or [Down] to move the row. If the [Meas. element] at the right lower of the page is different from the first
row element, the measurement is started from the [Meas. Element] and the elements upper than it are not to
be measured.
The [Edit Parameters] page will appear with the message on the lamp setup displayed again.
(2) Click on the [OK] button.
3-6 AA-7000
3.1 Software Basic Operation (Flame Continuous Method)
NOTE
When the [Lamp Position Setup] dialog box remains displayed, the lamp turret can be rotated to allow you to
mount or replace the lamp.
AA-7000 3-7
Chapter 3 Software Operation Flow and Basic Operation
(5) Select the lamp to be used and then click on the [OK] button. You will return to the previous [Optics
Parameters] sheet.
(6) Enter [Socket Number] and click on the [OK] button.
(1) Click on the row including the desired element for settings. Click on the [Calibration Curve Setup] button to
display the [Calibration Curve Setup] page.
For details, see 3.1.5.1 "Calibration Curve Setup".
Click on the [Sample Group Setup] button to display the [Sample Group Setup] page.
For details, see 3.1.5.2 "Sample Group Setup".
Now assume entering [Calibration Curve Setup] and [Sample Group Setup] under the standard
parameters.
(2) Set the [Preparation Parameters] and click [Next].
3-8 AA-7000
3.1 Software Basic Operation (Flame Continuous Method)
1
2
3
4
5
1 Since the calibration curve method is selected here, do not tick the [Method of Standard Addition] option.
To use the standard addition method or the simple standard addition method, see the section 4.6 "Standard
Addition Method and Simple Standard Addition Method".
2 [Order] means the order of the calibration curve equation. When the calibration curve is linear, select "1st".
If the calibration curve is likely to curve more or less, you may wish to select "2nd" or "3rd". Since this
setting may be changed after viewing the actually measured values, select "1st" for now.
3 The [Zero Intercept] is used to force the calibration curve to pass through the origin. This setting may be
changed later.
4 Select [Conc. Unit] of the prepared standard samples. Clicking on [T] button to select it from the list.
5 The explanation proceeds forward without the QAQC setup. Therefore, do not click on the [QC Blank/QC
Standard Setup] button. When the QAQC settings are necessary, refer to the Chapter 6 "QA/QC Setup".
AA-7000 3-9
Chapter 3 Software Operation Flow and Basic Operation
6 Clicking on the [Repeat Conditions] button displays the [Repeat measurement Conditions] page. The
number of measurements for the same one sample is set here. The default value of the number of
measurement repetitions is "1" in the case of flame continuous method. Click on the [OK] button to close
the window with the default value remaining unchanged.
7 In the [Blank Preparation Parameters], set up the automatic periodic blank measurement. The automatic
periodic blank measurement is a function to create a measurement procedure on the MRT to eliminate the
effect of baseline drift by inserting a blank measurement in a fixed interval. Use this function when there
are many samples to be measured or when the baseline drifts.
3-10 AA-7000
3.1 Software Basic Operation (Flame Continuous Method)
1 3
1 In this example, use the default value of "1" for [Sample Group Number] and proceed forward without
selecting the [Update Current Sample Group Settings] option and the [New Sample Group] option.
2 The [QA/QC Setup] will be described in the Chapter 6 "QA/QC Setup".
3 Enter [Weight Correction Factors]. These factors are required to calculate the actual concentrations.
Weight Factor [WF], Volume Factor [VF], Dilution Factor [DF], and Correction Factor [CF] are used for the
following equation:
Actual concentration = Concentration × [VF] × [DF] × [CF]/[WF]
The actual concentration is calculated with the above equation. The function for automatically converting
the units is not available. If conversion of any unit is required, make adjustment using Correction Factor
[CF]. (See the example.) If the calculation of the actual concentration is not required, leave all the factors
as "1".
To display the unit of the actual concentration, click the [T] button for [Actual Conc. Unit] and then select
the unit from the drop-down list.
AA-7000 3-11
Chapter 3 Software Operation Flow and Basic Operation
Example
Assume that 2 grams of sample is weighed, made up to 50 mL with a solution, and then diluted by a
factor of 5 for measurement. To obtain the actual concentration from measured concentration, enter 2
(g) for Weight Factor [WF], 50 (mL) for Volume Factor [VF], 5 for Dilution Factor [DF], and 1 for
Correction Factor [CF] as follows:
Actual concentration = Concentration × 50 (mL) × 5 (times) × 1/2 (grams)
In the same example, to obtain the actual concentration (%) from the concentration (ppm) by
converting the unit, use 0.0001 for Correction Factor [CF] since 1 ppm is equal to 0.0001%, as follows:
Actual concentration = Concentration × 50 (mL) × 5 (times) × 0.0001/2 (grams)
Remarks
The unit of ppm indicates a concentration using the unit of 10−6. In the atomic absorption analysis,
both of μg/g for solid samples and μg/mL (mg/L) for liquid samples are, in practice, expressed in ppm.
4 The [Unknown/Spike Preparation Parameters] allows you to enter the preparation parameters for unknown
samples and spike samples. Spiking is one of the QA/QC techniques that are used to obtain the recovery
rate by adding a solution of a known concentration to an unknown sample. In this example, proceed
forward without entering a value (i.e., using the [S A Conc.] of 0.0000).
5 In the [Unknown/Spike Measurement Sequence], enter the number of unknown samples and sample ID's.
Enter the number of unknown samples in the [No. of Samples] field and click on the [Update] button. A
table with that number of rows will be created. Sample ID can be entered one by one in the table, but can
be entered at a time by clicking on the [Collective Setup] button. If the ASC is used, enter each turntable
position (1 to 60) in the [Pos.] field.
NOTE
In the above 3, [Weight Correction Factors] has been entered. In general, [WF] varies depending upon each
sample and can be entered in the [Unknown /Spike Measurement Sequence] table. Only the sample for
which the [Add to MRT] field is ticked is inserted into the MRT worksheet on the main screen. The created
[Unknown/Spike Measurement Sequence] table can be saved or loaded.
6 If you click on the [Collective Setup] button on the [Sample Group Setup] page of Fig. 3.14, the [Sample ID
Collective Setup] dialog box will be displayed.
3-12 AA-7000
3.1 Software Basic Operation (Flame Continuous Method)
1 In the [Sample ID Collective Setup] dialog box, enter the number of unknown samples in the [Number of
Samples] field.
2 To enter sample ID (sample name), tick the [Create Sample ID] field.
3 When you enter a name and starting number in the enabled [Sample ID] field, the same name will be given
to all the samples with sequential numbers from the starting number given to them. If the ASC is used,
specify the position of the 1st unknown sample in the [ASC Start Pos.] field. The 2nd and subsequent
positions will be automatically entered in the table.
4 If [Pre-Digestion Spike (SPK)], [Post-Digestion Spike (PDS)], and [Duplicate (DUP)] are ticked, these
measurements will be inserted in the analysis sequence for samples each in the number indicated on the
right side field. Since these samples are used for QA/QC, proceed forward without ticking the above
options in this example.
AA-7000 3-13
Chapter 3 Software Operation Flow and Basic Operation
(1) Check that the AA main unit and the related units are ON and click on the [Next] button.
(2) Check that the chimney is correctly installed on the instrument and then click [Yes].
NOTE
If the chimney is not correctly installed on the instrument, the [Flame Monitor Check] may not be performed
correctly at initialization, leading to an [NG] result.
The connection to the instrument will be started with the [Initialize] screen displayed and then the AA main unit
will be initialized. After the initialization has been finished, the parameters for the element specified in [Meas.
Element] are automatically sent to set up the instrument.
Alternatively, you may want to press the [Connect/Send Parameters] button in the [Connect to Instrument/Send
Parameters] page to perform the same operation.
3-14 AA-7000
3.1 Software Basic Operation (Flame Continuous Method)
CAUTION
• Expiration dates apply to inspections of safety devices.
Once an expiration date has passed the instrument can no longer be used. Even if the safety devices
are within the expiration date for inspections, you are strongly recommended to implement an
inspection at initialization.
• If the result of the inspection is that there is a fault in a safety device, a message describing the
fault is displayed and the device cannot be used.
If a safety device is faulty, contact your Shimadzu representative.
1 Instrument information The models of the AA main unit, ASC and GFA, the ROM versions and
the machine identification numbers are displayed here. If neither ASC
nor GFA is connected, the ASC and GFA information is not displayed.
2 Automatic inspection These are inspections that the instrument performs automatically. If
points neither ASC nor GFA is connected, [Not Connected] ( ) is shown for
the [ASC Check] and [GFA Check] points.
3 Manual inspection points Messages are displayed to prompt the successive performance of each
of these inspection points. Carry out the inspections in accordance with
the messages.
AA-7000 3-15
Chapter 3 Software Operation Flow and Basic Operation
NOTE
The time required from the start of initialization to completion of the automatic inspection points is 4 to 5
minutes (it varies depending on whether or not options are installed).
(1) When initialization of the instrument starts, the instrument information is acquired and the automatic
inspection points are implemented. On completion of the automatic inspection points, the [Gas Adjustment]
screen is displayed. After setting the fuel gas and support gas, click [Close].
1 [Purge C2H2] Performs the acetylene (C2H2) gas purge operation (5 seconds per
purge, with a limit of 5 purges).
During the purge operation, set the acetylene supply pressure to
0.09 MPa.
2 [Purge Air] Performs the air purge operation (10 seconds per purge, with no limit on
the number of purges).
During the purge operation, set the air supply pressure to 0.35 MPa.
3 [Purge N2O] Performs the nitrous oxide (N2O) gas purge operation (10 seconds per
purge, with no limit on the number of purges), when the high-
temperature burner head (optional) is used.
During the purge operation, set the nitrous oxide gas supply pressure to
0.35 MPa.
3-16 AA-7000
3.1 Software Basic Operation (Flame Continuous Method)
(2) Carry out the burner identification sensor inspection, drain sensor inspection, and support gas monitor
inspection (air).
Clicking [Yes] starts the burner identification sensor inspection.
NOTE
• On clicking [No] when still within the expiration date, the following message is displayed without
implementing an inspection. You are strongly recommended to perform inspections within the expiration
date.
• On clicking [No] when the expiration date has passed, the following message is displayed. If using the
flame method, click [Recheck].
• If the following message is displayed after clicking [Yes], set the BURNER SELECT switch to the AIR-
C2H2 position.
AIR-C2H2 N2O-C2H2
BURNER SELECT
AA-7000 3-17
Chapter 3 Software Operation Flow and Basic Operation
(3) The drain sensor inspection starts. When the following message is displayed, remove the front panel.
For details, see 2.4.1 "Removing the Front Panel".
Take the sensor out of the drain tank, and lift it above the surface of the water.
(4) When the drain sensor is lifted above the surface of the water, the following error message will be
displayed. While continuing to hold the drain sensor where it is, click [OK] in response to the error
message.
(5) Click [OK] in the [Lift the Drain Sensor over the surface of water.] dialog box.
(6) When the following message is displayed, mount the drain sensor in its original position.
Mount the front panel and click [OK]. For details, see 2.4.2 "Mounting the Front Panel".
(7) When the support gas pressure monitor inspection (Air) starts, the following message is displayed. Supply
air and click [OK].
(8) When the support gas pressure monitor inspection (N2O) starts, the following message is displayed.
3-18 AA-7000
3.1 Software Basic Operation (Flame Continuous Method)
(9) Click [Yes]. The message shown below will be displayed. Supply N2O and click [OK].
NOTE
• If the high-temperature burner head (optional) is not being used, click [No].
On clicking [No], the following message is displayed without implementing an inspection. When the
high-temperature burner head (optional) is installed and the N2O - C2H2 flame is used, you are strongly
recommended to perform inspections within the expiration date.
• Even when the expiration date for the support gas pressure monitor inspection (N2O) has passed,
provided the instrument is still within the expiration date for the other inspection points, the Air- C2H2
flame can be used.
(10) When the fuel gas pressure monitor inspection starts, the following message is displayed.
(11) Click [Check it]. The following dialog box will be displayed. Supply C2H2 gas and click [OK].
AA-7000 3-19
Chapter 3 Software Operation Flow and Basic Operation
NOTE
• If you click [Don't check it], the following message is displayed.
(12) On completion of the fuel gas pressure monitor inspection, a 8-minute automatic gas leakage inspection
starts, and initialization is completed. On completion of initialization, click [OK]. The [Initialize] screen will
close.
NOTE
The flame cannot be ignited during a gas leakage inspection.
3-20 AA-7000
3.1 Software Basic Operation (Flame Continuous Method)
(3) When all the items are checked, you can select [OK].
CAUTION
The checklist for starting the flame measurement assumes that the user checks the safety. When using
flame, properly carry out the checks.
For details, see Chapter 8 "Maintenance".
AA-7000 3-21
Chapter 3 Software Operation Flow and Basic Operation
NOTE
This page displays the wavelength, slit width, socket number, lamp current, lamp mode and so on. These
parameters are set for only the element that will be firstly measured (has been specified in the [Meas.
Element] field located in the lower right part of the [Element Select] page or the [Connect to Instrument/Send
Parameters] page).
The measurement parameters for each element are loaded from the cookbook and automatically specified
when the elements are selected.
Normally, you do not need to enter these measurement parameters. To modify them, however, you can enter a
value for the wavelength and select a value for other conditions from the list pulled down by clicking on the [T]
button. The lamp current value can be changed in units of 1 mA by clicking on the [S] or [T] buttons.
3-22 AA-7000
3.1 Software Basic Operation (Flame Continuous Method)
(1) Click on the [Next] button. A message will be displayed prompting you to do line search. Click on the [OK]
button.
The [Line Search/Beam Balance] dialog box will be displayed and the process will be carried out
automatically.
• First the line search (wavelength matching) is carried out and then the beam balance (gain
control for the detector) is performed. If only the beam balance is necessary, the line search is
not performed.
• In the line search, the highest peak near the specified wavelength is detected. In some cases,
however, the neon gas contained in the hollow cathode lamp radiates more intense light than
the light from the element. In such a case, if the correctly analyzed line is stored by clicking on
the [Wavelength Memory] button, its wavelength will be used for the subsequent line searches.
(2) Upon completion of the process, click on the [Close] button to proceed forward to the [Atomizer/Gas Flow
Rate Setup] page.
NOTE
When measuring multiple elements, you cannot set parameters for the elements other than the current
measurement one on the [Optics Parameters] and [Atomizer/Gas Flow Rate Setup] pages. If you use the
ASC to measure multiple elements automatically and you need to modify the parameters for other elements
than the current measurement one, you can change these parameters by using the [Edit Parameters] button
in the [Element Selection] page.
NOTE
SR lamp intensity is hard to stabilize in using NON-BGC mode or BGC-D2 mode in comparison with a
normal lamp. Before performing the line search, wait for 15 to 20 minutes after turning on the lamp, and then
start measurement.
AA-7000 3-23
Chapter 3 Software Operation Flow and Basic Operation
(1) To set these parameters, ignite flame and allow a standard sample to be sucked.
Even if the ASC is used for the actual measurement, use this window to manually let the sample be
sucked. Set the parameters so that the absorbance of the standard sample with a known concentration
falls within the intended range of absorbance (normally the maximum absorbance is obtained).
3-24 AA-7000
3.1 Software Basic Operation (Flame Continuous Method)
• Leave the [Burner Angle] as "0" for usual use. Change it only when you want to decrease the
sensitivity by changing the burner angle for high-concentration samples.
• For the [Burner Height], an appropriate value is indicated according to the element, so you
need not change it for usual use. However, the optimum condition for the burner height may
differ depending on the gas flow rate or the sample type. To change the value, enter a new
value.
• When the instrument is equipped with Auto Atomizer Changer (optional), clicking on the [Up]
and [Down] buttons at the bottom of the page allows you to vertically change the burner
position. As the burner position is vertically changed, the value in the [Burner Height] field is
also changed accordingly.
• The [Burner Position Auto] button is used to obtain the optimum condition for the burner height
through the measurement of the actual sample. For the steps to perform [Burner Position Auto],
see the section 4.8.1 "Setting the Optimum Condition of Burner Height".
AA-7000 3-25
Chapter 3 Software Operation Flow and Basic Operation
NOTE
If the flow meter kit (optional) has been attached, the flow rate of the support gas can be increased and
decreased by using the flow rate adjusting control, and a setting can be recorded for [Support Gas Flow
Rate].
• The [Gas Flow Auto] button is used to obtain the optimum condition for the flow rate of fuel gas
through the measurement of the actual sample. For the steps to perform [Gas Flow Auto] see
the section 4.8.2 "Setting the Optimum Condition of Fuel Gas Flow Rate".
(2) After all the settings have been finished, click on the [Finish] button.
The wizard will be exited with the main screen displayed. To save the conditions specified here as a
template, proceed to the section 3.4 "Saving the Template"; to start the measurement, proceed to the
section Chapter 4 "Measurement Procedures".
3-26 AA-7000
3.2 Software Basic Operation (Flame Micro Sampling Method)
3.2 Software Basic Operation
(Flame Micro Sampling Method)
NOTE
When measuring multiple elements, you cannot set parameters for the elements other than the current
measurement one on the "8. Optics Parameters" and "9. Atomizer/Gas Flow Rate Setup" pages. If you use
the ASC to measure multiple elements automatically and you need to modify the parameters for other
elements than the current measurement one, you can change these parameters by using the [Edit
Parameters] button in the "3. Element Selection" page.
The [WizAArd Login] dialog box will appear at the center of the screen.
AA-7000 3-27
Chapter 3 Software Operation Flow and Basic Operation
(2) Enter "Admin" to the Login ID box and no password to the Password box to log in for the first use.
NOTE
If a login ID and password are already specified, only the authorized user is permitted to use the WizAArd.
Therefore, correctly enter the items to log in the WizAArd.
The [WizAArd Selection] dialog box will appear at the center of the screen.
NOTE
For the [Recent Files] screen and [Recent Templates] screen, you can open the recent files or templates
quickly by selecting from the list.
3-28 AA-7000
3.2 Software Basic Operation (Flame Micro Sampling Method)
AA-7000 3-29
Chapter 3 Software Operation Flow and Basic Operation
NOTE
You can use one of the methods below to select the element.
• Enter the element symbol directly in the element field from the keyboard.
• Click on the [T] button at the right of the element field, and select the element from the element symbol
list shown in alphabetical order.
• Click on the [Periodic Table] button and select the element from the periodic table.
4
Fig. 3.31 [Cookbook] Page in [Load Parameters]
1. Next, select [Flame Micro Sampling] for the measurement method by the radio button.
2. Select [Normal Lamp] when using a normal hollow cathode lamp ([SR Lamp] is selected only when
the SR method is used as the background correction method).
3. When using the autosampler, click on [Using ASC] check box.
4. After finishing the settings, click on the [OK] button. If the message on the lamp setup appears,
proceed to the section 3.2.4.1 "Lamp Setting Procedure".
(3) To continue measuring multiple elements, temporarily return to the [Element Selection] page, click on
[Select Elements], and then select the next element. Repeat the sequence of clicking on the [Select
Elements] button, selecting an element and then clicking on the [OK] button, the number of times required.
NOTE
When you return to the [Element Selection] page after completing selecting elements, the selected elements
are displayed in the order of selections. If there is any element you want to delete, click on the appropriate
row to highlight it and then click on the [Delete] button. The [Meas. Element] field in the lower right part of the
screen indicates the element to be measured first.
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3.2 Software Basic Operation (Flame Micro Sampling Method)
(4) If you click on the [Edit Parameters] button, the parameters for the element on the highlighted row on the
[Element Selection] page will be displayed. Those parameters may be modified as necessary. First
proceed with the operations without using this function.
(5) Click on [OK].
(6) If you click on the [Next] button, the [Preparation Parameters] page will be displayed.
NOTE
When analyzing multiple elements sequentially, the order on the [Element Selection] page becomes the
measurement order. If you need to change the order, click on the element to highlight it and then click on
[Up] or [Down] to move the row. If the [Meas. element] at the right lower of the page is different from the first
row element, the measurement is started from the [Meas. Element] and the elements upper than it are not to
be measured.
The [Edit Parameters] page will appear with the message on the lamp setup displayed again.
(2) Click on the [OK] button.
AA-7000 3-31
Chapter 3 Software Operation Flow and Basic Operation
NOTE
When the [Lamp Position Setup] dialog box remains displayed, the lamp turret can be rotated to allow you to
mount or replace the lamp.
(5) Select the lamp to be used and then click on the [OK] button. You will return to the previous [Optics
Parameters] sheet.
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3.2 Software Basic Operation (Flame Micro Sampling Method)
(1) Click on the row including the desired element for settings. Click on the [Calibration Curve Setup] button to
display the [Calibration Curve Setup] page.
For details, see 3.2.5.1 "Calibration Curve Setup".
Click on the [Sample Group Setup] button to display the [Sample Group Setup] page.
For details, see 3.2.5.2 "Sample Group Setup".
Now assume entering [Calibration Curve Setup] and [Sample Group Setup] under the standard
parameters.
(2) Set the [Preparation Parameters] and click [Next].
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1
2
3
4
5
1 Since the calibration curve method is selected here, do not tick the [Method of Standard Addition] option.
To use the standard addition method or the simple standard addition method, see the section 4.6 "Standard
Addition Method and Simple Standard Addition Method".
2 [Order] means the order of the calibration curve equation. When the calibration curve is linear, select "1st".
If the calibration curve is likely to curve more or less, you may wish to select "2nd" or "3rd". Since this
setting may be changed after viewing the actually measured values, select "1st" for now.
3 The [Zero Intercept] is used to force the calibration curve to pass through the origin. This setting may be
changed later.
4 Select [Conc. Unit] of the prepared standard samples. Clicking on [T] button to select it from the list.
5 The explanation proceeds forward without the QAQC setup. Therefore, do not click on the [QC Blank/QC
Standard Setup] button. When the QAQC settings are necessary, refer to the Chapter 6 "QA/QC Setup".
6 [Common Settings for Preparation Parameters] allows you to enable/disable mixing and specify the mixing,
the repeat conditions and the reagents.
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3.2 Software Basic Operation (Flame Micro Sampling Method)
• Tick the [Mixing ON] option and then click on the [Mixing] button. The [Mixing Setup] dialog box
will be displayed.
In the [Mixing Setup] dialog box, set the [Volume] in the [Injection Parameters]. The default value is
20 (μL), but 50 (μL) is suitable for the flame micro sampling method. Leave the other settings on the
[Mixing Setup] dialog box as they are as the default values.
• Clicking on the [Repeat Conditions] button displays the [Repeat measurement Conditions]
dialog box. The number of measurements for the same one sample is set here. For the
measurement by the flame micro sampling method, the default value of the number of
measurement repetitions is "2" (the allowable maximum is "3"). As the default value is to be
selected here, click on the [OK] button to close the dialog box.
NOTE
The number of repetition refers to the minimum number of measurement repetitions to be used in acquiring
data. After completing this set number of measurement repetitions, the average value, relative standard
deviation (RSD) and standard deviation (SD) are calculated. Then, the measurement repetitions will continue
until (1) the CV value limit is satisfied, (2) the standard deviation limit is satisfied, or (3) the maximum number
of repetition is reached. Setup is possible up to 20 for each item.
• Click on the [Reagent] button. The [Reagent Setup] dialog box will be displayed. This dialog
box allows you to enter [Reagent Name] and [Reagent Position] of 4 kinds of reagents.
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Chapter 3 Software Operation Flow and Basic Operation
7 In the [Blank Preparation Parameters], set up the automatic periodic blank measurement. The automatic
periodic blank measurement is a function to create a measurement procedure on the MRT to eliminate the
effect of baseline drift by inserting a blank measurement in a fixed interval. Use this function when there
are many samples to be measured or when the baseline drifts.
Mixing ON/OFF
When no samples are mixed using the ASC:
Do not tick [Mixing ON] or disable mixing. When mixing is disabled, the [Total Volume] in [Blank Preparation
Parameters], [Reslope Preparation Parameters] and [Measurement Sequence for Calibration Curve] will be the
amount injected to the micro sampling port. Enter the amount of the sample injected to the micro sampling port
in the [Vol] field. (You cannot directly enter it in [Total Volume].) Leave all the [Diluent], [Reagent 1], [Reagent 2]
and [Reagent 3] as zero. Then [Total Volume] will be the same value as [Vol]. When only sample is injected (all
of the diluent and reagent parameters are set to zero), the instrument will automatically determine that no
mixing is performed, even if the mixing is enabled.
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3.2 Software Basic Operation (Flame Micro Sampling Method)
NOTE
The [Total Volume] must meet the following conditions:
• When mixing is not performed:
(Injection Vol.) = (Total Vol.) </= 90 μL
• When mixing is performed:
(Injection Vol.) = (Max. No. of Reps.) + 50 μL </= (Total Vol.) </= 600 μL
(In this regard, the injection volume is the value specified on the [Mixing Setup] dialog box; +50 μL is the
dead volume of the mixing port.)
Example
To prepare each 400 μL of standard samples of 10, 20, and 30 ppb from the concentrate solution of a
standard sample of 100 ppb, assume the concentrate solution of the standard sample as a "sample" and
enter each value as follows. The total volume will be calculated automatically.
10 1 40 360 0 0 0 400
20 1 80 320 0 0 0 400
If the injection volume (entered on the [Mixing Setup] dialog box or the [ASC Parameters] page) is
assumed as 50 μL and the maximum number of repetition (entered in the [Repeat Measurement
Conditions] dialog box) as 3, the calculation is as follows:
50 μL × 3 + 50 μL </= 400 μL </= 600 μL
This means that the total volume meets the above condition.
Parameters Screens
(a) Measurement Type (calibration curve method / [Calibration Curve Setup] dialog box
standard addition method)
(c) Preparation Parameters (Blank, Reslope, STD) [Calibration Curve Setup] dialog box
(d) Reagent Name and Reagent Position [Reagent Setup] dialog box
AA-7000 3-37
Chapter 3 Software Operation Flow and Basic Operation
NOTE
No files in which (a) Measurement Type and (b) Mixing ON/OFF are different from the current settings can
be loaded.
1 3
1 In this example, use the default value of "1" for [Sample Group Number] and proceed forward without
selecting the [Update Current Sample Group Settings] option and the [New Sample Group] option.
2 The [QA/QC Setup] will be described in the Chapter 6 "QA/QC Setup".
3 Enter [Weight Correction Factors]. These factors are required to calculate the actual concentrations.
Weight Factor [WF], Volume Factor [VF], Dilution Factor [DF], and Correction Factor [CF] are used for the
following equation:
Actual concentration = Concentration × [VF] × [DF] × [CF]/[WF]
The actual concentration is calculated with the above equation. The function for automatically converting
the units is not available. If conversion of any unit is required, make adjustment using Correction Factor
[CF]. (See the example.) If the calculation of the actual concentration is not required, leave all the factors
as "1".
To display the unit of the actual concentration, click the [T] button for [Actual Conc. Unit] and then select
the unit from the drop-down list.
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3.2 Software Basic Operation (Flame Micro Sampling Method)
Example
Assume that 2 grams of sample is weighed, made up to 50 mL with a solution, and then diluted by a factor
of 5 for measurement. To obtain the actual concentration from measured concentration, enter 2 (g) for
Weight Factor [WF], 50 (mL) for Volume Factor [VF], 5 for Dilution Factor [DF], and 1 for Correction Factor
[CF] as follows:
Actual concentration = Concentration × 50 (mL) × 5 (times) × 1/2 (grams)
In the same example, to obtain the actual concentration (%) from the concentration (ppm) by converting
the unit, use 0.0001 for Correction Factor [CF] since 1 ppm is equal to 0.0001%, as follows:
Actual concentration = Concentration × 50 (mL) × 5 (times) × 0.0001/2 (grams)
Remarks
The unit of ppm indicates a concentration using the unit of 10-6. In the atomic absorption analysis, both of
μg/g for solid samples and μg/mL (mg/L) for liquid samples are, in practice, expressed in ppm.
4 The [Unknown/Spike Preparation Parameters] allows you to enter the preparation parameters for unknown
samples and spike samples. Spiking is one of the QA/QC techniques that are used to obtain the recovery
rate by adding a solution of a known concentration to an unknown sample. In this example, proceed
forward without entering a value (i.e., using the [S A Conc.] of 0.0000).
5 In the [Unknown/Spike Measurement Sequence], enter the number of unknown samples and sample ID's.
Enter the number of unknown samples in the [No. of Samples] field and click on the [Update] button. A
table with that number of rows will be created. Sample ID can be entered one by one in the table, but can
be entered at a time by clicking on the [Collective Setup] button. If the ASC is used, enter each turntable
position (1 to 60) in the [Pos.] field.
NOTE
In the above 3, [Weight Correction Factors] has been entered. In general, [WF] varies depending upon each
sample and can be entered in the [Unknown /Spike Measurement Sequence] table. Only the sample for
which the [Add to MRT] field is ticked is inserted into the MRT worksheet on the main screen. The created
[Unknown/Spike Measurement Sequence] table can be saved or loaded.
6 If you click on the [Collective Setup] button on the [Sample Group Setup] page of Fig. 3.41, the [Sample ID
Collective Setup] dialog box will be displayed.
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Chapter 3 Software Operation Flow and Basic Operation
1 In the [Sample ID Collective Setup] dialog box, enter the number of unknown samples in the [Number of
Samples] field.
2 To enter sample ID (sample name), tick the [Create Sample ID] field.
3 When you enter a name and starting number in the enabled [Sample ID] field, the same name will be given
to all the samples with sequential numbers from the starting number given to them. If the ASC is used,
specify the position of the 1st unknown sample in the [ASC Start Pos.] field. The 2nd and subsequent
positions will be automatically entered in the table.
4 If [Pre-Digestion Spike (SPK)], [Post-Digestion Spike (PDS)], and [Duplicate (DUP)] are ticked, these
measurements will be inserted in the analysis sequence for samples each in the number indicated on the
right side field. Since these samples are used for QA/QC, proceed forward without ticking the above
options in this example.
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3.2 Software Basic Operation (Flame Micro Sampling Method)
(1) Check that the AA main unit and the related units are ON and click on the [Next] button.
(2) Check that the chimney is correctly installed on the instrument and then click [Yes].
NOTE
If the chimney is not correctly installed on the instrument, the [Flame Monitor Check] may not be performed
correctly at initialization, leading to an [NG] result.
The connection to the instrument will be started with the [Initialize] screen displayed and then the AA main
unit will be initialized. After the initialization has been finished, the parameters for the element specified in
[Meas. Element] are automatically sent to set up the instrument.
Alternatively, you may want to press the [Connect/Send Parameters] button in the [Connect to Instrument/
Send Parameters] page to perform the same operation.
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Chapter 3 Software Operation Flow and Basic Operation
CAUTION
• Expiration dates apply to inspections of safety devices.
Once an expiration date has passed the instrument can no longer be used. Even if the safety devices
are within the expiration date for inspections, you are strongly recommended to implement an
inspection at initialization.
• If the result of the inspection is that there is a fault in a safety device, a message describing the
fault is displayed and the device cannot be used.
If a safety device is faulty, contact your Shimadzu representative.
1 Instrument information The models of the AA main unit, ASC and GFA, the ROM versions and
the machine identification numbers are displayed here. If neither ASC
nor GFA is connected, the ASC and GFA information is not displayed.
2 Automatic inspection These are inspections that the instrument performs automatically. If
points neither ASC nor GFA is connected, [Not Connected] ( ) is shown for
the [ASC Check] and [GFA Check] points.
3 Manual inspection points Messages are displayed to prompt the successive performance of each
of these inspection points. Carry out the inspections in accordance with
the messages.
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3.2 Software Basic Operation (Flame Micro Sampling Method)
NOTE
The time required from the start of initialization to completion of the automatic inspection points is 4 to
5 minutes (it varies depending on whether or not options are installed).
(1) When initialization of the instrument starts, the instrument information is acquired and the automatic
inspection points are implemented. On completion of the automatic inspection points, the [Gas Adjustment]
screen is displayed. After setting the fuel gas and support gas, click [Close].
1 [Purge C2H2] Performs the acetylene (C2H2) gas purge operation (5 seconds per
purge, with a limit of 5 purges).
During the purge operation, set the acetylene supply pressure to
0.09 MPa.
2 [Purge Air] Performs the air purge operation (10 seconds per purge, with no limit on
the number of purges).
During the purge operation, set the air supply pressure to 0.35 MPa.
3 [Purge N2O] Performs the nitrous oxide (N2O) gas purge operation (10 seconds per
purge, with no limit on the number of purges), when the high-
temperature burner head (optional) is used.
During the purge operation, set the nitrous oxide gas supply pressure to
0.35 MPa.
AA-7000 3-43
Chapter 3 Software Operation Flow and Basic Operation
(2) Carry out the burner identification sensor inspection, drain sensor inspection, and support gas monitor
inspection (air).
Clicking [Yes] starts the burner identification sensor inspection.
NOTE
• On clicking [No] when still within the expiration date, the following message is displayed without
implementing an inspection. You are strongly recommended to perform inspections within the expiration
date.
• On clicking [No] when the expiration date has passed, the following message is displayed. If using the
flame method, click [Recheck].
• If the following message is displayed after clicking [Yes], set the BURNER SELECT switch to the AIR-
C2H2 position.
AIR-C2H2 N2O-C2H2
BURNER SELECT
3-44 AA-7000
3.2 Software Basic Operation (Flame Micro Sampling Method)
(3) The drain sensor inspection starts. When the following message is displayed, remove the front panel.
For details, see 2.4.1 "Removing the Front Panel".
Take the sensor out of the drain tank, and lift it above the surface of the water.
(4) When the drain sensor is lifted above the surface of the water, the following error message will be
displayed. While continuing to hold the drain sensor where it is, click [OK] in response to the error
message.
(5) Click [OK] in the [Lift the Drain Sensor over the surface of water.] dialog box.
(6) When the following message is displayed, mount the drain sensor in its original position.
Mount the front panel and click [OK]. For details, see 2.4.2 "Mounting the Front Panel".
(7) When the support gas pressure monitor inspection (Air) starts, the following message is displayed. Supply
air and click [OK].
(8) When the support gas pressure monitor inspection (N2O) starts, the following message is displayed.
AA-7000 3-45
Chapter 3 Software Operation Flow and Basic Operation
(9) Click [Yes]. The message shown below will be displayed. Supply N2O and click [OK].
NOTE
• If the high-temperature burner head (optional) is not being used, click [No].
On clicking [No], the following message is displayed without implementing an inspection. When the
high-temperature burner head (optional) is installed and the N2O - C2H2 flame is used, you are strongly
recommended to perform inspections within the expiration date.
• Even when the expiration date for the support gas pressure monitor inspection (N2O) has passed,
provided the instrument is still within the expiration date for the other inspection points, the Air- C2H2
flame can be used.
(10) When the fuel gas pressure monitor inspection starts, the following message is displayed.
(11) Click [Check it]. The following dialog box will be displayed. Supply C2H2 gas and click [OK].
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3.2 Software Basic Operation (Flame Micro Sampling Method)
NOTE
• If you click [Don't check it], the following message is displayed.
(12) On completion of the fuel gas pressure monitor inspection, a 8-minute automatic gas leakage inspection
starts, and initialization is completed. On completion of initialization, click [OK]. The [Initialize] screen will
close.
NOTE
The flame cannot be ignited during a gas leakage inspection.
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Chapter 3 Software Operation Flow and Basic Operation
(3) When all the items are checked, you can select [OK].
CAUTION
The checklist for starting the flame measurement assumes that the user checks the safety. When using
flame, properly carry out the checks.
For details, see Chapter 8 "Maintenance".
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3.2 Software Basic Operation (Flame Micro Sampling Method)
NOTE
This page displays the wavelength, slit width, socket number, lamp current, lamp mode and so on. These
parameters are set for only the element that will be firstly measured (has been specified in the [Meas.
Element] field located in the lower right part of the [Element Select] page or the [Connect to Instrument/Send
Parameters] page).
The measurement parameters for each element are loaded from the cookbook and automatically specified
when the elements are selected.
Normally, you do not need to enter these measurement parameters. To modify them, however, you can enter a
value for the wavelength and select a value for other conditions from the list pulled down by clicking on the [T]
button. The lamp current value can be changed in units of 1 mA by clicking on the [S] or [T] buttons.
AA-7000 3-49
Chapter 3 Software Operation Flow and Basic Operation
(1) Click on the [Next] button. A message will be displayed prompting you to do line search. Click on the [OK]
button.
The [Line Search/Beam Balance] dialog box will be displayed and the process will be carried out
automatically.
• First the line search (wavelength matching) is carried out and then the beam balance (gain
control for the detector) is performed. If only the beam balance is necessary, the line search is
not performed.
• In the line search, the highest peak near the specified wavelength is detected. In some cases,
however, the neon gas contained in the hollow cathode lamp radiates more intense light than
the light from the element. In such a case, if the correctly analyzed line is stored by clicking on
the [Wavelength Memory] button, its wavelength will be used for the subsequent line searches.
(2) Upon completion of the process, click on the [Close] button to proceed forward to the [Atomizer/Gas Flow
Rate Setup] page.
NOTE
When measuring multiple elements, you cannot set parameters for the elements other than the current
measurement one on the [Optics Parameters] and [Atomizer/Gas Flow Rate Setup] pages. If you use the
ASC to measure multiple elements automatically and you need to modify the parameters for other elements
than the current measurement one, you can change these parameters by using the [Edit Parameters] button
in the [Element Selection] page.
NOTE
SR lamp intensity is hard to stabilize in using NON-BGC mode or BGC-D2 mode in comparison with a
normal lamp. Before performing the line search, wait for 15 to 20 minutes after turning on the lamp, and then
start measurement.
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3.2 Software Basic Operation (Flame Micro Sampling Method)
(1) To set these parameters, ignite flame and allow a standard sample to be sucked.
Even if the ASC is used for the actual measurement, use this window to manually let the sample be
sucked. Set the parameters so that the absorbance of the standard sample with a known concentration
falls within the intended range of absorbance (normally the maximum absorbance is obtained).
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• Leave the [Burner Angle] as "0" for usual use. Change it only when you want to decrease the sensitivity by
changing the burner angle for high-concentration samples.
• For the [Burner Height], an appropriate value is indicated according to the element, so you need not
change it for usual use. However, the optimum condition for the burner height may differ depending on the
gas flow rate or the sample type. To change the value, enter a new value.
• When the instrument is equipped with Auto Atomizer Changer (optional), clicking on the [Up] and [Down]
buttons at the bottom of the page allows you to vertically change the burner position. As the burner position
is vertically changed, the value in the [Burner Height] field is also changed accordingly.
• The [Burner Position Auto] button is used to obtain the optimum condition for the burner height through the
measurement of the actual sample. For the steps to perform [Burner Position Auto], see the section 4.8.1
"Setting the Optimum Condition of Burner Height".
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3.2 Software Basic Operation (Flame Micro Sampling Method)
NOTE
If the flow meter kit (optional) has been attached, the flow rate of the support gas can be increased and
decreased by using the flow rate adjusting control, and a setting can be recorded for [Support Gas Flow
Rate].
• The [Gas Flow Auto] button is used to obtain the optimum condition for the flow rate of fuel gas
through the measurement of the actual sample. For the steps to perform [Gas Flow Auto] see
the section 4.8.2 "Setting the Optimum Condition of Fuel Gas Flow Rate".
(2) After all the settings have been finished, click on the [Finish] button.
The wizard will be exited with the main screen displayed. To save the conditions specified here as a
template, proceed to the section 3.4 "Saving the Template"; to start the measurement, proceed to the
section Chapter 4 "Measurement Procedures".
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3.3 Software Basic Operation (Furnace Method)
NOTE
When measuring multiple elements, you cannot set parameters for the elements other than the current
measurement one on the "8. Optics Parameters" and "9. Furnace Program" pages. If you use the ASC to
measure multiple elements automatically and you need to modify the parameters for other elements than the
current measurement one, you can change these parameters by using the [Edit Parameters] button in the "3.
Element Selection" page.
The [WizAArd Login] dialog box will appear at the center of the screen.
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3.3 Software Basic Operation (Furnace Method)
(2) Enter "Admin" to the Login ID box and no password to the Password box to log in for the first use.
NOTE
If a login ID and password are already specified, only the authorized user is permitted to use the WizAArd.
Therefore, correctly enter the items to log in the WizAArd.
The [WizAArd Selection] dialog box will appear at the center of the screen.
NOTE
For the [Recent Files] screen and [Recent Templates] screen, you can open the recent files or templates
quickly by selecting from the list.
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3.3 Software Basic Operation (Furnace Method)
NOTE
You can use one of the methods below to select the element.
• Enter the element symbol directly in the element field from the keyboard.
• Click on the [T] button at the right of the element field, and select the element from the element symbol
list shown in alphabetical order.
• Click on the [Periodic Table] button and select the element from the periodic table.
1
2
3
4
Fig. 3.58 [Cookbook] Page in [Load Parameters]
1. Next, select [Furnace] for the measurement method by the radio button.
2. Select [Normal Lamp] when using a normal hollow cathode lamp ([SR Lamp] is selected only when
the SR method is used as the background correction method).
3. When using the autosampler, click on [Using ASC] check box.
4. After finishing the settings, click on the [OK] button. If the message on the lamp setup appears,
proceed to the section 3.3.4.1 "Lamp Setting Procedure".
(3) To continue measuring multiple elements, temporarily return to the [Element Selection] page, click on
[Select Elements], and then select the next element. Repeat the sequence of clicking on the [Select
Elements] button, selecting an element and then clicking on the [OK] button, the number of times required.
NOTE
When you return to the [Element Selection] page after completing selecting elements, the selected elements
are displayed in the order of selections. If there is any element you want to delete, click on the appropriate
row to highlight it and then click on the [Delete] button. The [Meas. Element] field in the lower right part of the
screen indicates the element to be measured first.
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(4) If you click on the [Edit Parameters] button, the parameters for the element on the highlighted row on the
[Element Selection] page will be displayed. Those parameters may be modified as necessary. First
proceed with the operations without using this function.
(5) Click on [OK].
(6) If you click on the [Next] button, the [Preparation Parameters] page will be displayed.
NOTE
When analyzing multiple elements sequentially, the order on the [Element Selection] page becomes the
measurement order. If you need to change the order, click on the element to highlight it and then click on
[Up] or [Down] to move the row. If the [Meas. element] at the right lower of the page is different from the first
row element, the measurement is started from the [Meas. Element] and the elements upper than it are not to
be measured.
The [Edit Parameters] page will appear with the message on the lamp setup displayed again.
(2) Click on the [OK] button.
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3.3 Software Basic Operation (Furnace Method)
NOTE
When the [Lamp Position Setup] dialog box remains displayed, the lamp turret can be rotated to allow you to
mount or replace the lamp.
(5) Select the lamp to be used and then click on the [OK] button. You will return to the previous [Optics
Parameters] sheet.
(6) Enter [Socket Number] and click on the [OK] button.
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(1) Click on the row including the desired element for settings. Click on the [Calibration Curve Setup] button to
display the [Calibration Curve Setup] page.
For details, see 3.3.5.1 "Calibration Curve Setup".
Click on the [Sample Group Setup] button to display the [Sample Group Setup] page.
For details, see 3.3.5.2 "Sample Group Setup".
Now assume entering [Calibration Curve Setup] and [Sample Group Setup] under the standard
parameters.
(2) Set the [Preparation Parameters] and click [Next].
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3.3 Software Basic Operation (Furnace Method)
1
2
3
4
5
1 Since the calibration curve method is selected here, do not tick the [Method of Standard Addition] option.
To use the standard addition method or the simple standard addition method, see the section 4.6 "Standard
Addition Method and Simple Standard Addition Method".
2 [Order] means the order of the calibration curve equation. When the calibration curve is linear, select "1st".
If the calibration curve is likely to curve more or less, you may wish to select "2nd" or "3rd". Since this
setting may be changed after viewing the actually measured values, select "1st" for now.
3 The [Zero Intercept] is used to force the calibration curve to pass through the origin. This setting may be
changed later.
4 Select [Conc. Unit] of the prepared standard samples. Clicking on [T] button to select it from the list.
5 The explanation proceeds forward without the QAQC setup. Therefore, do not click on the [QC Blank/QC
Standard Setup] button. When the QAQC settings are necessary, refer to the Chapter 6 "QA/QC Setup".
6 [Common Settings for Preparation Parameters] allows you to enable/disable mixing and specify the mixing,
the repeat conditions, the coating/boost cycle and the reagents.
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• Tick the [Mixing ON] option and then click on the [Mixing] button. The [Mixing Setup] dialog box
will be displayed.
In the [Mixing Setup] dialog box, set the [Volume] in the [Injection Parameters]. The default value is
20 (μL). Leave the other settings on the [Mixing Setup] dialog box as they are as the default values.
• Clicking on the [Repeat Conditions] button displays the [Repeat measurement Conditions]
dialog box. The number of measurements for the same one sample is set here. For the
measurement by the furnace method, the default value of the number of measurement
repetitions is "2" (the allowable maximum is "3"). As the default value is to be selected here,
click on the [OK] button to close the dialog box.
NOTE
The number of repetition refers to the minimum number of measurement repetitions to be used in acquiring
data. After completing this set number of measurement repetitions, the average value, relative standard
deviation (RSD) and standard deviation (SD) are calculated. Then, the measurement repetitions will continue
until (1) the CV value limit is satisfied, (2) the standard deviation limit is satisfied, or (3) the maximum number
of repetition is reached. Setup is possible up to 20 for each item.
• Click on the [Coating] button. The [Coating and Boost Cycles] dialog box will be displayed.
Coating refers to injecting a specified reagent into the furnace and drying it prior to the sample
injection (i.e., coating the tube surface). First, the checked mark reagent is injected in the furnace, and
heating is executed up to the furnace program stage specified in [Last Coating Cycle]. After this, the
sample is injected.
Furnace boost cycle refers to the repetitive cycle of sample injection into the furnace, and drying and
ashing of the sample in order to raise the concentration of the target element in the sample. Repeating
this boost cycle enables measurement of the sample whose concentration is lower than the
quantification range by concentrating it and raising its absorbance to the quantitative range of the
calibration curve.
In this case, use the default values as they are.
• Click on the [Reagent] button. The [Reagent Setup] dialog box will be displayed. This dialog
box allows you to enter [Reagent Name] and [Reagent Position] of 4 kinds of reagents, and
setup the intake order for the four reagents.
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3.3 Software Basic Operation (Furnace Method)
7 In the [Blank Preparation Parameters], set up the automatic periodic blank measurement. The automatic
periodic blank measurement is a function to create a measurement procedure on the MRT to eliminate the
effect of baseline drift by inserting a blank measurement in a fixed interval.
Mixing ON/OFF
When no samples are mixed using the ASC:
Do not tick [Mixing ON] or disable mixing. When mixing is disabled, the [Total Volume] in [Blank Preparation
Parameters], [Reslope Preparation Parameters] and [Measurement Sequence for Calibration Curve] will be the
amount injected to the graphite tube. Enter the amount of the sample injected to the graphite tube in the [Vol]
field. (You cannot directly enter it in [Total Volume].) Leave all the [Diluent], [Reagent 1], [Reagent 2] and
[Reagent 3] as zero. Then [Total Volume] will be the same value as [Vol]. Ensure that Total does not exceed
90 μL. Normally, approximately 20 μL would be appropriate. When only sample is injected (all of the diluent and
reagent parameters are set to zero), the instrument will automatically determine that no mixing is performed,
even if the mixing is enabled.
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Chapter 3 Software Operation Flow and Basic Operation
NOTE
The [Total Volume] must meet the following conditions:
• When mixing is not performed:
(Injection Vol.) = (Total Vol.) </= 90 μL
• When mixing is performed:
(Injection Vol.) = (Max. No. of Reps.) × (No. of Boost cycles) + 50 μL </= (Total Vol.) </= 600 μL
(In this regard, the injection volume is the value specified on the [Mixing Setup] dialog box; +50 μL is the
dead volume of the mixing port.) If the boost cycle is not used, the No. of Boost cycles is "1".
Example
To prepare each 400 μL of standard samples of 10, 20, and 30 ppb from the concentrate solution of a
standard sample of 100 ppb, assume the concentrate solution of the standard sample as a "sample" and
enter each value as follows. The total volume will be calculated automatically.
10 1 40 360 0 0 0 400
20 1 80 320 0 0 0 400
If the injection volume (entered on the [Mixing Setup] dialog box or the [ASC Parameters] page) is
assumed as 20 μL and the maximum number of repetition (entered in the [Repeat Measurement
Conditions] dialog box) as 5, and the boost cycles as not performed ([Number of Boost Cycles] in the
[Coating and Boost Cycles] dialog box is set to "1"), the calculation is as follows:
20 μL × 5 × 1 + 50 μL </= 400 μL </= 600 μL
This means that the total volume meets the above condition.
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3.3 Software Basic Operation (Furnace Method)
Parameter Screens
(a) Measurement Type (calibration curve method / [Calibration Curve Setup] dialog box
standard addition method)
(c) Preparation Parameters (Blank, Reslope, STD) [Calibration Curve Setup] dialog box
(d) Reagent Name and Reagent Position [Reagent Setup] dialog box
(f) Coating and Boost Cycles [Coating and Boost Cycles] dialog box
NOTE
No files in which (a) Measurement Type and (b) Mixing ON/OFF are different from the current settings can
be loaded.
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1
3
1 In this example, use the default value of "1" for [Sample Group Number] and proceed forward without
selecting the [Update Current Sample Group Settings] option and the [New Sample Group] option.
2 The [QA/QC Setup] will be described in the Chapter 6 "QA/QC Setup".
3 Enter [Weight Correction Factors]. These factors are required to calculate the actual concentrations.
Weight Factor [WF], Volume Factor [VF], Dilution Factor [DF], and Correction Factor [CF] are used for the
following equation:
Actual concentration = Concentration × [VF] × [DF] × [CF]/[WF]
The actual concentration is calculated with the above equation. The function for automatically converting
the units is not available. If conversion of any unit is required, make adjustment using Correction Factor
[CF]. (See the example.) If the calculation of the actual concentration is not required, leave all the factors
as "1".
However, when the "Auto Dilution and Remeasurement" is performed, the dilution ratio used for the
automatic dilution by the ASC is displayed in the [ASC DF] field (ASC dilution factor) on the MRT
worksheet and the actual concentration is calculated as follows:
Actual concentration = Concentration × [VF] × [DF] × [ASC dilution factor] × [CF]/[WF]
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3.3 Software Basic Operation (Furnace Method)
Example
Assume that a reagent and diluent are added to 50 μL of a sample into a total of 250 μL. To obtain the
actual concentration from the measured concentration, calculate it using 50 (μL) for Weight Factor [WF],
250 (μL) for Volume Factor [VF], and 1 for Correction Factor [CF] as follows:
Actual concentration = Concentration × (250 μL) × 1 × 1/(50 μL)
To obtain the actual concentration by converting the measured concentration (ppb) into the actual one
(ppm) in the same example, use 0.001 (1 ppb = 0.001 ppm) for Correction Factor [CF] in the above
equation as follows:
Actual concentration in ppm = Concentration in ppb × (250 μL) × 1 × 0.001/(50 μL)
4 The [Unknown/Spike Preparation Parameters] allows you to enter the preparation parameters for unknown
samples and spike samples. Spiking is one of the QA/QC techniques that are used to obtain the recovery
rate by adding a solution of a known concentration to an unknown sample. In this example, proceed
forward without entering a value (i.e., using the [S A Conc.] of 0.0000).
5 In the [Unknown/Spike Measurement Sequence], enter the number of unknown samples and sample ID's.
Enter the number of unknown samples in the [No. of Samples] field and click on the [Update] button. A
table with that number of rows will be created. Sample ID can be entered one by one in the table, but can
be entered at a time by clicking on the [Collective Setup] button. If the ASC is used, enter each turntable
position (1 to 60) in the [Pos.] field.
NOTE
In the above 3, [Weight Correction Factors] has been entered. In general, [WF] varies depending upon each
sample and can be entered in the [Unknown /Spike Measurement Sequence] table. Only the sample for
which the [Add to MRT] field is ticked is inserted into the MRT worksheet on the main screen. The created
[Unknown/Spike Measurement Sequence] table can be saved or loaded.
6 If you click on the [Collective Setup] button on the [Sample Group Setup] page of Fig. 3.68, the [Sample ID
Collective Setup] dialog box will be displayed.
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Chapter 3 Software Operation Flow and Basic Operation
1 In the [Sample ID Collective Setup] dialog box, enter the number of unknown samples in the [Number of
Samples] field.
2 To enter sample ID (sample name), tick the [Create Sample ID] field.
3 When you enter a name and starting number in the enabled [Sample ID] field, the same name will be given
to all the samples with sequential numbers from the starting number given to them. If the ASC is used,
specify the position of the 1st unknown sample in the [ASC Start Pos.] field. The 2nd and subsequent
positions will be automatically entered in the table.
4 If [Pre-Digestion Spike (SPK)], [Post-Digestion Spike (PDS)], and [Duplicate (DUP)] are ticked, these
measurements will be inserted in the analysis sequence for samples each in the number indicated on the
right side field. Since these samples are used for QA/QC, proceed forward without ticking the above
options in this example.
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3.3 Software Basic Operation (Furnace Method)
(1) Check that the AA main unit and the related units are ON and click on the [Next] button.
NOTE
• With the AA-7000F, check that the chimney has been correctly installed on the instrument, then click
[Yes].
• If the chimney is not correctly installed on the instrument, the [Flame Monitor Check] may not be
performed correctly at initialization, leading to an [NG] result.
The connection to the instrument will be started with the [Initialize] screen displayed and then the AA main unit
will be initialized. After the initialization has been finished, the parameters for the element specified in [Meas.
Element] are automatically sent to set up the instrument.
Alternatively, you may want to press the [Connect/Send Parameters] button in the [Connect to Instrument/Send
Parameters] page to perform the same operation.
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Chapter 3 Software Operation Flow and Basic Operation
1 Instrument information The models of the AA main unit, ASC and GFA, the ROM versions and
the machine identification numbers are displayed here. If neither ASC
nor GFA is connected, the ASC and GFA information is not displayed.
2 Automatic inspection These are inspections that the instrument performs automatically. If
points neither ASC nor GFA is connected, [Not Connected] ( ) is shown for
the [ASC Check] and [GFA Check] points.
NOTE
• The time required from the start of initialization to completion of the automatic inspection points is 4 to 5
minutes (it varies depending on whether or not options are installed).
• For the Fuel Gas Pressure Monitor Check, Support Gas Pressure Monitor Check, or Drain Sensor
Check item during the initialization, some messages may be displayed prompting you to check the
safety devices. These checks must be periodically performed to check that the safety devices operate
properly. When only the furnace measurement is performed, no check options are required. Click on the
[No] button for all the options and then proceed with the initialization.
(1) After all the items have been checked, a message may be displayed indicating that the fuel gas pressure
or the drain tank water level is low. Click on the [OK] button here.
(2) After the completion of the initialization, click on the [OK] button to close the [Initialize] screen.
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3.3 Software Basic Operation (Furnace Method)
If you click on the [Yes] button when the flame measurement is not to be performed, tick all the check items in
the Instrument Check List for Flame Analysis. This allows you to proceed forward to the next step.
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Chapter 3 Software Operation Flow and Basic Operation
NOTE
This page displays the wavelength, slit width, socket number, lamp current, lamp mode and so on. These
parameters are set for only the element that will be firstly measured (has been specified in the [Meas.
Element] field located in the lower right part of the [Element Select] page or the [Connect to Instrument/Send
Parameters] page).
The measurement parameters for each element are loaded from the cookbook and automatically specified
when the elements are selected.
Normally, you do not need to enter these measurement parameters. To modify them, however, you can enter a
value for the wavelength and select a value for other conditions from the list pulled down by clicking on the [T]
button. The lamp current value can be changed in units of 1 mA by clicking on the [S] or [T] buttons.
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3.3 Software Basic Operation (Furnace Method)
(1) Click on the [Next] button. A message will be displayed prompting you to do line search. Click on the [OK]
button.
The [Line Search/Beam Balance] dialog box will be displayed and the process will be carried out
automatically.
• First the line search (wavelength matching) is carried out and then the beam balance (gain
control for the detector) is performed. If only the beam balance is necessary, the line search is
not performed.
• In the line search, the highest peak near the specified wavelength is detected. In some cases,
however, the neon gas contained in the hollow cathode lamp radiates more intense light than
the light from the element. In such a case, if the correctly analyzed line is stored by clicking on
the [Wavelength Memory] button, its wavelength will be used for the subsequent line searches.
(2) Upon completion of the process, click on the [Close] button to proceed forward to the [Atomizer/Gas Flow
Rate Setup] page.
NOTE
When measuring multiple elements, you cannot set parameters for the elements other than the current
measurement one on the [Optics Parameters] and [Furnace Program] pages. If you use the ASC to measure
multiple elements automatically and you need to modify the parameters for other elements than the current
measurement one, you can change these parameters by using the [Edit Parameters] button in the [Element
Selection] page.
NOTE
SR lamp intensity is hard to stabilize in using NON-BGC mode or BGC-D2 mode in comparison with a
normal lamp. Before performing the line search, wait for 15 to 20 minutes after turning on the lamp, and then
start measurement.
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Chapter 3 Software Operation Flow and Basic Operation
When changing/creating a furnace program, you can save it so that you can use the same program next time.
For details, see 3.3.8.1 "Furnace Program Setup".
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3.3 Software Basic Operation (Furnace Method)
1
2
3
4
5
6
7
8
9
1 [Load]
To open the furnace program file, click on [Load]. The [Open] dialog box will appear. Then click on the
file name to be opened and click on [Open].
2 [Save]
To save the furnace program, click on [Save] and enter the file name on the [Save As] dialog box. The
extension for furnace program is ".fur" (For example, "copper.fur"). Then click on <Save>.
3 When editing a ready-made furnace program, use the [Insert Row] or [Delete Rows] buttons to insert
a row or delete rows.
4 [Coating/Boost Cycle] button
Coating refers to injecting a specified reagent into the furnace and drying it prior to the sample
injection (i.e., coating the tube surface). First, the checked mark reagent is injected in the furnace, and
heating is executed up to the furnace program stage specified in [Last Coating Cycle]. After this, the
sample is injected.
Furnace boost cycle refers to the repetitive cycle of sample injection into the furnace, and drying and
ashing of the sample in order to raise the concentration of the target element in the sample. Repeating
this boost cycle enables measurement of the sample whose concentration is lower than the
quantification range by concentrating it and raising its absorbance to the quantitative range of the
calibration curve.
5 Clicking on the [Test Meas.] starts the test measurement allowing you to check to see whether the
temperature program is appropriate. The peak profile of the measurement result will be displayed as a
graph on the screen.
6 Clicking on the [Cleaning] button displays the [Cleaning] dialog box. If you click on the [Start] button,
the graphite tube will be heated without a sample in accordance with the built-in heating program for
cleaning. Also use the [Test Meas.] as necessary.
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Chapter 3 Software Operation Flow and Basic Operation
7 Clicking on the [Change Graphite Tube] button displays the [Change Graphite Tube] dialog box.
8 Clicking on the [Temp. Search] button displays the [Optimum Furnace Program Search] dialog box.
This allows you to automatically carry out the operation of gradually changing the heating conditions
and plotting the resulting data as a graph on the screen. Accordingly, the optimum atomization and
ashing temperatures can be determined.
9 Clicking on the [Auto Zero] button shifts the current displayed value to zero.
(2) After completing all the settings, click on [Finish]. The Wizard finishes and the main window will appear.
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3.4 Saving the Template
3.4 Saving the Template
If you want to use the parameters set with the above procedures from the next time, you can save them as a
template. Then you can load it in the [Wizard Selection] dialog box.
(1) Click on [File] in the menu bar and select [Save As].
(2) Select "template (*.taa)" for [Save as type]. The extension of the file name displayed in [File name] is
changed to ".taa".
Example
If "notitle.aa" is displayed in [File name] when the [Save As] dialog box is opened, selecting "template
(*.taa)" changes the file name to "notitle.taa".
(3) Input the file name. Leave the extension as ".taa".
Example
Change the part "notitle" in the "notitle.taa" to a name you like.
(4) Press [Save] button. [Save As] dialog box is closed and the template file is saved.
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Chapter 3 Software Operation Flow and Basic Operation
3.5 Explanation of Main Window
1 Menu bar
2 Standard tool bar
3 Measurement element tool bar (Current measurement element)
4 Absorbance digital display
5 Real time graph (and temperature program graph)
6 Peak profile (latest four measurements and overlay display)
7 Calibration curve tool bar (Selection of calibration curve and type)
8 Calibration curve display
9 MRT work sheet
0 Function buttons
a Status bar
3 1 4 6 7 8
0 9 a
Fig. 3.78 Main Window
NOTE
While the [Properties] is opened from the right mouse button menu on the graph or MRT work sheet, the
measurement is stopped. In this case, the measurement can be continued again when the [Properties] is
closed.
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3.5 Explanation of Main Window
New : All the data and parameters are cancelled and parameters are set newly.
(Same as [File]-[New] in the menu bar)
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Chapter 3 Software Operation Flow and Basic Operation
3-80 AA-7000
3.5 Explanation of Main Window
1
2
3
4
5
1 [Properties]
[Real Time Graph Scale] (Flame)
You can change the graph ordinate and abscissa scale. Enter the maximum value and minimum value in
[Ordinate Max] and [Ordinate Min], respectively. Enter a numeric value in [Time Interval] (unit: second) for
abscissa. Clicking on [Reset] sets them to the values specified in [Parameters]-[Default Parameters]-
[Graph].
[Scale] (Furnace)
You can change the scales for [Absorbance], [Time] and [Temperature]. Enter the maximum value and
minimum value in [Max] and [Min], respectively. Clicking on [Reset] sets the absorbance scale to the
values specified in [Parameters]-[Default Parameters]-[Graph], and sets the time and temperature scales
according to the furnace program.
[Color]
You can select colors of [Data Line], [BG Line], [Background] and [Grid] (also [Furnace Program] for
furnace method). Click on the T and select the color from the list.
[Grid]
You can select grids to be displayed from [Major & Minor Grid], [Major Grid] or [None]. You can also select
the line type of [Major Grid Line] and [Minor Grid Line].
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Chapter 3 Software Operation Flow and Basic Operation
2 [Copy]
Executing [Copy] copies the image data of currently displayed graph to the clipboard. Then start up the
word processor or other application and move the cursor to the location where you want to paste the
graph. Select [Paste] command in the word processor, etc., and the graph will be displayed at the cursor
position.
3 [Cross Hair] (Furnace)
This is used to read coordinate values in the graph.
• Move the mouse cursor in the graph area first, then select [Cross Hair]-[Display] in the right
button menu. When the mouse cursor is in the graph area, the coordinate values at the cross
hair intersection position are displayed.
• While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross
Hair]-[Lock] will fix the cross hair at that position. To free the cross hair, click on the right mouse
button again and select [Cross Hair]-[Lock] (then the check mark of [Lock] will be deleted).
• While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross
Hair]-[Display] (then the check mark of [Display] will be deleted) will erase the cross hair
regardless of the [Lock] condition.
4 [Radar]
The display range is automatically set so as to display the entire graph selected by the mouse cursor.
5 [Print]
Selecting this opens the [Print] dialog box. Check the printer name, copies, etc. and click on [OK]. The real
time waveform currently displayed will be printed.
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3.5 Explanation of Main Window
1
2
3
4
5
6
1 [Properties]
[Scale]
You can set the maximum value [Max] and minimum value [Min] of the graph ordinate and abscissa scales.
The scale setting is used commonly for the five graphs. Clicking on [Reset] sets the Y-axis to the value
specified in [Parameters]-[Default Parameters]-[Graph].
[Color]
You can select colors of [Data Line], [BG Line], [Background] and [Grid]. Click on the T and select the
color from the list.
[Grid]
You can select grids to be displayed from [Major & Minor Grid], [Major Grid] or [None]. You can also select
the line type of [Major Grid Line] and [Minor Grid Line].
2 [Draw BG Line]
Selecting this displays a profile of background signal. The display is deleted by selecting this menu again
(The check mark of [Draw BG Line] is deleted).
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Chapter 3 Software Operation Flow and Basic Operation
3 [Copy]
Executing [Copy] copies the currently displayed graph to the clipboard. Then start up the word processor
or other application and move the cursor to the location where you want to paste the graph. Select [Paste]
command in the word processor, etc., and the graph will be displayed at the cursor position.
4 [Cross Hair]
This is used to read coordinate values in the graph.
• Move the mouse cursor in the graph area first, then select [Cross Hair]-[Display] from the right
button menu. When the mouse cursor is in the graph area, the coordinate values at the cross
hair intersection position are displayed.
The graph area is divided into five areas, and the coordinate values can be read only in each area.
• If you want to read an coordinate value in another graph, erase the cross hair cursor once by
clicking the right mouse button and selecting [Cross Hair]-[Display] (then the check mark of
[Display] will be deleted), then set the mouse cursor to another area and select Cursor]-
[Display] again.
• While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross
Hair]-[Lock] will fix the cross hair at that position. To free the cross hair, click on the right mouse
button again and select [Cross Hair]-[Lock] (then the check mark of [Lock] will be deleted).
• While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross
Hair]-[Display] (then the check mark of [Display] will be deleted) will erase the cross hair
regardless of the [Lock] condition.
5 [Radar]
This automatically sets the display range so that the selected graph by the mouse cursor is displayed in an
appropriate size. At the same time, other four data scales are also changed to the same scale.
6 [Print]
Move the mouse cursor to the graph area to be printed. Then the [Print] dialog box appears. Check the
printer name, copies, etc. and click on <OK>. Only the selected peak profile will be printed.
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3.5 Explanation of Main Window
Changing the condition and clicking on [OK] immediately recalculates the concentration of unknown samples
based on the new calibration curve and renews the quantification result on the MRT work sheet. The
recalculation is only applied to the unknown sample using the same C# as changed calibration curve. The result
is invalid when the element is different, or when the C# is different even if the element is same. In the case of
furnace method, whether the absorbance is obtained from the peak height or from the peak area is switched in
this window.
NOTE
After the validation based on the QA/QC setup is executed, the calibration curve order, zero intercept and
signal processing mode settings cannot be changed after the measurement. For details on QA/QC setup,
refer to the Chapter 6 "QA/QC Setup".
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Chapter 3 Software Operation Flow and Basic Operation
Symbol Meaning
Abs Absorbance
Conc. Concentration
r Correlation Coefficient
e When a coefficient is very small, this symbol is used to express it by using index.
"AeB" means "A × 10B"
Example
Calibration curve equation <1> means equation <2>.
Abs = -9.5e-005Conc^2 + 0.011636Conc + 0 ....................................... <1>
Abs = -9.5 × 10−5 × Conc2 + 0.011636 × Conc. + 0 .............................. <2>
1
2
3
4
5
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3.5 Explanation of Main Window
1 [Properties]
[Scale]
You can set the maximum value [Max] and minimum value [Min] of the graph ordinate and abscissa scales.
Enter the values.
[Options]
You can set the graph color and data point shape. Clicking on each [T] of [Data Point], [Calibration Curve],
[Background] and [Grid] displays the list from which you can select the color. The shape of [Data Point] can
be selected from the list displayed by clicking on the [T].
[Grid]
You can select grids to be displayed from [Major & Miner Grids], [Major Grid] or [None]. You can also select
the line type of [Major Grid Line] and [Minor Grid Line].
2 [Copy]
Executing [Copy] copies the currently displayed graph to the clipboard. Then start up the word processor
or other application and move the cursor to the location where you want to paste the graph. Select [Paste]
command in the word processor, etc., and the graph will be displayed at the cursor position.
3 [Cross Hair]
This is used to read coordinate values in the graph. Move the mouse cursor in the graph area first, then
select [Cross Hair]-[Display] from the right button menu. When the mouse cursor is in the graph area, the
coordinate values at the cross hair intersection position are displayed.
To erase the cross hair, select [Cross Hair]-[Display] (then the check mark of [Display] will be deleted).
While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross Hair]-
[Lock] will fix the cross hair at that position. To free the cross hair, click on the right mouse button again and
select [Cross Hair]-[Lock] (then the check mark of [Lock] will be deleted).
While the cross hair cursor is displayed, clicking on the right mouse button and selecting [Cross Hair]-
[Display] (then the check mark of [Display] will be deleted) will erase the cross hair regardless of the [Lock]
condition.
4 [Radar]
This automatically sets the display range so that the entire graph can be displayed.
5 [Print]
Move the mouse cursor to the graph area to be printed. Then the [Print] dialog box appears. Check the
printer name, copies, etc. and click on [OK]. Then the calibration curve currently displayed is printed out.
This menu is not displayed when no calibration curve exists.
NOTE
The currently measured element (or the element about to be measured) can be changed not by the tab at
the left lower of the main window but by the measurement element tool bar.
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[START] button : [F5], [F6] keys This switches to [STOP] button during measurement.
The relations between the current measurement mode and the available buttons are shown below. "Auto (using
ASC)" means the status where the ASC is connected and the [Using ASC] check box is check marked in
[Parameters]-[Edit Parameters]-[Sequence] page from the menu bar.
Flame Micro
Flame Continuous Sampling
Method Manual Flame Continuous Method Auto
Furnace Method (using ASC)
Operation Method Auto
Manual
Flame Micro (using ASC)
Furnace Method
Sampling Method
Auto (using ASC)
Manual
[AUTO ZERO]
[BLANK]
[START]
[TEST MEAS.]
[RINSE]
• Clicking on [AUTO ZERO] button executes the Auto Zero while rinsing the nozzle in the case of flame
continuous method auto (using ASC). In other cases, only the Auto Zero is executed.
• If you click on [Rinse] button, the nozzle is rinsed for the flame continuous method or the nozzle and mixing
port are rinsed for the flame micro sampling method and the furnace method (the mixing port is only rinsed
when the mixing ON option is selected.) The nozzle rinse time in flame continuous measurement is set in
[Configuration] dialog box opened by selecting [Instrument]-[Configuration] from the menu bar. If the
setting is "0", 10 seconds rinse is executed regardless the setting.
• Clicking on [STOP] stops the measurement. However, while acquiring the data, the measurement is
stopped after the data acquisition is finished.
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3.5 Explanation of Main Window
1 2 3 4 5 6 7 8
Fig. 3.88 Status Bar
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Chapter 3 Software Operation Flow and Basic Operation
3.6 Operating the MRT Work Sheet
In the MRT (Measurement Result Table) work sheet, the functions of setting of measurement sequence,
execution of measurement, result display, actual concentration calculation, and setting of ASC sample position
are integrated. For example, if you create a calibration curve by measuring three standard samples and
measure eight unknown samples, the measurement is proceeded in the following procedure.
As the measurement procedure, prepare the sample shown in the [Action] column and click on [START]. You
can proceed the measurement in the order from top row to down. When a repeat measurement is set, rows for
repetition are inserted at the time of measurement.
• [Action]
Clicking on the cell in this field opens the drop-down list, showing the following indications. This [Action]
field contains the measurement operations, operation using the ASC, QA/QC operation, etc.
For details, see 3.6.1.1 "Drop-down List of [Action]".
• [Sample ID]
In normal operation, sample ID is entered in this field. Sample name can be entered only when [Action]
field indicates measurement of standard sample or unknown sample (BLK, STD, UNK, LCS, SPK,
RESLOPE, MSA, SMSA, MSA-RES, ICV, CCV, ICB, CCB, PB, PDS, DUP, and CRA). When the [Action] is
CAL-CHK, the sample name cannot be entered.
If you previously enter Sample ID in the [Calibration Curve Setup] page or the [Sample Group Setup] page
and then execute [Edit]-[Insert Calibration Curve] or [Insert Sample Group] from the menu bar, the data on
rows of MRT worksheet can be given at a time. This eliminates the labor of entering data on each row.
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3.6 Operating the MRT Work Sheet
NOTE
In the following six cases, the [Sample ID] has a special meaning.
• When [RINSE] is set in flame continuous measurement (using ASC), enter the rinsing time in second
unit (0 to 600 seconds) in this [Sample ID].
• When [PAUSE] is set, enter the message to be displayed on the message dialog box in this [Sample
ID].
• When [WAIT] is set, enter the wait time of second unit in this [Sample ID] (0 to 7200 seconds).
• When [COMMAND] is set, describe the command line in this [Sample ID].
• When [FILESAVE] is set, enter the file name together with path to save the data measured so far (e.g.
C:\AA\WATER_CU.aa). Use ".aa" for extension.
• When [FILEEXPORT] is set, enter the file name together with path. Then the data on the MRT work
sheet data of the currently measured element is saved in a text file (e.g. C:\AA\WATER_CU.txt). Use
".txt" for extension.
• [Graph]
When overlaying the peak profiles, click on the right part of the cell and select the color of data lines from
the list. The overlaid profiles are displayed on the rightmost of peak profile area. On the other hand, the BG
lines are overlaid by the same one color.
• [X] (Exclusion)
Double-clicking this excludes the data in the row. The exclusion can be deselected if you double-click on
this button again.
• [M] (Modified)
Rewriting the sample ID and true value after measurement displays M mark (Modified). Once rewritten, this
check mark is always displayed and the original data cannot be recovered.
• [Q]
A mark is displayed for each row to which the QA/QC check selected in the [QC Blank/QC Standard Setup]
page or the [Sample Group QA/QC Setup] page has been applied.
Marked data cannot be excluded or modified.
• [True Value (and unit)]
The set concentration (and unit) of standard samples is indicated. This can be entered only when the
[Action] is STD, LSC, SPK, RESLOPE, MSA, ICV, CCV, PDS, and CRA. In the case of "SPK" and "PDS",
enter the added concentration.
• [Conc. (and Unit)]
Displays the result of concentration obtained with measurement. As the [True Value] column heading, the
unit specified in the [Calibration Curve Setup] page is automatically displayed.
• [Abs.]
Displays the measured absorbance. Energy intensity is displayed instead in the case of EMISSION mode.
If a blank measurement is executed prior to this, the value is indicated after the measured blank value is
subtracted from the actual measured value.
• [BG]
For measurement in BGC-D2 or BGC-SR mode, absorbance of background signal is displayed. This is not
displayed in the lamp modes in which the background signal is not acquired.
When "Peak Height" is selected for signal processing mode in furnace measurement, this field indicates
the background value at the time of acquisition of the absorbance signal peak height data.
AA-7000 3-91
Chapter 3 Software Operation Flow and Basic Operation
NOTE
The actual concentration is calculated using the equation: Actual concentration = (concentration) × VF × DF
× ASC DF × CF/WF. However, no functions are available for specifying the units of WF and VF. To convert
the units, use CF.
ASC Dilution Factor is a value used to prevent the actual dilution ratio from changing when the software
automatically modifies the mixing conditions due to the automatic dilution and remeasurement.
3-92 AA-7000
3.6 Operating the MRT Work Sheet
• [C#]
Indicates calibration curve number. When plural calibration curves are created on the same sheet, number
is put in the order of creation and indicated.
If entering a changed number, in the case of standard sample, a calibration curve is created by the
standard samples of the same curve number and in the case of unknown sample, the concentration is
calculated using the calibration curve of the entered number. This can be entered when the [Action] is
STD, UNK, CAL-CHK, LCS, SPK, RESLOPE, MSA, SMSA, MSA-RES, ICV, CCV, ICB, CCB, PB, PDS,
DUP or CRA.
This number is also used when selecting the calibration curve to be displayed (refer to the section 3.5.7
"Calibration Curve Display").
• [SG#]
Displays the sample group number.
• [Out of Control Remark]
A Note is displayed when QA/QC function judges that the acquired data is out of acceptance range.
• [Date]
Displays the date when the data was obtained by measurement.
• [Time]
Displays the time when the data was obtained by measurement. In the case of repeat measurement, the
time displayed in the average row is the time of the first measurement.
• [User Name]
Displays the user name who acquired the data.
• [Device Name]
Displays the device name used to acquired the data. The device name comes from [Instrument]-
[Configuration]-[Device Name].
BLK: Specifies the blank sample measurement. The blank measured value will be subtracted from
the measured values of standard or unknown samples until the next blank measurement is
executed.
AA-7000 3-93
Chapter 3 Software Operation Flow and Basic Operation
CAL-CHK: Specifies the evaluation of calibration curve after the standard sample measurement (the
correlation coefficient is checked). This is usually inserted to the row just after the last "STD".
In the case of standard addition method or simple standard addition method, this setting is
not necessary because this is checked in the "MSA-RES" row.
LCS: Specifies the measurement and evaluation by LCS (Laboratory Control Sample/Standard
substance).
SPK: Specifies the measurement and evaluation by SPK (Pre-Digestion Spike/ addition and
recovery check without pretreatment). This is usually inserted to the row just after the
objective "UNK".
RESLOPE: Specifies the measurement for sensitivity correction (Usually, the standard sample of highest
concentration is used). After this, "A, B, C..." is added to C# on the MRT and a new
calibration curve number (C#) is created.
SMSA: Specifies the unknown sample measurement by simple standard addition method.
MSA-RES: Specified as the result of standard addition method. When the measurement of a set of
standard addition samples is finished, the calibration curve is created and the result is
indicated in this row at the same time.
AUTOZERO: Shifts the current displayed value to zero. In the case of flame continuous method using the
ASC, the Auto Zero can be executed while aspirating the rinse solution. The aspirating time
(0 to 600 seconds) in second unit can be specified in [Sample ID] field.
RINSE: In the case of flame micro sampling method or furnace method, the nozzle and mixing port
are rinsed (mixing port is rinsed only when Mixing is ON). In the case of flame continuous
method, the nozzle is rinsed. When the ASC is used, the rinse time (0 to 600 seconds) in
second unit can be specified in [Sample ID] field.
PAUSE: Specifies temporary stop until the [OK] is selected. Input a message to be displayed on the
message dialog box in the [Sample ID] field.
WAIT: Specifies a stop in a fixed time. Input waiting time in the unit of second in the [Sample ID]
field (0~7200 seconds).
COMMAND: Specifies execution of command line. Specify the command to be executed in the [Sample
ID] field.
FILESAVE: Specifies the file saving of the data collected so far. Specify the file name in the [Sample ID]
field.
FILE Specifies the text file saving of the data collected so far on the MRT work sheet. Specify the
EXPORT: file name in the [Sample ID] field.
ICV, CCV, ICB, CCB, PB, PDS, DUP, and CRA also carry out the measurement and evaluation using each QC
sample as LCS and SPK do. Normally, insert PDS and DUP next to the targeted UNK.
3-94 AA-7000
3.6 Operating the MRT Work Sheet
NOTE
1. Executing "FILESAVE" overwrites and saves the file even if the file of the same name exists.
2. When the path name is not set at all in [FILESAVE] or [FILEEXPORT], a path name is created based on
the setting [File]-[Auto Save]. When only the file name is set, the file is saved in the folder that was used
in the last time for [Open] or [Save As] screen.
3. To enable the QA/QC actions, it is necessary to put a check mark in the check box of each QA/QC type
in the [QC Blank/QC Standard Setup] page and [Sample Group QA/QC Setup] page.
1
2
3
4
5
6
7
8
AA-7000 3-95
Chapter 3 Software Operation Flow and Basic Operation
1 [Properties]
[Table Show/Hide]
You can select to show or hide each column on the MRT work sheet. Only check marked items are
displayed. Click on the item you don't want to show, and erase the check mark. The show/hide selection for
each column has no relation to the print items in the [File]-[Print Table Data]. To select the items to be
printed in Table Print, select [File]-[Print Style] from the menu and select the items in [Table Show/Hide]
page.
When the ASC is set not to be used in the [Parameters]-[Edit Parameters]-[Sequence], the items related to
ASC such as [Pos.], [VOL], [Diluent], [Reagent 1], [Reagent 2], [Reagent 3], [Total Volume] and [ASC DF]
are not shown or printed, even if these items are set to be shown or printed in the [Table Show/Hide] page.
3-96 AA-7000
3.6 Operating the MRT Work Sheet
[Row Style]
Font (character style, size, etc.), color and ruled line type can be set for each row group (row and column
header, basic style, current row, measurement result row and excluded row).
2 [Hide Repetition]
When this is selected in the case of repeat measurement, only the row of average value is shown and the
rows of repeating process are not shown. The repetition rows are not printed in the "Print Table Data",
either. While this is selected, a check mark is indicated in the drop-down menu.
3 [Hide Excluded Row]
When this is selected, a row with a check mark in its [X] (excluded) field is not shown. The excluded rows
are not printed in the "Print Table Data", either.
4 [Hide Blank]
When this is selected, a row of blank measurement is not shown. The blank rows are not printed in the
"Print Table Data", either.
5 [Hide Command Row]
When this is selected, a row whose [Action] field is "Command" is not shown. The command rows are not
printed in the "Print Table Data", either.
6 [Keep Meas. Row Visible]
When this is selected, the MRT work sheet is automatically scrolled as the measurement proceeds so that
the row under measurement may be always displayed.
AA-7000 3-97
Chapter 3 Software Operation Flow and Basic Operation
(3) When completed, click on [OK] to close the [Collective Edit] dialog box. Settings are changed and the
actual concentration is recalculated simultaneously and the work sheet is renewed.
In rows already measured, however, [Volume] and [Coating] cannot be edited.
3-98 AA-7000
3.6 Operating the MRT Work Sheet
NOTE
Insertion and deletion of a row next to current measuring row cannot be done during measurement.
Home
This key moves the active cell to the leftmost cell that can be active in the current row.
End
This key moves the active cell to the rightmost cell that can be active in the current row.
Ctrl+Home
These keys move the active cell to the leftmost cell that can be active in the first row unexecuted.
Ctrl+End
These keys move the active cell to the rightmost cell that can be active in the last measurement row.
Tab
This key moves the active cell to the right. After moving to the rightmost cell, it moves to the leftmost cell in
the next row below. It skips a cell that cannot be activated and moves to the next cell.
Shift+Tab
These keys move the active cell to the left. After moving to the leftmost cell, it moves to the rightmost cell in
the upper row. It skips a cell that cannot be activated and moves to the next cell.
AA-7000 3-99
Chapter 3 Software Operation Flow and Basic Operation
Cell range
Click the cell in the upper left corner of the region to be selected and drag to the cell in the lower right
corner.
Column
When selecting a column, click the column header of the column to be selected. When selecting
contiguous plural columns, drag along the column header.
Row
When selecting a row, click the row header of the row to be selected. When selecting contiguous plural
rows, drag along the row header.
Whole table
Click the upper left cell of the header. Then all of the rows entered on the table are selected.
3.6.6.1 Copy
Select an area on the worksheet to be copied using the mouse and select [Edit]-[Copy] menu or press [Ctrl] +
[C] key. Then the values in the selected area are copied to the clipboard. These copied values can be pasted as
text data to the word processor or spreadsheet software.
NOTE
• The contents of column header and row header are not copied.
• Graph column is never copied.
• Hidden column is not copied.
• Hidden row included in the selected area is always copied.
3.6.6.2 Paste
Text data can be pasted from the clipboard to the sample ID column.
3-100 AA-7000
3.6 Operating the MRT Work Sheet
(4) When the number of sample ID in the copy source is over the number of rows in the paste destination, the
excess are added as new rows.
NOTE
• If a value other than numeric value is pasted to the items for which should be set in the sample ID field
(WAIT, AUTO ZERO or RINSE at the use of ASC), it is reset to "0". Numeric values out of the
acceptable entry range are also ignored.
• If the paste is applied to the items for which nothing can be entered in sample ID field (CAL-CHK, etc.),
it is ignored.
• Also, sample IDs created using word processor or spreadsheet software can be pasted to the MRT
worksheet. When creating sample IDs using a word processor, insert a line feed between the sample
IDs. Also, the sample ID must not contain the tab code.
AA-7000 3-101
Chapter 3 Software Operation Flow and Basic Operation
3-102 AA-7000
Chapter 4
Measurement Procedures
After completing all the settings, prepare the samples. Perform the measurement following the
procedure indicated on the MRT work sheet. The current row is highlighted and its [Action] field
shows the type of measurement. When using the ASC, set the samples in proper positions.
If no setting is made on the MRT work sheet, a message appears to indicate that no schedule
exists. In this case, select [Parameters]-[Schedule Creation Wizard] from the menu and set the
measurement procedures.
NOTE
If a menu or dialog box is kept opened during the measurement operation, the measurement
operation may be interrupted. Be careful about it when checking the setup parameters during
the operation.
CONTENTS
AA-7000 4-1
Chapter 4 Measurement Procedures
4.1 Measurement Operation (for Flame Method)
In the case of flame methods (Flame Continuous Method and Flame Micro Sampling Method), read 4.5 "Igniting
and Extinguishing the Flame" thoroughly before starting the measurement. Confirm that the gases are supplied
at correct pressures and the burner head is mounted properly. If the lamp warm-up time (unit: minute) is set,
you may not start the measurement during the time after lighting on the lamp.
NOTE
If the "AUTO ZERO" line has already been set in the MRT worksheet, press [START] (or the [F5]/[F6] key).
NOTE
• When the "BLANK" row is prepared on the MRT worksheet beforehand, press [START] (or [F5]/[F6]
key).
• If the standard or unknown samples are measured after executing the blank measurement, their
measured values (absorbance or energy) are indicated after the measured blank value is subtracted
from their actual measured values. The difference between this measured blank value and the actual
measured standard or unknown sample value is displayed in [Abs] (or [Energy]) on the MRT until the
next blank measurement is executed.
4-2 AA-7000
4.1 Measurement Operation (for Flame Method)
4. If you want to change the order or other parameters for calibration curve, click on [Type] above the
calibration curve graph then make a change on the [Change Calibration Curve Condition] dialog box.
(6) Unknown Sample Measurement
1. Spray the unknown sample. Click on [START] at the bottom of the Main window (or press the [F5] or
[F6] key).
2. If the repeat measurement is selected, clicking on [START] inserts a new row for repeat measurement
according to the set repeat parameters.
3. Repeat the measurement following the row indication. Then continue to measure the unknown
samples according to the specified order. Measure an unknown sample while checking that it accords
with the current row on the window.
NOTE
If [START] key is pressed when all the rows on the MRT work sheet have been executed, a new "UNK" row
(unknown sample row) is added and its measurement result is displayed.
When the "Auto Blank" is ticked in the [Calibration Curve Setup] page, a blank measurement is inserted in
the specified interval. Spray the blank and measure it.
If you want to make the size of MRT work sheet larger, set the mouse cursor onto the upper border of the
table to indicate an arrow with two directions. Press down the mouse left button and drag it to specify the
range. More number of rows can be displayed. For details on changing sizes or using a scroll bar, refer to the
Windows documentation.
NOTE
When using the ASC, put a check mark in the check box of [Using ASC] in the [Sequence] page of [Edit
parameters] property sheet.
When using the ASC, verify that the position of each actual sample on the ASC turntable accords with the
setting on the MRT work sheet.
(1) Igniting the Flame
Press the IGNITE button and the PURGE button on the front of the AA main unit to ignite the flame.
(2) Starting the Measurement
Click on [START] at the bottom of the Main window (or press the [F5] or [F6] key). The automatic
measurement is started with the ASC.
(3) Extinguishing the Flame
After finishing the measurement, press the EXTINGUISH button on the front of the AA main unit to
extinguish the flame (A flame is automatically extinguished if the automatic flame extinction is selected).
(4) Checking the MRT work sheet
Check the measured results on the MRT work sheet. If a remeasurement is necessary, refer to the section
3.6 "Operating the MRT Work Sheet". When printing or saving the data, proceed to the section 4.4 "Saving
and Printing the Data".
AA-7000 4-3
Chapter 4 Measurement Procedures
NOTE
When performing measurement in the flame method, you might find the absorbance value displayed as "-1".
This tends to occur in case that there is strong emission of light from flame, such as N2O-C2H2 flame or
flame in spraying the sample such as Na, K, etc., although it depends on a target element, sample
concentration and flame condition.
If such is the case, carry out countermeasures in order as indicated below.
Note that if "-1" absorbance value is no longer displayed after spraying the sample, start measurement
without taking other countermeasures.
• In BGC-D2 mode, confirm whether the hollow cathode lamp beam and D2 lamp beam meat at the
burner. If not, adjust D2 lamp position in accordance with 8.8.2 "Replacing Procedures of Deuterium
Lamp".
• Perform the line search and beam balance while spraying the blank sample.
• Perform the line search and beam balance while spraying the standard sample with the highest
concentration. Then, execute AUTO ZERO while spraying the blank sample.
If the concentration of the standard sample is too high, signal becomes noisy in measuring the low-
concentration sample.
• Reduce fuel gas flow rate or change the burner angle, and perform the line search and beam balance.
Note that this procedure results in deteriorating the sensitivity.
4-4 AA-7000
4.2 Measurement Operation (for Furnace Method)
4.2 Measurement Operation (for Furnace Method)
NOTE
Note that heating is performed when the temperature calibration is executed.
(5) After the temperature calibration has been finished, the message "Inject a sample." should appear. Using a
pipette or the like, inject the sample into the graphite tube.
(6) After the sample has been injected, click on the [OK] button in the message dialog box. The measurement
will be started.
AA-7000 4-5
Chapter 4 Measurement Procedures
4.3 Completing the Measurement
(1) When the measurement is completed, verify that the flame is extinguished and tighten the main valve of
the gas cylinder and compressor in the case of flame method. Close the main valves of the cooling water
and gas in the case of furnace method.
(2) Quit the software. For example, select [File]-[Exit] from the menu bar.
NOTE
The communication with the instrument is shut off first, and then the main window is closed. It takes
approximately 30 seconds.
NOTE
When using the GFA-7000, be sure to turn off the HEAT switch.
4-6 AA-7000
4.4 Saving and Printing the Data
4.4 Saving and Printing the Data
NOTE
A measurement data whose repeat measurement has not finished is not saved in the file. If the data is
necessary although the repeat measurement cannot be completed, print it out before ending the AA
software.
AA-7000 4-7
Chapter 4 Measurement Procedures
(3) After the print settings have been completed, click on [OK].
4-8 AA-7000
4.4 Saving and Printing the Data
[Print Data/Parameters]
The measurement parameters and measured data are printed.
AA-7000 4-9
Chapter 4 Measurement Procedures
4.5 Igniting and Extinguishing the Flame
Support gas Air, Nitrous oxide (N2O) 0.35 MPa ± 0.03 MPa
The above supply pressure must be kept during flame combustion.
(3) Confirm visually that the drain tank is filled with water.
When supplying water to the drain tank, refer to 2.8 "Supplying Water to the Drain Tank (AA-7000F)".
Drain tank
If the front panel and chimney have been removed, mount them as they were originally.
For details, see 2.4 "Removing and Mounting the Front Panel" and 2.5 "Removing and Mounting the
Chimney (AA-7000F)".
(4) Verify that there are no leaks in any of the gas lines (Refer to the section 8.5 "Checking for Gas Leaks" on
the Chapter 8 "Maintenance").
(5) Verify that the flame and burner head to be used are appropriately matched.
4-10 AA-7000
4.5 Igniting and Extinguishing the Flame
NOTE
The flow rate of support gas is fixed (at 15 L/min).
If the flow meter kit (optional) is installed, set the flow rate of the support gas to the value indicated below.
(2) Simultaneously press two buttons, IGNITE and PURGE. The pilot flame will be ignited and then the burner
head is ignited.
1. Keep pressing the IGNITE button until the flame is completely ignited. If the flame does not ignite even
if the buttons are pressed for ten seconds or more, the igniting operation is automatically stopped.
2. Retry after releasing the buttons for ten seconds or more.
NOTE
• If ignition fails, the AA software may display a message such as "Flame has been extinguished". If such
a message is displayed, the AA instrument is locked so that ignition is not possible. To release this lock,
close all of the error messages.
• If you cannot ignite the flame, see 9.1 "Failure to Ignite".
(3) After the flame is ignited, confirm the settings of the fuel gas pressure and flow rate, and support gas
pressure.
NOTE
If the flow meter kit (optional) is installed, you can also check the setting for the support gas flow rate.
AA-7000 4-11
Chapter 4 Measurement Procedures
NOTE
• After the flame has been extinguished a gas leakage inspection is automatically started, but the flame
can be re-ignited by pressing the IGNITE and PURGE buttons.
• If the gas pressure decreases while the flame is burning, the flame is automatically extinguished. In that
case, check the gas supply pressure before igniting the flame again.
• If a momentary AC supply power outage should occur, the flame is automatically extinguished.
• When the following error messages are displayed on the AA software, the AA main unit is locked so that
the ignition cannot be done. To release this lock, solve the problems in the instrument settings then
close all the error messages displayed on the software. While the error message is displayed, the
ignition cannot be done.
a. Fuel gas pressure is too low.
b. Support gas pressure is too low.
c. Flame has been extinguished.
d. Drain tank water level is too low.
e. Momentary electric shutdown occurred in the gas controller.
f. Vibration was detected by the instrument.
• If the flame should not be extinguished even by pressing the EXTINGUISH button, do NOT panic and
take action of following operation.
1. Turn off the main unit POWER switch (on the right side of the main unit). This operation
mechanically closes the solenoid valve of the gas controller, shutting off the gas supply safely.
2. Close the gas main valve.
3. Contact your service representative immediately. Do NOT operate the instrument until the repair by
service person completes.
4-12 AA-7000
4.5 Igniting and Extinguishing the Flame
NOTE
The flow rate of support gas is fixed (at 11 L/min).
If the flow meter kit (optional) is installed, set the flow rate of the support gas to the value indicated below.
(4) Press the ignition buttons (PURGE and IGNITE) at the same time to ignite the flame.
First, the Air-C2H2 flame will be ignited.
Approx. 10 seconds after the flame ignition is achieved, the C2H2 flow rate is automatically increased 5.0 L/
min and the flame emission intensity is increased. Then the support gas is automatically switched from Air
to N2O, changing the Air-C2H2 flame to N2O-C2H2 flame.
1. Keep pressing the IGNITE button until the flame is completely ignited. If the flame does not ignite even
if the buttons are pressed for ten seconds or more, the igniting operation is automatically stopped.
2. Retry after releasing the buttons for ten seconds or more.
NOTE
• If ignition fails, the AA software may display a message such as "Flame has been extinguished". If such
a message is displayed, the AA instrument is locked so that ignition is not possible. To release this lock,
close all of the error messages.
• Even if the [Flame Type] is set to N2O-C2H2, the flame will not be switched unless the BURNER
SELECT switch is set to N2O-C2H2 with a key attached to the high temperature burner head. In this
case, if the BURNER SELECT switch is changed from the Air-C2H2 to the N2O-C2H2 position while the
Air-C2H2 flame is combusting, the support gas is automatically switched from Air to N2O, changing the
Air-C2H2 flame to N2O-C2H2 flame.
• If you cannot ignite the flame, see 9.1 "Failure to Ignite".
AA-7000 4-13
Chapter 4 Measurement Procedures
(5) After the flame is ignited, confirm the settings of the fuel gas pressure and flow rate, and support gas
pressure.
NOTE
If the flow meter kit (option) is installed, you can also check the setting for the support gas flow rate.
(6) To extinguish the flame, press the EXTINGUISH button. The support gas is automatically switched from
N2O to Air, changing the N2O-C2H2 flame to Air-C2H2 flame. Then the flame is extinguished.
NOTE
• After the flame has been extinguished a gas leakage inspection is automatically started, but the flame
can be re-ignited by pressing the IGNITE and PURGE buttons.
• If the gas pressure decreases while the flame is burning, the flame is automatically extinguished. In that
case, check the gas supply pressure before igniting the flame again.
• If a momentary AC supply power outage should occur, the flame is automatically extinguished.
• When the following error messages are displayed on the AA software, the AA main unit is locked so that
the ignition cannot be done. To release this lock, solve the problems in the instrument settings then
close all the error messages displayed on the software. While the error message is displayed, the
ignition cannot be done.
a. Fuel gas pressure is too low.
b. Support gas pressure is too low.
c. Flame has been extinguished.
d. Drain tank water level is too low.
e. Momentary electric shutdown occurred in the gas controller.
f. Vibration was detected by the instrument.
• If the flame should not be extinguished even by pressing the EXTINGUISH button, do NOT panic and
take action of following operation.
1. Turn off the main unit POWER switch (on the right side of the main unit). This operation
mechanically closes the solenoid valve of the gas controller, shutting off the gas supply safely.
2. Close the gas main valve.
3. Contact your service representative immediately. Do NOT operate the instrument until the repair by
service person completes.
4-14 AA-7000
4.5 Igniting and Extinguishing the Flame
CAUTION
1. Always use high temperature burner head when using a nitrous oxide-acetylene flame. Using the
standard burner head with this gas causes a danger of flashback.
2. When the acetylene flow rate is high, carbon is deposited around the burner slot. When this occurs, use
the provided large screwdriver to scrap off the carbon deposit while taking care about the following
points.
Insert the screwdriver at the center on the burner slot while keeping the top portion of the screwdriver
lengthwise. Don't close a large part of the burner slot by keeping the top portion of screwdriver
horizontally.
While keeping the top portion of screwdriver lengthwise, slide it from the center to the outside (right or
left side) and scrap off the carbon deposit gently. To prevent the flame from going out, don't slide the
screwdriver from the outside to the center. Insert it at the center again and scrap off to the outside.
Be careful not to scratch the burner head and slot.
Remove the carbon deposit inside the burner slot using a piece of hard paper, after the flame is
extinguished and the burner is completely cooled.
Carbon deposit
3. When using a nitrous oxide-acetylene, decreasing the acetylene or increasing the nitrous oxide will
cause the pink portion of the flame (red feather) to gradually decrease. If this decreases to less than
2 mm, the flame will split, and if the acetylene flow is further reduced, a flashback may occur.
Therefore, control the gas flow rate so that the red feather does not become shorter than 2 mm.
Blue
AA-7000 4-15
Chapter 4 Measurement Procedures
CAUTION
If flashback should occur, perform the checks in accordance with "Measures When Flashback Occurs" on
the yellow pages.
WARNING
• Check that the parts of the atomizer are resistant to the chemicals used.
See 10.1.2 "Flame Specifications".
Since an organic solvent itself will burn in the flame, the flame will not be completely combusted using the
normal flame conditions, as the result, the measurement accuracy will be decreased. To perform an accurate
measurement, it is necessary to decrease the sample spray amount as well as decrease the acetylene gas flow
rate, compared with the aqueous solution. The procedure for setting the flame conditions when using organic
solvent is as follows.
(1) Replace the suction nozzle with the provided polyethylene capillary tube.
(2) While solvent is being sprayed into the flame, decrease the acetylene gas flow rate so that the color of the
flame is from blue or slightly red (in the case of air-acetylene flame).
(3) While organic sample is being sprayed, try various acetylene flow rates and burner heights until the
maximum S/N ratio (signal to noise ratio) is achieved.
NOTE
Overly decreasing the acetylene flow may cause the flame to go out when spraying of the organic sample is
stopped. In this situation, increase the acetylene gas flow rate in 0.1 L/min increments until the flame no
longer goes out at the end of spraying the organic solvent sample, and then adjust the flame condition by
increasing the support gas flow rate. To use flame of N2O-C2H2, ensure that the pink portion of the flame
(red feather) does not become shorter than 2 mm even if solvent spraying is stopped.
4-16 AA-7000
4.6 Standard Addition Method and Simple Standard Addition
4.6 Standard Addition Method and Simple Method
Standard Addition Method
The standard addition method is used when there is interference by coexistent material (matrix) in the sample
and its influence is given to the measured value. For the standard addition method, equal volumes of unknown
sample solution are prepared, and a standard solution of different but known concentration is added to each of
the unknown sample solutions. The absorbance is measured for each of these samples, and a calibration curve
is created. The unknown sample concentration is obtained from the point at which the extended calibration
curve intersects with the horizontal axis.
Absorbance
Standard addition
Concentration of unknown sample
When the coexistent material or matrix of plural unknown samples are similar, measure one of them by
standard addition method, and you can use the slope of the same calibration curve to determine the
concentrations of other unknown samples. This is called simple standard addition method.
Absorbance
AA-7000 4-17
Chapter 4 Measurement Procedures
NOTE
When the ASC is used, the [Pos.] field is displayed, but does not accept input. Leave the field blank.
(5) Click on the [OK] button in the [Calibration Curve Setup] page. The [Preparation Parameters] page will be
displayed.
(6) Click on the [Sample Group Setup] button. The [Sample Group Setup] page will be opened.
(7) Enter values for [Weight Factor], [Volume Factor], [Dilution Factor] and [Correction Factor] in the [Weight
Correction Factors] section.
(8) Enter a value in [No. of Samples] under the [Unknown/Spike Measurement Sequence] section and click on
[Update] button. The table will be displayed with the corresponding number of rows. Enter [Sample ID] and
[WF] as necessary.
NOTE
When the ASC is used, the [Pos.] field is also displayed. In the standard addition method, there are multiple
standard added samples for a single unknown sample. In this field, enter the position of the standard added
sample of the smallest added concentration.
(9) After finishing the settings, click on the [OK] button. You will return to the [Preparation Parameters] page.
NOTE
• To measure multiple elements, similarly enter the settings for the other elements.
When the wizard is completed, the measurement procedure specified in the [Preparation Parameters]
page is inserted into the MRT worksheet. Check that the measurement procedures for the calibration
curves in the same number as that of unknown samples have been created and automatically given C#
(calibration curve numbers).
• When the ASC is used, the same value is included in the [Pos.] field for the standard added samples for
a single unknown sample. Manually change it to a correct value on the MRT worksheet.
4-18 AA-7000
4.6 Standard Addition Method and Simple Standard Addition
Method
NOTE
In the standard addition method, you may wish to have multiple sample groups in the [Sample Group Setup]
page box, but no SG# (sample group number) can be given to the actual sample information.
NOTE
When the ASC is used, the [Pos.] field is displayed, but does not accept input. Leave the field blank.
(5) To automatically add standard samples to mix them using the ASC, enter data in the [VOL], [Diluent], ...,
[Reagent 3] fields. Specify each standard sample as [Reagent 3].
(6) Click on the [OK] button in the [Calibration Curve Setup] page. The [Preparation Parameters] page will be
displayed. Click on the [Sample Group Setup] button. The [Sample Group Setup] page will be opened.
(7) Enter values for [Weight Factor], [Volume Factor], [Dilution Factor] and [Correction Factor] in the [Weight
Correction Factors] section.
In the standard addition method, the settings for [Unknown/Spike Preparation Parameters] are irrelevant.
Leave them the default values.
(8) Enter a value in [No. of Samples] under the [Unknown/Spike Measurement Sequence] section and click on
[Update] button. The table will be displayed with the corresponding number of rows. Enter [Sample ID] and
[WF] as necessary. When the ASC is used, also enter a correct value in the [Pos.] field.
(9) After finishing the settings, click on the [OK] button. You will return to the [Preparation Parameters] page.
NOTE
• To measure multiple elements, similarly enter the settings for the other elements.
When the wizard is completed, the measurement procedure specified in the [Preparation Parameters]
page is inserted into the MRT worksheet. Check that the measurement procedures for the calibration
curves in the same number as that of unknown samples have been created and automatically given C#
(calibration curve numbers).
• When standard added samples are previously supplied, i.e., when no standard samples are
automatically mixed with the ASC, manually change the value in the [Pos.] field on the MRT worksheet
as described in the above paragraph "In the case of flame continuous method".
NOTE
In the standard addition method, you may wish to have multiple sample groups in the [Sample Group Setup]
page box, but no SG# (sample group number) can be given to the actual sample information.
AA-7000 4-19
Chapter 4 Measurement Procedures
NOTE
The C# (calibration curve number) that is automatically given here is increased by 1 from the C# of the
previous calibration curve. However, manually change it to the C# of the previous calibration curve. Repeat
the operations for "SMSA" settings by the number of unknown samples.
(4) After the settings for [Action] have been finished, enter data in the [Pos.], [Weight Factor], [Volume Factor],
[Dilution Factor], [Correction Factor] etc. The input operation will become easier if you drag the cursor on
the MRT worksheet to define a range, click on the right mouse button, and then use the [Collective Edit]
function.
NOTE
In the simple standard addition method, no SG# (sample group number) can be given to the sample
information.
Example
In this example, the ASC is used to add the standard samples of 0 ppb, 10 ppb, 20 ppb and 30 ppb to the
unknown samples, which are being diluted 5 times. Standard sample of 100 ppb is prepared for addition
and is regarded as the Reagent 3.
As other conditions, assume that [Mixing] is to be performed; [Injection Volume] is 20 μL, and [No. of
repetition] is 3 ([Max No. of repetition] is 5).
The [Sample] must be constant for all the concentrations. Here, assume it is 40 (μL).
0 40 160 0 0 0 200
10 40 140 0 0 20 200
20 40 120 0 0 40 200
30 40 100 0 0 60 200
4-20 AA-7000
4.6 Standard Addition Method and Simple Standard Addition
Method
Assume that there are unknown samples B and C, which have similar matrix components to that of unknown
sample A in the above setup example. These concentrations are calculated using the calibration curve created
by unknown sample A (simple standard addition method). In this case, since the [Sample] is 40 μL and the
[Total Vol] is 200 μL, the [Unknown Sample] preparation parameters are set as below.
40 160 0 0 0 200
In the [Weight Correction Factors] section, enter 40 (μL) in [Weight Factor] and 200 (μL) in [Volume Factor].
Then the actual concentration before dilution can be calculated.
AA-7000 4-21
Chapter 4 Measurement Procedures
MSA-RES : Indicates the concentration of unknown sample calculated from the result of measuring a set of
standard addition samples.
SMSA : Indicates simple standard addition method. Unknown sample is measured using a calibration
curve created by another sample for standard addition method.
When samples A, B, and C are being measured by the standard addition method, three calibration curves will
be created. When MSA is added to the MRT worksheet, C# (calibration curve numbers) are allocated
automatically. Check that C# correctly correspond to the series of standard samples in the standard addition
method.
Table 4.3 Measurement sequence for standard addition method
Assume that there are unknown samples B and C that contain similar components to those of unknown sample
A. To obtain their concentrations from the calibration created with unknown sample A, the following
measurement sequence is used:
4-22 AA-7000
4.6 Standard Addition Method and Simple Standard Addition
Method
AA-7000 4-23
Chapter 4 Measurement Procedures
4.7 Conditions and Operation for Flame Emission
Analysis
Flame emission quantitative analysis is described here. As the case of atomic absorption analysis, the Wizard
can be used for setup. However, the setup procedures in the [Optics Parameters] and [Atomizer/Gas Flow Rate
Setup] pages are different in some points. Other operations are the same as those of the flame continuous
method of atomic absorption analysis.
2 5
3
6
4
1 [Wavelength]
For wavelength used for flame emission analysis, refer to Table 4.5. Enter the numeric value if the
wavelength is different from that for atomic absorption analysis.
2 [Slit Width]
Normally, this value is 0.2 nm, but use 0.7 nm if there is a problem with baseline drifts.
3 [Lamp Mode]
Set the [Lamp Mode] to "EMISSION".
4 [Socket #]
Although a lamp is not used, it is necessary to set an arbitrary socket number as a dummy.
(Procedure for dummy setup)
1. Press the [Lamp Pos. Setup] button to display the [Lamp Position Setup] dialog box.
2. For an arbitrary [Socket #], select " * " in the [Element] and "Normal" in the [Lamp Type].
3. Select [Emission] in [Lamp ID]. This lamp ID is a special ID of dummy lamp for flame emission
analysis.
4. Press [OK] to close the [Lamp Position Setup] dialog box and return to the [Optics Parameters] page.
Then select the socket # in which the dummy lamp for flame emission analysis was set.
When performing the line search using a lamp, set a proper lamp in [Lamp Position Setup] dialog box.
4-24 AA-7000
4.7 Conditions and Operation for Flame Emission Analysis
5 [Lamp Current]
Set the [Low] to "0" (zero). When the lamp mode is set to "EMISSION", the [High] is automatically set to "0"
(zero) and cannot be entered.
6 [ASC Sample Pos. for EMISSION Line Search]
If the sample position of the highest concentration standard sample on the ASC turntable is set, automatic
spray using the ASC is possible.
7 [Line Search]
In the case of flame emission analysis, a line search has to be performed when the flame has been ignited
and the standard sample is being sprayed. So, the line search should not be performed at first. Proceed to
the next [Atomizer/Gas Flow Rate Setup] page first and set the parameters so that ignition can be possible.
After that, return to this page to perform the line search.
It is also possible to perform a line search using the hollow cathode lamp. In this case, light on the hollow
cathode lamp to perform the line search. If the lamp is lit on in the EMISSION mode, the lamp is
automatically turned off when the [START] key is pressed to start the measurement. Don't forget to turn off
the lamp, however, when observing a signal in the [Atomizer/Gas Flow Rate Setup] page while aspirating
the sample.
AA-7000 4-25
Chapter 4 Measurement Procedures
Table 4.5 Analysis Line Wavelength Table for Flame Emission Analysis
Ge 265.1 Rb 794.8
* Band spectrum
4-26 AA-7000
4.7 Conditions and Operation for Flame Emission Analysis
1
2
Fig. 4.11 [Atomizer/Gas Flow Rate Setup] Page (in the case of [Gas Flow Rate])
1 [Flame Type]
Since the flame used for atomic absorption analysis is indicated, click on the [T] and select the flame
type used for flame emission analysis. As a flame type used for flame emission analysis, generally,
the high temperature N2O-C2H2 flame is good. However, in the cases of alkaline metals (Na, K, etc.),
other flame (Air-C2H2) is also available for measurement of sufficiently minute quantities.
AA-7000 4-27
Chapter 4 Measurement Procedures
(2) Select the [Atomizer Position] for [Operation Object] by clicking on the radio button.
Fig. 4.12 [Atomizer/Gas Flow Rate Setup] Page (in the case of [Atomizer Position])
1 [Burner Height]
Since the value for atomic absorption analysis is indicated by default, enter the optimum value for
flame emission analysis. If the optimum value is not known, as a first step, set it to 7 mm for Air-C2H2
and 11 mm for N2O-C2H2. Then, after spraying the standard sample and performing the line search,
obtain the optimum value again.
To obtain the optimum burner position, the function of [Burner Position Auto] button is convenient.
2 [Burner Angle]
After adjusting the angle of the burner head, you can record the reading on the scale.
Generally, the S/N ratio is better when the angle is set at 0 degree for optical axis (parallel) than at
90 degrees, but its linearity may become worse. When the concentration of analysis element is
relatively high, the burner head is used at 90 degrees.
4-28 AA-7000
4.7 Conditions and Operation for Flame Emission Analysis
NOTE
When the ASC is used, the spray of the sample in the specified position on the ASC turntable is started
before starting the line search/beam balance. The line search/beam balance is started when the pre-spray
time set in the [Parameters]-[Edit Parameters]-[Measurement Parameters] is finished after starting the spray.
(4) If the line search fails and the message stating insufficient energy is displayed, prepare and spray a
standard sample of even higher concentration and try it again.
(5) When the line search is completed, click on [Close] to return to the [Optics Parameters] page. Then click
on [Next] button to proceed to the [Atomizer/Gas Flow Rate Setup] page again. While monitoring the real
time graph on the [Atomizer/Gas Flow Rate Setup] page, spray distilled water and check that the signal
becomes almost zero.
NOTE
If the signal does not become small, it is possible that the analysis line was not correctly detected. In that
case, go back to the [Optics Parameters] page and perform the line search once again following the
procedures (1) to (5).
AA-7000 4-29
Chapter 4 Measurement Procedures
In order to perform wavelength shift, select [Instrument] - [Set Wavelength to Background WL] from the menu.
When no line search has been conducted, only wavelength editing is valid.
1 6
2
7
3
4 5
Fig. 4.13 [Set Wavelength to Background WL] Dialog Box
1 [Current Set Wavelength] The currently set wavelength (nm) is indicated here.
If the instrument settings have not been made, "----" is displayed.
2 [Ca] Shifts the wavelength for Ca to the wavelength shown to the right of this
button (default: 430 nm).
3 [Na] Shifts the wavelength for Na to the wavelength shown to the right of this
button (default: 580 nm).
4 [Sr] Shifts the wavelength for Sr to the wavelength shown to the right of this
button (default: 458 nm).
5 [K] Shifts the wavelength for K to the wavelength shown to the right of this
button (default: 760 nm).
6 [Set Back to Original WL] Returns the wavelength to the setting before the wavelength was
shifted.
7 [Edit Background WL] Displays the screen on which the wavelength to be shifted can be
edited.
4-30 AA-7000
4.8 Specifying Optimal Conditions for Flame
4.8 Specifying Optimal Conditions for Flame
In the atomic absorption analysis, the [Fuel Gas Flow Rate] and [Burner Height] affect the absorption sensitivity.
Although standard values are automatically set as default values by selecting an element, the optimum
condition may differ depending on the sample characteristics and matrix components.
The "Optimum Burner Height Search" and "Optimum Gas Flow Rate Search" are the functions to search the
optimum conditions by the measurement while changing the burner height or gas flow rate automatically. In this
section, the operation procedures are described. For the details of each item in the window, refer to the HELP
information in the WizAArd software.
In addition, read the section 4.5 "Igniting and Extinguishing the Flame" thoroughly and set the conditions for
ignition.
1. Set the [Start] and [End] of the burner position search range. Although the available search range is
within 5 to 23 (mm), you may set the range 5 to 10 (mm) for Air-C2H2 and 8 to 14 (mm) for N2O-C2H2.
2. Press the PURGE button and IGNITE button on the front side of AA main unit to ignite a flame.
3. Start spraying the blank solution and click on [Blank Meas.] button. The measurement is performed
while the burner height is changed by 0.5 mm step in the selected range. Continue to spray it until the
measurement is completed.
4. Next, start spraying the standard (or sample) solution and click on [STD Meas.] button. In the same
way as blank measurement, the measurement is performed while the burner height is changed.
Continue to spray it until the measurement is completed.
The dialog box displays the graph which is created by subtracting the measurement result of <3> from
the measurement result here. And the burner height with which the absorbance becomes the highest
is also displayed in [Current Value].
AA-7000 4-31
Chapter 4 Measurement Procedures
5. If the result is acceptable, extinguish the flame and click on [OK]. The [Optimum Burner Height
Search] dialog box is closed to return to the [Atomizer/Gas flow Rate Setup] page, and the obtained
value is indicated and used as the [Burner Height]. If the [Cancel] is pressed, the burner height is
returned to the original position.
1. Set the [Start] and [End] of the gas flow search range. The range can be set within 0.8 to 4.0 L/min in
the case of Air-C2H2 and within 5.8 to 9.0 L/min in the case of N2O-C2H2. It is recommended to set the
range within the standard condition ±0.5 L/min. The flow rate of support gas is fixed at the currently
entered value. The optimal value for the flow rate of fuel gas must be obtained considering this fixed
value.
2. Press the PURGE button and IGNITE button on the front side of AA main unit to ignite a flame.
3. Start spraying the blank solution and click on [Blank Meas.] button. The measurement is performed
while the fuel gas flow rate is changed by 0.1 L/min step in the selected range. Continue to spray it
until the measurement is completed.
4. Next, start spraying the standard (or sample) solution and click on [STD Meas.] button. In the same
way as blank measurement, the measurement is performed while the fuel gas flow rate is changed.
Continue to spray it until the measurement is completed.
The dialog box displays the graph which is created by subtracting the measurement result of <3> from
the measurement result here. And the fuel gas flow rate with which the absorbance becomes the
highest is also displayed in [Current Value].
4-32 AA-7000
4.8 Specifying Optimal Conditions for Flame
5. If the result is acceptable, extinguish the flame and click on [OK]. The [Optimum Gas Flow Rate
Search] dialog box is closed to return to the [Atomizer/Gas Flow Rate Setup] page, and the obtained
value is indicated as the [Fuel Gas Flow Rate]. If the [Cancel] is pressed, the fuel gas flow rate is
returned to the original position.
NOTE
• If the [Fuel Gas Flow Rate] is changed, distribution of atoms in the flame changes, as the result, the
optimum [Burner Height] also changes. On the other hand, changing the [Burner Height] also changes
the optimum [Fuel Gas Flow Rate]. Note that the optimum condition changes if the other condition is
changed.
• To search the optimum condition precisely, for example, select several levels of burner height and
search the optimum gas flow rate at each level of burner height. Then select the best combination that
shows highest sensitivity. (Or you can also select several levels of gas flow rate and search the burner
height at each flow rate). Although some elements (such as Cu) are not affected so much by these
conditions, some elements (such as Cr) are affected greatly.
• If these settings are not appropriate, not only the sensitivity decreases, but also poor reproducibility of
data may be caused by sensitivity fluctuation. Utilize these functions for setting the optimum conditions
when required.
AA-7000 4-33
Chapter 4 Measurement Procedures
4-34 AA-7000
Chapter 5
User Administration
CONTENTS
AA-7000 5-1
Chapter 5 User Administration
5.1 GxP Support Functions
This software is equipped with functions that meet the reliability requirements of GLP/GMP and FDA 21 CFR
Part 11. The GxP support functions of this software provide effective and efficient help in achieving compliance
with the rules and requirements of GLP/GMP and FDA 21 CFR Part 11.
This chapter explains the basics of GLP/GMP and FDA 21 CFR Part 11, and gives an overview of GxP support
functions provided in this software.
Preparation of Standard
Operational Procedure (SOP)
The characteristic of this method is that an audit trail may be reviewed by managing and recording the entire
process (validation, work flow, and data) until the results are obtained, in order to ensure the quality of the final
results (data).
NOTE
• This software treats GLP and GMP together in the GxP support because, though they are different
guidelines, there are many commonalities between the two in terms of methodology.
• For proper execution of a task, we recommend the usage of GLP/GMP methods, even in the analysis
lab where GLP/GMP compliance is not necessarily required.
5-2 AA-7000
5.1 GxP Support Functions
Data Administration
The use of the GxP support functions available in the WizAArd is optional, but will powerfully support and save
your GLP/GMP-related work that tends to become troublesome.
NOTE
For electronic signatures for reviews and approvals of electronic records or for long-term storage of such
records, the combination with the optionally available CLASS-Agent conforms to the FDA 21 CFR Part 11.
Though this software is equipped also with the electronic signature function, this function only is insufficient
for the FDA 21 CFR Part 11.
AA-7000 5-3
Chapter 5 User Administration
5.2 System Administration
4
5 6
1 [User ID] Enter a user ID for login or a user name for display. Since the same name/ID
[User Name] can be used only one time in this software, you can enter your full name or
detailed information in the [Description] field and an abbreviated name or alias
in the [User Name] field.
4 [Administrator] Put a check mark to provide the system administration right to the currently
registered user. The administrator has complete access and cannot be
registered in a group.
5 [Group] Select groups where the user belongs. The user can use all functions that his/
her group has the rights to use.
5-4 AA-7000
5.2 System Administration
6 [Instruments] Select the analytical instrument that the user can use.
To use functions that require their usage rights, the user needs to enter his/her registered ID and password
in the [Login] window displayed when each program starts up.
If an ID or password entered in the [Login] window is different from the ones registered, the program will
not start up.
(2) Rights (Group)
The [Rights] setting can limit the functions that can be used, using the system administration function.
The following groups with the rights shown have been registered. Registering a user to a group that has
the necessary rights enables the user to have the same usage rights.
Right a
Right b
User 1 Group A
Right c
Group B
Right d
User 2
Group C
Right e
Right f
AA-7000 5-5
Chapter 5 User Administration
Default rights
Group with H/W Group with
Group with
Right Administrator Method
Operator rights
rights Developer rights
Edit Configuration 3
Run Measurement 3 3
Edit Measurement Table 3 3
Edit Measurement Parameters 3
Edit Data Processing Method 3
Edit Acquisition Display Method 3 3
Edit Print Format 3
Put Electronic Signature 3 3
Maintenance 3
QAQC Settings 3
Instrument Manipulation 3 3 3
Exit during Screen Lock 3
Invalidate Electronic Signature
NOTE
1. A user can belong to more than one group. In this case, that user will have all the rights of whichever
groups he/she belongs.
2. The "System administrator" will have complete rights.
3. A new group with the desired rights can also be created.
For more information about creating new rights groups, refer to 5.2.3.2 "Registering (Changing/Deleting) Rights
Groups".
5-6 AA-7000
5.2 System Administration
Uses passwords.
If the registered password is not entered correctly in the [Password] field in the [Login] window, the
program will not start.
AA-7000 5-7
Chapter 5 User Administration
Register a user
[User Administration]-[Users] Tab
5-8 AA-7000
5.2 System Administration
On the [System Policy], the security level basically* becomes higher as the number of checked setting
items increases.
The numeric settings are regarded appropriate if each parameter falls within the practical range* when a
sufficiently short life span of password (approximately one several thousandth or less) is set for the mean
decryption time for a password, which is obtained from the following equation:
* It is important to specify such Minimum Password Length and Maximum Password Age as you can
remember without writing them down, such a Lockout Duration value as would not cause great
inconveniences on your tasks if you should become unable to log in the system, and such a Login
Attempt Limit value as provides allowance for you to correct it if necessary.
NOTE
If the user ID is properly managed, it requires decryption resulting in a higher security level. For the above
calculation, however, no user ID is taken into consideration assuming that character strings such as
employee numbers, which may be found externally, are used.
The following example calculated by the above procedure shows one of the recommended set of values:
In the case, the mean decryption time (converted into years) is 4,000 years or more providing an allowance
of at least 8,000 times the above life span value of password (0.5 year). If you need an allowance of 10,000
times or more, enter stricter values than those specified in parentheses, which may be regarded as falling
in the practical ranges.
If any of the above values is less strict, the other values will relatively become stricter for practical use.
Therefore, Minimum Password Length = 6 and Maximum Password Age = 180 days are general settings
for similar types of systems.
* Assuming that only alphanumeric characters are used. This case is not (Upper/Lower) case-sensitive for
difficulty to force random mixed-case-strings.
AA-7000 5-9
Chapter 5 User Administration
NOTE
The WizAArd has more powerful user administration functions than Windows in that:
• Even if a user is deleted, it is only hidden, but its entry is retained. This prevents any other user with the
same name from being registered. Therefore, the traceability of data that was acquired by the deleted
user can be kept intact.
• The user ID is managed in combination with the corresponding user name and only used at login. For
the subsequent display, the user name is used.
(1) When the [WizAArd] launcher has not started yet, double-click the (WizAArd) icon on the desktop.
(2) Click on [Administration] tab from the [WizAArd] launcher. Log in with a User ID that has system
administration right.
NOTE
The settings entered [System Policy] and [User Administration] will become effective from the next time the
program window is started (logged in).
5-10 AA-7000
5.2 System Administration
System
Administration
Function Right Remarks
Yes No
[System Policy]
[User Administration]
[Log Browser]
AA-7000 5-11
Chapter 5 User Administration
(1) When the [WizAArd] launcher has not started yet, double-click the (WizAArd) icon on the desktop.
(2) Click on [System Policy] on the [WizAArd] launcher.
2
3
4
5-12 AA-7000
5.2 System Administration
1 [Level] allows you to select the preset policy settings by clicking on the [Setting] button.
Level Description
21 CFR P11 High The system must comply with the FDA21 CFR Part 11.
2 [Minimum Password Minimum number of password characters, used for user registration, and
Length] user password changes.
3 [Maximum Password If a program is started after number of password effective days, window
Age] appears to change password.
4 [Password must meet Allows you to disable to set password with using dictionary word.
complexity requirement]
[Login Attempt Limit] If login failures exceed the specified number of times, all the users on the
PC or network will become unable to log into the PC or network for the
specified period of time.
[Lockout Duration] Allows you to set the login lockout duration in the unit of PC.
[Login Attempt Limit] Allows you to set the upper limit of the number of login attempts in the unit
of user.
[Lockout Duration] Allows you to set the login lockout duration in the unit of user.
7 [# of levels for Duplicate If this is set, different password is required at changing in specified times
Password Checking] memorized.
AA-7000 5-13
Chapter 5 User Administration
To set the system administration policies other than user administration, use the right half of the [System Policy]
window.
1 [Audit Trail]
[Apply audit trail function when If this check mark is checked, audit trails are recorded automatically
creating file] since a new file is created.
[Require input of reason in If this check mark is checked, the screen prompting to enter the
recording audit trail] reason for operation is displayed every time an audit trail is
recorded automatically.
2 [Report]
[Output data status in header] If this check mark is checked, "Status: Temporary" is printed at the
header of the printed matter when printing is executed while data is
not saved.
The user can check for mismatch between the printed information
and the information registered in the Agent.
5-14 AA-7000
5.2 System Administration
3 [File Management]
[Prohibit overwriting of other If this check mark is checked, if there is a file having the same name
data files] in the saving folder at the time of saving, overwriting the existing file
is disabled.
[Prohibit overwriting of other If this check mark is checked, if there is a file having the same name
template files] in the saving folder at the time of saving, overwriting the existing file
is disabled.
[Prohibit disposing of unsaved If this check mark is checked, if there is unsaved measured data,
measured data on the shutdown of the WizAArd, creation of new files, reading of files and
memory] deletion of elements are disabled.
NOTE
1. The settings on the [System Policy] window will become valid at the next login.
2. The above setting to protect against overwriting files is not applicable when you open a file and modify it
and then save. The setting is applied to prohibit overwriting other existing files if autosave function
works during data acquisition or if the file is saved using [Save As] function.
3. "unsaved measured data" means the data that is acquired from the instrument and is not saved to a file
yet. If you just open a data file and modify it and then the modified file is not saved yet, data in the file is
not "unsaved measured data".
4. If file editing itself is the problem, use User Administration tool to specify whether or not to authorize
each user with the right to perform edit and postrun analysis, or enable the audit trail for data files and
record the modification log when saving the file.
(1) When the [WizAArd] launcher has not started yet, double-click the (WizAArd) icon on the desktop.
AA-7000 5-15
Chapter 5 User Administration
(3) Click on the [Group] tab from the [User Administration] property sheet.
1 [Add] Click [Add] to display [Add Group] window. Settings are same as [Group
Properties] as follows.
2 [Remove] Click [Remove] and a highlighted group name in group list is deleted.
(4) Click on [Properties] in the [User Administration] property sheet to set the group property.
Group Property
3
2
5-16 AA-7000
5.2 System Administration
3 [Add] Click [Add] to move the item from [Rights] to [Selected Rights]. Those rights
are given to the group.
NOTE
To specify a system administrator, use the [Add User] or [User Property] window.
AA-7000 5-17
Chapter 5 User Administration
(1) When the [WizAArd] launcher has not started yet, double-click the (WizAArd) icon on the desktop.
(2) Click on [User Administration] icon from the [WizAArd] launcher.
1 [Add] Click [Add] to display [Add User] window. Settings are same as [User
Property] as follows.
2 [Remove] Clicking on the [Remove] button hides the user highlighted in the users list
as deleted user.
5-18 AA-7000
5.2 System Administration
User Property
2
3
5 6
3 [Confirm Password] Enter password twice for confirmation. Password length must be longer
than that specified on [System Policy]'s [Minimum Password Length:]. Input
will display with '*' marks.
5 [Groups] Select desired item from [Group List] and move to [Selected Groups:] using
[Add>>]. User will have group's rights.
6 [Instruments] Select desired item from [Selected Instrument items:] and move to
[Instrument Item List:] using [<<Remove]. User can't use that Analytical
Instrument.
NOTE
If you try to register a user with the same user ID/user name as that of a previously deleted user through the
[Add User] window, a dialog box will be opened prompting you to confirm whether or not to restore the
previous user.
AA-7000 5-19
Chapter 5 User Administration
Log Browser
3
Fig. 5.17 [Log Browser]
5-20 AA-7000
5.2 System Administration
1 [Search] Enter search parameters and click [Search] button to pickup the records of
Log.
2 Event log Event log data can be converted to text file as input to commercial
spreadsheet software such as MS-Excel.
3 [Delete Log] If log data is not necessary, it can be deleted. The operation to save the log
as a text file is required before it is deleted.
(1) When the [WizAArd] launcher has not started yet, double-click the (WizAArd) icon on the desktop.
(2) Click on [User Administration] Icon from the [WizAArd] launcher.
(3) Click on [Password] Tab from the [User Administration] property sheet.
[User Administration] - [Password] Tab
AA-7000 5-21
Chapter 5 User Administration
2 [New Password] Enter new password twice for confirmation. Password length must be
[Confirm New Password] longer than that specified on [System Policy]'s [Minimum Password
Length:].
Input will display with '*' marks.
NOTE
If a user logs in who does not have system administration right, [User Administration] window displays only
[Password] tab.
NOTE
A user with the system administration right can perform initial settings/resettings of passwords all user
(except Admin) in the [Users] tab's [User Property] window.
For more information about of the initial settings/resettings of user's passwords, refer to 5.2.4 "Registering
(Changing/Deleting) Users".
5-22 AA-7000
5.3 Using the Security Support Functions
5.3 Using the Security Support Functions
The use of the security support functions facilitates controlling the workflow and improves the reliability of the
obtained data.
• The combination of two components (login ID and password) serves as an electronic signature.
• The login ID is only used at login and subsequently the user name is used for display.
• The entered password is displayed using asterisks (*). The system policy settings allow you to specify the
minimum length and life span for a password.
NOTE
Employment of two distinct components in an electronic signature such as combination of a login ID and
password is mandatory for compliant systems; however, it is meaningful only when accompanied by proper
user management. Below are examples of some common practices that must be avoided.
• Multiple individuals use the same login ID (i.e. "Admin") for login. This practice is dangerous as it inhibits
the ability to identify who handled the data, and to prevent unauthorized access to the system.
• Registers multiple login IDs with no password. Users can use any login IDs easily and there is no record
who actually performed the operation.
For more information, refer to 5.2.3.1 "Setting User Administration Policies", 5.2.4 "Registering (Changing/
Deleting) Users".
AA-7000 5-23
Chapter 5 User Administration
Left menu All the operations can be performed under the system administration right.
Right menu If the operator level right is selected, analytical tasks can only be done through a prepared
method.
5-24 AA-7000
5.3 Using the Security Support Functions
NOTE
1. The GLP/GMP assures the quality of the acquired data by showing the fact that the section for securing
the reliability has been separated from that for actually carrying out the inspection and analysis and by
certifying that the tasks are performed in accordance with the standardized procedures.
2. This function is also effective for preventing wrong operations and decreasing the time required for
mastering the operations by hiding the unnecessary functions.
For more information, refer to 5.2.3.2 "Registering (Changing/Deleting) Rights Groups", 5.2.4 "Registering
(Changing/Deleting) Users".
NOTE
If you attempt to open the screen, the [User Authentication] dialog box will pop up. The system will accept no
operation while this dialog box is open.
AA-7000 5-25
Chapter 5 User Administration
5.4 Audit Trail
The WizAArd supports the following two major types of audit trails as shown in the table below.
1 Data History This is the history of transitions contained in the measurement data itself, and
used to verify the integrity of the data. This history is displayed from the
WizAArd.
2 System History This is the history of transitions indicating changes on the workstation. The
WizAArd supports the following logs.
5-26 AA-7000
5.4 Audit Trail
(1) When the [WizAArd] launcher has not started yet, double-click the (WizAArd) icon on the desktop.
(2) Click on [Log Browser] from the [WizAArd] launcher.
AA-7000 5-27
Chapter 5 User Administration
NOTE
When the optional Agent Connection Kit and the Public Agent are installed, the instrument log and system
administration log (indicating the history of changes in the lamp settings, print settings, environmental
settings, etc.) which are specific to the WizAArd can be registered to the CLASS-Agent, and managed.
5-28 AA-7000
5.5 Performing Software Validation
5.5 Performing Software Validation
(1) Specify a program used in the program alteration check, then click on [Check].
AA-7000 5-29
Chapter 5 User Administration
Program check result details are viewed via the Result Viewer.
After program check is complete, check results appear.
NOTE
To get report of Program Check Result, Click on the [Print] button.
5-30 AA-7000
5.5 Performing Software Validation
NOTE
Load the check data file from the WizAArd Setup CD-ROM every time software validation is performed to
prevent it from being overwritten in previous function checks or operations. The data is saved in the
"\Sample" folder in the WizAArd setup disk.
(2) Change the calibration curve type, and confirm that the quantitative result is calculated again correctly.
Check the quantitative result using the concentration of "UNK1-AV" in the sample table.
AA-7000 5-31
Chapter 5 User Administration
5.6 Data Administration
NOTE
CLASS-Agent and some of other archiver products that have been described above support the capability of
storing files on CD-R.
5-32 AA-7000
5.6 Data Administration
NOTE
Managing PDF file with CLASS-Agent is optional.
AA-7000 5-33
Chapter 5 User Administration
5.7 Other System Management Tools
3. When the user having the system administration right logs in the system, the [Database Maintenance]
window will be displayed.
1 3
1 [Repair Database] Clicking on this button duplicates the database and then
reconstructs the fragmented database into a more compact one or
attempts to repair the database having a fault.
2 [Change Database] Clicking on this button displays the Select File window. If a file in a
new reference source is selected, that management database will
be referenced starting with the next activation.
5-34 AA-7000
5.7 Other System Management Tools
NOTE
If the network mode is selected, the system administration information (user rights, etc.) entered from one
point on the LAN can be shared by all the WizAArd that uses the common system administration database.
NOTE
• MSDE (Microsoft Data Engine) is required to use Shimadzu user authentication tool on the network.
MSDE installer is attached in CLASS-Agent setup disk, Office2000/XP setup disk. You can download it
from Microsoft web site.
• If you use MSDE installer of Office2000/XP or one downloaded from web site, and do NOT use one of
CLASS-Agent setup disk, please note the followings. If MSDE2000 is installed by default options, it is
Windows authentication mode and it requires password. It is also prohibited from using it on the network
by default. Thus, add the following options to MSDE2000 install command for Shimadzu user
authentication tool to use it.
• MSDE has different programs for each language. If you use CLASS-Agent English version, install
MSDE English version. If you install other language version of MSDE, CLASS-Agent does not work.
AA-7000 5-35
Chapter 5 User Administration
CAUTION
If you share system the administration database file on the network, please note the followings.
1. Setup to use Shimadzu user authentication tool on the network.
2. If you edit PC information, device name, user information, etc., exit all other WizAArd programs that
share the administration database file on the network.
The [Maintenance of Instrument Information] window is opened when the following steps are performed:
(1) Shut down all the WizAArd programs.
(2) Using the [Database Maintenance] tool, select the network mode for all the WizAArd software that
shares the system administration information.
1 Check this option to select the network mode for the system administration function.
2 Select referencing the system administration database files that are shared on the network.
5-36 AA-7000
5.7 Other System Management Tools
(5) Log in with a User ID that has system administration right. The [Add/Specify Computer] dialog box of
the [Maintenance of Instrument Information] will appear.
NOTE
If the Add/Specify Computer option is already selected and if the current PCs are associated with PC
information, then this window is skipped.
1 Add the computer as the one that is managed (identified) on the system administration
database in the network mode.
2 For the computer that is already registered on the system administration database (e.g., the
first computer or a computer that was once added, but has the software reinstalled for any
reason), select it from the list and then specify it so that it is associated with the displayed
existing computer information.
AA-7000 5-37
Chapter 5 User Administration
[Maintenance of Instrument Information] main window comes up after finishing the above setting.
1 Displays the list of computers that are centrally managed on the network
2 Analytical Instruments, which are linked with the computer above selected, is shown here.
The entry of the analysis system selected from the [Instrument] list may be deleted,e.g., when
the actual system is abolished.
(6) At this point, the network settings for the system administration are complete. After checking that there
is any registration in the [Computer] pull-down list, click on the [Close] button to close the
[Maintenance of Instrument Information] window.
5-38 AA-7000
Chapter 6
QA/QC Setup
CONTENTS
AA-7000 6-1
Chapter 6 QA/QC Setup
6.1 What is QA/QC?
QA/QC as described here is an abbreviation for Quality Assurance/Quality Control included in the analysis
method that the U.S. Environmental Protection Agency requires for inorganic analysis of water and soil (USEPA
Contract Laboratory Program Statement of Work for Inorganic Analysis).
The Statement of Work for Inorganic Analysis describes the specific methods of demonstrating that the quality
of the actually collected data is assured, as well as the pretreatment method and analysis conditions that should
be observed by the analyst.
It is not obligatory to perform the QA/QC checks for any document other than the reports to the EPA. However,
the concepts and approaches of the QA/QC checks seem effective in many cases. The WizAArd software
allows you to automatically perform these checks.
This chapter describes the requirements of the QA/QC checks and the corresponding settings of the WizAArd
software.
The QA/QC check items are classified into those used to validate the created calibration curve and those used
to verify the effects of the pretreatment and liquid properties.
(1) In validating the calibration curve, the calibration curve is evaluated using the correlation coefficient and a
standard solution other than the one used for creating the calibration curve is measured. These checks are
classified into ICV and ICB that are carried out immediately after a calibration curve has been created, and
CCV and CCB that are used to check the sensitivity of the instrument that changes with time.
(2) For the effects of the pretreatment and liquid properties, conduct the spike test. The spike test is an
addition/recovery test, which includes SPK (to comprehensively verify the sublimation during processing
and the effect of liquid properties) in which a known amount of a standard solution is added before the
pretreatment and PDS in which a known amount of a standard solution is added after the pretreatment.
This test also includes duplication in which the same pretreatment is separately applied to the same
samples to verify the reproducibility of the pretreatment and PB in which a blank for the pretreatment is
verified. If samples are common, they may be handled as a group. When one sample from that group is
verified, the entire group is also verified.
In EPA, a reference value is established for each check item. There are different instructions depending on
whether the established value is met or not met. More specific reference values and instructions will be
mentioned in the description of each item.
6-2 AA-7000
6.2 QA/QC Check Items and Their Settings
6.2 QA/QC Check Items and Their Settings
This section specifically describes the QA/QC items in the order conforming to the USEPA's standard.
Order
1. Calibration of instrument (creation of calibration curve)
2. ICV and ICB
3. CCV and CCB
4. CRA: CRDL for AA
5. PB: Preparation blank
6. LCS: Laboratory control sample analysis
7. S: Spike test
8. D: Duplicate sample analysis
9. IDL: Instrument detection limit determination
The reference value for each item must be met. If it is met, you unconditionally go forward to the next
measurement. If it is not met, you may select processing.
"Mark & : A comment stating the reference value is not met is displayed in Out-of-Control
Continue" Note and the measurement continues.
"Pause" : The measurement stops when the reference value is not met (a message is
displayed in the case of the manual measurement).
[Retry] : If ticked, only the samples that did not meet the reference value will be re-
measured only once under the same conditions. Either "Mark & Continue" or
"Pause" is selected in accordance with the 2nd result.
AA-7000 6-3
Chapter 6 QA/QC Setup
(1) In the WizAArd software, click on the [Calibration Curve Setup] button in the [Preparation Parameters]
page of the element selection wizard.
The [Calibration Curve Setup] window is displayed.
(2) Click on the [QC Blank/QC Standard Setup] button.
6-4 AA-7000
6.2 QA/QC Check Items and Their Settings
1 2 3
To perform the QA/QC checks, tick desired QA/QC Type as shown in the figure.
1 [Acceptance Criteria] [Acceptance Criteria] may be set freely, but the default value that is first
displayed is the USEPA's recommended condition.
3 [Out of Control Action] [Out of Control Action] allows you to select either "Mark & Continue" or
"Pause". Select "Mark & Continue", if you want to continue the
measurement regardless of the result of the QA/QC check. Select
"Pause" to review the preparation of the sample and other factors when
the result shows a failure in meeting the reference value.
AA-7000 6-5
Chapter 6 QA/QC Setup
4 [CORR] (Correlation This coefficient shows how much the measured value is close to the
coefficient = r) calibration curve obtained by the least square method. As the
coefficient is closer to 1, the result becomes better. r is calculated with
the following equation.
r = (N Σ xi yi- Σ xi Σ yi)/{N Σ xi2-( Σ xi)2}1/2{N Σ yi2-( Σ yi)2}1/2
To evaluate the correlation coefficient, tick this check box and select
"CAL-CHK" in the [Action] field of the MRT worksheet.
NOTE
"CAL-CHK" must be selected only for the calibration curve method.
This setting is not required for the simple standard addition method
or the standard addition method.
5 [%TV] (Self-determined The calibration curve obtained by measuring a set of standard samples
true value) is used to evaluate how much the result obtained by re-determining the
concentration of the standard sample at different points is correct
relative to the prepared concentration. The difference from the prepared
concentration must be within 5% (USEPA's recommended condition).
To enter the %TV applicable lower limit, tick the [Set %TV Application
Lower Limit] check box and enter a value. The %TV applicable lower
limits of only 23 elements are recommended by the USEPA as shown in
the Table below, but the measurement method differs depending upon
the element. (Flame) indicates that this element is used for
measurement by the flame continuous method. As, Se, and Sb are
used for the hydride generation method, Hg for the reduction and
vaporization method, and others for the furnace method.
Sb (*) 60 Mn 15
Ba 200 Ni 40
Be 5 K (Flame) 5000
Cd 5 Se (*) 5
Ca (Flame) 5000 Ag 10
Cr 10 Na (Flame) 5000
Co 50 Thallium 10
Cu 25 V 50
Fe 100 Zn 20
Pb 3
IDL/CRDL may also be specified in the window displayed by selecting [Parameters]-[IDL/CRDL Setup] from the
menu bar.
6-6 AA-7000
6.2 QA/QC Check Items and Their Settings
1 [ICV] (Initial Calibration Perform this verification immediately after a calibration has been
Verification) created. The solution for use in verification is different from the standard
solution used to create the calibration curve and must have a different
concentration from the one used for creating the calibration curve,
within the concentration range for calibration curves. The EPA's
acceptance criteria require that the measured value fall within a range
between 90% and 110% of the prepared concentration (between 80%
and 120% for HG). If the result exceeds this range, the measurement is
stopped.
2 [ICB] (Initial Calibration Perform this measurement immediately after ICV. It is intended to check
Blank) that the blank value decreases properly. The EPA's acceptance criteria
requires that the analysis should be stopped if CRDL is exceeded and
that the re-measurement should be performed after the problem has
been solved.
AA-7000 6-7
Chapter 6 QA/QC Setup
2 [CCB] (Continuing Perform blank measurement immediately after CCV. The EPA's
Calibration Blank) acceptance criteria requires that the analysis should be stopped if
CRDL is exceeded and that the re-measurement be performed either
for 10 previous samples or for all the samples up to the former ICB and
CCB after the problem has been solved.
6-8 AA-7000
6.2 QA/QC Check Items and Their Settings
(1) Click on the [Action] cell in the row to which CRA is applied, to display the drop-down list.
(2) Select CRA from the list to establish it. After establishing the CRA, enter a value in the [True Value] field.
AA-7000 6-9
Chapter 6 QA/QC Setup
(1) Click on the [Sample Group Setup] button in the [Preparation Parameters] page of the element selection
wizard, and then the [Sample Group Setup] window shown in Fig. 6.6 is displayed.
(2) Click on the [QAQC Setup] button.
6-10 AA-7000
6.2 QA/QC Check Items and Their Settings
(3) In the window shown in Fig. 6.7, tick the [Preparation Blank (PB)] check box. If the ASC is used, enter the
preparation parameters such as position and sample volume in the preparation parameters table located at
the bottom of the window.
PB must be lower than CRDL, but if CRDL is exceeded, mark the measurement result in accordance with
actions (2) and (3).
NOTE
Like LCS, PB is automatically inserted into the MRT worksheet after the wizard has been completed, so far
as the corresponding check mark is ticked in the [Sample Group QA/QC Setup] dialog box. To add PB to the
already prepared MRT worksheet, [Action] may be specified in any row of the MRT as shown in Fig. 6.8. If
the ASC is used, enter the preparation parameters such as position and sample volume.
AA-7000 6-11
Chapter 6 QA/QC Setup
(1) For the LCS settings, tick the [LCS] check box in the [Sample Group QA/QC Setup] dialog box shown in
Fig. 6.7. Enter the known concentration in the preparation parameters table at the bottom of the window. If
the ASC is used, also enter the preparation parameters such as position and sample volume.
NOTE
Like PB, LCS is automatically inserted into the MRT worksheet after the wizard has been completed, so far
as the corresponding check mark is ticked in the [Sample Group QA/QC Setup] dialog box. To add LCS to
the already prepared MRT worksheet, [Action] may be specified in any row of the MRT as shown in Fig. 6.9
and enter the known concentration to the [True Value] field. If the ASC is used, enter the preparation
parameters such as position and sample volume.
6-12 AA-7000
6.2 QA/QC Check Items and Their Settings
PDS
In case of the flame AA (and ICP), if the pre-digestion/pre-distillation spike ratio does not fall within a range
between 75% and 125% and if the sample concentration does not exceed 4 times the spike concentration, then
carry out post-digestion/post-distillation spike (except for Ag). The added concentration must be 2 times the
original sample concentration or 2 times CRDL, whichever higher (PDS is not required for Hg).
SSR-SR
%Recovery= x100
SA
NOTE
When the same sample as the spiked one is duplicated, use the analysis result of the original sample rather
than the mean value for the duplicated one.
AA-7000 6-13
Chapter 6 QA/QC Setup
The SPK and PDS settings can be entered in the [Sample ID Collective Setup] dialog box displayed by clicking
on the [Collective Setup] button in the [Sample Group Setup] Page in Fig. 6.6.
(1) Tick the [Pre-Digestion Spike (SPK)] and [Post-Digestion Spike (PDS)] check boxes and enter a
measurement interval (the default value is 20) in the respective right fields. This measurement interval
must be smaller than the number of samples.
(2) Click on the [OK] button to return to the [Sample Group Setup] page. Now [Pre-Digestion Spike (SPK)] and
[Post-Digestion Spike (PDS)] are automatically entered in the [Unknown/Spike Measurement Sequence]
table of the current sample group number.
To add them to the prepared MRT worksheet, specify "SPK" or "PDS" action in any row of the MRT
worksheet and then enter the added concentration as shown in Fig. 6.11. If the ASC is used, enter the
preparation parameters such as position and sample volume.
NOTE
The [Unknown/Spike Measurement Sequence] table in the [Sample Group Setup] page shown in Fig. 6.6
also allows you to enter "SPK" and "PDS" actions by performing similar operations.
SPK and PDS must be compared with directly previous UNK. Therefore, specify the preparation parameters
accordingly. (Fig. 6.11 shows that SPK will be performed for UNK3.)
6-14 AA-7000
6.2 QA/QC Check Items and Their Settings
|S-D|
RPD= x100
(S+D)/2
If the concentrations of both (S and D) are more than 5 times CRDL, the reference value for RPD is 20%
maximum. If either or both of S and D do not reach 5 times CRDL, use the reference value for ±CRDL (i.e.,
enter the absolute value for CRDL as the reference value for RPD).
(1) For the duplication settings, tick the [Duplicate] check box in [Sample ID Collective Setup] dialog box
shown in Fig. 6.12 and then enter a measurement interval (the default value is 20) in the right field, as in
the case of Spike. This measurement interval must be smaller than the number of samples.
(2) Click on the [OK] button to return to the [Sample Group Setup] page. Now Duplicate is automatically
entered in the [Unknown/Spike Measurement Sequence] table of the current sample group number.
To add it to the prepared MRT worksheet, specify "DUP" action in any row of the MRT worksheet. If the ASC is
used, enter the preparation parameters such as position and sample volume.
NOTE
The [Unknown/Spike Measurement Sequence] table in the [Sample Group Setup] page shown in Fig. 6.6
also allows you to enter "DUP" action by performing similar operations.
DUP must be compared with directly previous UNK. Therefore, specify the preparation parameters
accordingly.
AA-7000 6-15
Chapter 6 QA/QC Setup
This software allows you to automatically evaluate the measurement results of the above items, stop
measurement, or mark and continue the measurement. Notice, however, that some of the acceptance criteria
do not accurately conform to the EPA's QA/QC reference (e.g., the ratio between the sample concentration and
spike concentration at the Spike test and that between the measured concentration and CRDL at the Duplicate
test).
Abbreviation Description
PB Preparation Blank
Standard sample for analysis use containing water and reagents used in analysis process
SPK Spike
Spike of adding a standard solution before digestion
D Duplicate
The second sample that has been pretreated like the original sample to determine the
accuracy of the measuring method
6-16 AA-7000
6.2 QA/QC Check Items and Their Settings
TV True Value
Self-determination true value
r Correlation coefficient
AA-7000 6-17
Chapter 6 QA/QC Setup
6-18 AA-7000
Chapter 7
Hardware Validation
CONTENTS
AA-7000 7-1
Chapter 7 Hardware Validation
7.1 What is Hardware Validation?
The hardware validation is intended to check the basic performance of the AA-7000 series, evaluate the results,
and then record the validation results together with the date and time.
To ensure the reliability of data obtained from the analytical instrument, it is important to check the performance
of analytical instruments periodically, record the data, and take measures such as a correction work based on
the check result.
The hardware validation is based on the performance check procedures carried out in our factory, therefore,
you can execute the performance check work properly and more easily by utilizing this software.
7-2 AA-7000
7.2 Necessary Items
7.2 Necessary Items
The necessary tools and samples are shown in Table 7.1 below. These tools and samples are necessary when
the standard parameters of hardware validation are used for the performance check.
NOTE
Be sure to prepare the hollow cathode lamp (Hg) that is necessary for the wavelength accuracy check in any
cases.
AA-7000 7-3
Chapter 7 Hardware Validation
7.3 Outline of Standard Test Item
The test items in the hardware validation and their outlines are introduced.
For the default tolerance limit for each test item, see 10.1.4 "Performance Specifications".
• Necessary tool
Hollow cathode lamp (Se)
• Necessary tool
Hollow cathode lamp (Cu)
7-4 AA-7000
7.3 Outline of Standard Test Item
Stability = w/B
AA-7000 7-5
Chapter 7 Hardware Validation
7-6 AA-7000
7.4 Basic Operation Procedures
7.4 Basic Operation Procedures
In this section, the basic operation procedures are described. When changing the parameters, refer to the
section 7.5 "Parameter Change".
7.4.1 Preparation
7.4.1.1 Preparation of Hollow Cathode Lamp
First, set the hollow cathode lamps to the AA main unit referring to Table 7.3 below.
Distilled water R0
Blank solution R1
In the case of manual measurement, prepare the above samples in the measuring flasks or beakers.
Blank solution R1
In the case of manual measurement, prepare the above samples in the measuring flasks or beakers and
prepare a pipette for sample injection (with which 20 μL injection is possible).
Set a pyrolytic coated graphite tube in the graphite furnace.
AA-7000 7-7
Chapter 7 Hardware Validation
NOTE
Alternatively, you may want to double-click on the AA hardware validation icon on the Desktop.
(2) After the software has been started, the following login dialog box is opened allowing you to log in.
7-8 AA-7000
7.4 Basic Operation Procedures
After the login has been completed, the window shown in Fig. 7.3 is displayed.
The test items that can be validated through the hardware validation are roughly classified as follows:
a. Common test items involving no sample measurement
Wavelength accuracy
NON-BGC and BGC-D2 noise levels
Baseline drift
b. Flame method test items involving sample measurement
Absorbance/Repeatability
Detection limit
Stability
c. Furnace method test items involving sample measurement
Absorbance/Repeatability
Detection limit
The items in group (a) are automatically proceed, but those in groups (b) and (c) proceed semi-automatically or
interactively.
No flame is ignited for the items in group (a).
If the ASC is used for the items in groups (b) and (c), the procedure for nozzle position adjustment is performed
before the tests.
AA-7000 7-9
Chapter 7 Hardware Validation
(1) Select [Tests]-[Modify Batch] in the menu bar. Or click on the in the tool bar.
The dialog box for [Modify Batch] is displayed. The inspection items indicated in the "Item to Perform" will be
executed.
NOTE
Since all the test items are displayed in the right-side column "Item to Perform" on the screen when sent from
the factory, delete unnecessary items for execution from this table.
(3) Press the [Delete] button at the center on the screen with the mouse. The selected items are moved to the
left column [Selectable item].
(4) When adding an item from the [Selectable item] to the [Item to Perform], select the item to add with the
mouse and press the [Add] button at the center of the screen with the mouse.
(5) With the above procedures, select the items for execution and press the [OK] button with the mouse. The
[Modify Batch] dialog box will be closed.
7-10 AA-7000
7.4 Basic Operation Procedures
(2) Click on the check box to make the ASC connection operative.
NOTE
• Without this setting, the ASC cannot be operated even if the ASC is connected to the AA main unit.
• If the ASC is used, match the position settings for [Blank] and [Sample] with the position of the ASC
turntable for the sample under measurement. In 7.4.1.2 "Sample Preparation", the position of the
turntable for the sample used to verify the detection limit is specified as "R3". Therefore, also specify
"R3" for the sample used to verify the lower detection limit in the [ASC Parameters] dialog box.
Refer to 7.4.1.2 "Sample Preparation".
AA-7000 7-11
Chapter 7 Hardware Validation
7.4.4 Setting the Warm-up Time of Lamps and Stabilization Time for
Flame
Set the warm-up lighting time of the hollow cathode lamp and D2 lamp when starting the performance check. If
the lamps are not stable, they may cause a drift and noises.
It is recommended to prepare the warm-up time longer than approx. 10 to 15 minutes in the case of hollow
cathode lamp, and the warm-up time for approx. 5 to 10 minutes in the case of D2 lamp.
Also, in the case of tests for Absorbance, repeatability, detection limit and stability with the flame analysis, the
waiting time for starting the data acquisition after the flame ignition can be set. Since the temperature of the
burner head is not constant right after the flame ignition, the flame temperature is not stable and it may cause a
sensitivity drift or instability. It is recommended to prepare the stabilization time at least longer than 1 minute
after the flame ignition.
(2) Input the stabilization time for each item and press the [OK] button.
The waiting condition continues during the input time, which works as the warm-up time in the case of lamp
and as the measurement waiting time (burner head preheating time) in the case of flame.
7-12 AA-7000
7.4 Basic Operation Procedures
NOTE
If another WizAArd software for controlling AA main unit is already connected for communication, firstly finish
the connection with the WizAArd software, then connect this validation program.
When the connection is started, the AA main unit is initialized. During initialization of the instrument, carry
out inspection of the safety devices.
For AA-7000F, see 3.1.6.1 "Initializing the Instrument".
For AA-7000G, see 3.2.6.1 "Initializing the Instrument".
(2) When all the items on the initialization screen are indicated in green, click on the [OK] button.
The main screen appears again. Before starting the tests, check that the printer is connected to the PC
correctly, the power is turned on and the printer paper is set.
AA-7000 7-13
Chapter 7 Hardware Validation
(3) Click on the in the tool bar as shown in the right figure, or select [Perform]-[Start] in the menu bar.
The validation proceeds from the top of the test items. The result for each item is indicated on the right of
each item in the test item column as [OK] or [NG].
The following indications are displayed according to the result and conditions.
7-14 AA-7000
7.4 Basic Operation Procedures
The tolerance limits and measurement value, result of OK or NG, and message showing the condition of
test are indicated on the lower right part of the screen.
Whenever one test item is completed, the measurement data is output to the printer.
AA-7000 7-15
Chapter 7 Hardware Validation
NOTE
In the case of test items except the wavelength accuracy, the [Abort] button is on the measurement screen
as shown in Fig. 7.14 below. Clicking on this button stops the current measurement. In the case of furnace
measurement, inspection stops after the current measurement finishes.
7-16 AA-7000
7.4 Basic Operation Procedures
AA-7000 7-17
Chapter 7 Hardware Validation
7-18 AA-7000
7.5 Parameter Change
7.5 Parameter Change
The test parameters can be changed except when the test item is the wavelength accuracy.
NOTE
When the measured data exists, the parameter cannot be changed. In this case execute [File]-[New] in the
menu bar to clear all the data.
AA-7000 7-19
Chapter 7 Hardware Validation
NOTE
1. When the element name of the hollow cathode lamp is input, the typical set wavelength and lamp
current are set. When changing the set wavelength and lamp current, change them after inputting the
element name.
2. When changing the lamp socket No., don't use the same socket No. for different hollow cathode lamps.
3. Also, since the mercury (Hg) hollow cathode lamp is usually set to the socket No. 1, select the No. from
No.2 to 6. in the case of the test items except the wavelength accuracy test.
4. "Detection limit" is calculated with the result from "Absorbance/ Repeatability". Set the same element for
these two inspections. When they have the different element set, "Detection limit" will not be calculated
properly.
The test parameters, which can be set for each item, are as follows.
7-20 AA-7000
7.5 Parameter Change
AA-7000 7-21
Chapter 7 Hardware Validation
(1) Select [Graph]-[Set Y-Axis in Each Test], then the dialog box "Set Y Axis Limits" as shown in Fig. 7.19
opens.
(2) Double-click on the test item to be changed with mouse or move the cursor to click on the [Change].
The dialog box to input the upper and lower limits of the ordinate scale opens. Input the values so that the
range for display/output may be in accordance with the tolerance limits.
7-22 AA-7000
7.5 Parameter Change
The contents saved as the information specific to the file are shown as follows.
a. Test item to be executed
b. Test parameters for each test item
c. Ordinate scale for graph display/output
d. Test result
NOTE
The parameters which can be set in the [Configuration] in the menu bar (preheating time set, ASC setting)
are not saved as the parameters specific to the file. When the program is started, these parameters are set
to the same condition that is set at the previous time.
NOTE
It is convenient to use different files according to the test content differences. For example, you can save a
validation file used for monthly performance check and a validation file for semiannual performance check
separately.
AA-7000 7-23
Chapter 7 Hardware Validation
NOTE
Since there is a default (initial condition just after installation) validation file "autoload.vld" as read-only,
rename "autoload.vld" to "autoload.org" before this operation.
(1) After setting the test items and test parameters, select [File]-[Save As] in the menu bar.
Then the dialog box [Save As] opens.
(2) Select the folder where the validation program execution file "aaval.exe" exists (usually ":\Program
Files\Shimadzu\WizAArd") first, then input the file name "autoload.vld" and click on [Save].
From the next time, the newly set "autoload.val" will be automatically read in when the validation software is
started up.
NOTE
When setting the start-up validation file back to the default, delete the "autoload.vld" file, and then rename
"autoload.org" to "autoload.vld".
7-24 AA-7000
7.6 Functions of Operation Menu
7.6 Functions of Operation Menu
In this chapter, the items displayed on the screen and their functions are described.
1
2
7
Fig. 7.22 Main screen
1 This is called menu bar, which shows a basic menu. Set the mouse cursor onto the function indication (File
etc.) and click on the left button of the mouse to select.
2 This is called tool bar, which used to shortcut selecting the same functions as the commands selected from
the Menu bar.
The each tool function is shown as below.
AA-7000 7-25
Chapter 7 Hardware Validation
3 This indicates the available test items. The test is executed according to the order indicated here.
After executing the test, the result OK / NG is indicated. The data of the finished test items can be checked
by selecting the item with double-clicking.
4 The current absorbance value is indicated at the time of measurement.
5 The measured data profile is displayed here.
6 The detail information of the test result is indicated here. The tolerance limits and measured values, the
result of OK / NG judgment and the message showing other test conditions are indicated.
7 This is called status bar, which indicates the current instrument working conditions, messages and
connections of the peripheral equipment (ASC, GFA).
7.6.2 File
Selecting [File] in the menu bar will show the screen as Fig. 7.23. The functions related to the validation files are
collected.
The validation file is a file with extension ".vld" and contains the test items, measurement parameters and test
result data.
1
2
3
4
5
6
3 [Save As] This is used to save the current validation file with a new name.
5 [Print Measured Data] All the measured data of each test item are output to the printer.
6 [Print Setup] Settings related to the printer are set up. Selecting this function will
open the dialog box [Print Setup].
See 7.6.2.1 "[Print Setup] Dialog Box".
7-26 AA-7000
7.6 Functions of Operation Menu
7 [File History] Maximum four validation files, which are lately read in, can be
displayed.
Click on the displayed file name. Then the validation file can be read in.
8 [Exit] This is selected to close this program. If the test data is not saved, the
warning message verifying that you wish to close this program is
indicated.
1 2
3 4
3 [Paper] The paper size and paper feed method are selected.
AA-7000 7-27
Chapter 7 Hardware Validation
7.6.3 Tests
Under this menu, the functions related to the setup of the test items to be executed are collected.
1
2
2 [Set Parameters] This is used to change the test parameters for each test item. However,
the parameters for the wavelength accuracy items cannot be changed.
The parameters cannot be changed if the test data exists.
7.6.4 Configuration
Under this menu, the functions to set up the conditions for executing this software are collected.
1
2
3
4
5
1 [Connect The communication between the AA main unit and the PC are set ON/
Spectrophotometer] OFF.
Start the instrument before setting the communication ON. For details, see
2.1 "Power ON/OFF".
Selecting this function after starting the instrument sets the
communication ON and indicates the check mark on the head of the
menu.
When setting OFF the communication, select this function again.
2 [Check Accessories] The communication between the AA main unit and the peripheral
equipment (ASC, GFA) is set ON.
3 [Instrument Settings] This is used to set up the serial port of the PC used for connection with
the AA main unit.
4 [Warm-up Time] The lamp warm-up time and the waiting time after flame ignition during
the tests are set.
5 [ASC Parameters] This is used to select whether the ASC is used for the test or not and to
set the sample position when using the ASC.
7-28 AA-7000
7.6 Functions of Operation Menu
7.6.5 Perform
This is the menu to start or stop the menu.
1
2
1 [Start] This is used to start the test. Before starting, it is necessary that the
connection for communication between the PC and the AA main unit is
completed.
7.6.6 Graph
This is the menu to set up the graph scale when the result data of each test is displayed or output.
1
2
1 [Set Limits] The result of the finished test item is displayed on the main screen as
the profile graph. This is used when changing the graph ordinate/
abscissa scale for the data currently displayed on the main screen.
The scale values are valid only right after they are set. If another item
graph is displayed once, the scale returns to the initial condition.
2 [Set Y Axis in Each Test] This is used to set up the initial scale values of the ordinate when the
graph of each test result is displayed or output.
They can be set for each test item except the wavelength accuracy. The
scale values set here are saved together with the test parameters as
the initial ordinate values for the graph display and printer output when
the file is saved (Refer to the section 7.5.3 "Setting the Scale for Graph
Display/Output of Each Data").
AA-7000 7-29
Chapter 7 Hardware Validation
7-30 AA-7000
Chapter 8
Maintenance
CONTENTS
AA-7000 8-1
Chapter 8 Maintenance
8.1 Routine Inspections and Periodic Inspections
In order to keep the instrument in good condition, carry out routine inspections and periodic inspections.
WARNING
• The items with marked in the "Safety" column are the inspection points that relate to safety.
Failure to complete these inspection points may result in gas leaks or flashback.
8.1.1.2 AA-7000F
Points to check before ignition
Burner head If there is clogging in the burner slot, See 8.2.1 "Burner Head
wash it free. Maintenance".
Nebulizer If the nebulizer fixing screws are loose, See Fig. 8.2.
tighten them up.
Drain tank Check the water level in the drain tank. See 2.8 "Supplying Water to
If it has dropped, supply water. the Drain Tank (AA-7000F)".
Nebulizer If the capillary tube is clogged, clean it. See 8.2.2 "Nebulizer
If the polythene tube that covers the Maintenance".
capillary tube is broken, replace it.
8-2 AA-7000
8.1 Routine Inspections and Periodic Inspections
WARNING
• The items with marked in the "Safety" column are the inspection points that relate to safety.
Failure to complete these inspection points may result in gas leaks or flashback.
8.1.2.2 AA-7000F
Points to check before ignition
Burner head If the burner slot is clogged or has Use the card provided as an
been widened, replace it with a new accessory.
one.
Pilot flame section If any soot has settled on the See 8.4 "Checking the Pilot
electrode, remove it. Flame Unit".
Drain tube Check that there is no damage or See 8.7 "Replacing the Drain
deformation. Tube".
AA-7000 8-3
Chapter 8 Maintenance
Flame monitor When the flow rate of the fuel gas has If the gas does not stop
been set to 0.8 L/min, check that the automatically there has been a
flame is extinguished and the gas failure. Implement the "In an
stops automatically. Emergency" and contact your
To specify the flow rate of fuel gas, see Shimadzu representative.
3.1.8 "Atomizer/Gas Flow Rate Setup".
Gas piping Check that there are no leaks in the See 8.5 "Checking for Gas
equipment piping and joints. Leaks".
Pressure regulator Check that there is nothing abnormal in See 8.5 "Checking for Gas
the operation of the pressure gauge Leaks" and 8.6 "Checking for
and check that there is no gas leak in Leaks of Pressure Regulators
any part. (Optional)".
8-4 AA-7000
8.2 Burner Maintenance (AA-7000F)
8.2 Burner Maintenance (AA-7000F)
When foreign objects such as dirt and contaminants adhere to the burner head, nebulizer or chamber interior,
the indicated value becomes unreliable and absorbance sensitivity is decreased. It is recommended that these
burner components be periodically cleaned.
WARNING
• Wear protective goggles and protective gloves to maintain the burner head.
If chemicals get into the eyes, there is a risk of loss of sight.
For details, see "Precautions on Handling Chemicals and Samples" in the introductory section.
• Do NOT remove parts inside the burner compartment during flame combustion.
Otherwise there will be a risk of gas leakage or flashback.
• Check that an O-ring is fitted, and check that the O-ring is not damaged or deformed.
If no O-ring is fitted, or if the O-ring is damaged or deformed, it could cause an accident.
To replace the O-ring, contact your Shimadzu representative.
AA-7000 8-5
Chapter 8 Maintenance
The construction of the burner is as shown below. For the function of each part, see 1.4.3 "Burner".
Burner head
Mixer Nebulizer
Chamber
Burner socket
Nebulizer Nebulizer
fixing screw fixing screw
U-tube
NOTE
• Do NOT use metal brushes to maintain the burner head.
This will scratch the burner head and shorten its replacemental interval.
WARNING
• Immediately after the flame has been extinguished the burner head is hot, so leave it for at least
30 minutes to cool before removing it.
If you touch the burner head immediately after the flame has been extinguished, you risk being burned.
If the slot of burner head is clogged by carbide or salts etc., the reduction flame will have fine irregularities when
the degree of blockage is small. When the slot is clogged more heavily, the flame splits as the left figure in Fig.
8.3 (The figure is exaggerated to illustrate). Before the flame becomes the state indicated in the figure,
extinguish the flame and then clean the inner wall of the slot by lightly rubbing it with the burner slot cleaning/
burner height check card.
8-6 AA-7000
8.2 Burner Maintenance (AA-7000F)
Clogged Normal
NOTE
• When measuring samples with high concentrations of coexistent components, such as salts etc, these
may adhere to the slot inner wall or inside of burner head. In some cases, orange colored flame may
flicker when the burner is ignited again. In such cases, spray distilled water until flickering stops.
If flickering does not easily disappear, after extinguishing the flame and cooling down the burner head
for 30 minutes or more, remove the burner head from the chamber; wash the inside with distilled water.
If it is extremely dirty, soak it in acid or an appropriate detergent overnight then brush the inner wall of
the slot with the burner slot cleaning/burner height check card.
• After washing, mount the burner head and adjust the burner position.
For details, see the section 8.3.1 "Burner Positioning Adjustment".
WARNING
• Do NOT disconnect the gas piping connected to the spray unit and disperser.
Otherwise there will be a risk of gas leakage.
Fig. 8.4 shows the construction of the nebulizer. The nebulizer comprises the spray unit and the disperser.
AA-7000 8-7
Chapter 8 Maintenance
Disperser
Spray unit
O-ring
Shield cover
CAUTION
• The capillary is a thin and easily broken part.
Take care not to apply too much force during this operation.
(1) While the flame is extinguished, insert the cleaning wire provided as an accessory into the capillary.
(2) Clean the inner wall of the capillary by repeatedly passing the cleaning wire in and out of it.
(3) Withdraw the cleaning wire, ignite the flame and spray distilled water.
(4) Install a sampling tube and check absorption sensitivity and stability using, for example, the standard
sample.
NOTE
If no improvement is seen after performing steps (1) to (4) above, inspect and replace the polyethylene tube.
8-8 AA-7000
8.2 Burner Maintenance (AA-7000F)
CAUTION
• If the polyethylene tube at the capillary of the spray unit has deteriorated or has come off,
sample suction or mounting and holding of the sampling tube will not be possible.
• Do NOT remove the capillary from the spray unit.
This could affect performance.
(1) While the flame is extinguished, take out the sampling tube.
(2) Turn the cap to the left and remove it.
(3) Inspect the polyethylene tube fitted to the capillary and, if it has deteriorated, remove it.
(4) Cut the accessory polyethylene tube to a length of approximately 5 mm and slide it carefully onto the
capillary while taking care not to bend the capillary.
NOTE
If it is difficult to slide the polyethylene tube on, increase the internal diameter at one of its ends by using a
pointed implement such as a toothpick.
(5) Once the polyethylene tube has been slid on, refit the cap as it was originally.
(6) Install the sampling tube.
(7) Ignite the flame and spray distilled water.
(8) Check absorption sensitivity and stability using, for example, the standard sample.
NOTE
If no improvement is seen after performing steps (1) to (8) above, inspect and clean the tip of the spray unit.
AA-7000 8-9
Chapter 8 Maintenance
(2) Pull the spray unit toward you without disconnecting the gas piping.
NOTE
Check whether there is any scratching or deformation of the O-ring.
For the position of the O-ring, see Fig. 8.4 "Detail of Nebulizer Section".
(3) Check the end of the spray unit and, if there is any contamination adhering to it, clean it off, for example
with a plastic brush.
NOTE
If no improvement is seen after performing steps (1) to (8) above, clean the disperser.
(2) Pull the body of the nebulizer toward you without disconnecting the gas piping.
NOTE
Check whether there is any scratching or deformation of the O-ring.
For the position of the O-ring, see Fig. 8.4 "Detail of Nebulizer Section".
8-10 AA-7000
8.2 Burner Maintenance (AA-7000F)
(3) Check the disperser and, if there is any contamination adhering to it, clean it off, for example with a plastic
brush.
NOTE
If no improvement is seen after performing steps (1) to (8) above, ask your Shimadzu representative to
replace the nebulizer.
WARNING
• Do NOT disconnect the piping that is connected to the nebulizer.
This could cause a gas leak.
CAUTION
• Do NOT use metal brushes.
This will scratch the chamber and shorten its replacement interval.
• On assembly after cleaning take care about the direction in which the mixer is mounted.
The mixer has a slightly tapered shape, so insert it in the direction in which its taper agrees with the
taper of the inside wall of the chamber. If it is not inserted in the correct direction, performance will be
affected.
(1) Remove the burner head (refer to 8.2.1 "Burner Head Maintenance").
(2) Remove the sampling tube that is connected to the nebulizer.
AA-7000 8-11
Chapter 8 Maintenance
(3) Remove the 2 nebulizer fixing screws, and pull the nebulizer toward you.
(4) Take the mixer out from the chamber.
(5) Wash the inside of the chamber and the mixer with distilled water.
NOTE
If there is heavy soiling, remove it with a brush for plastics.
Mixer Chamber
WARNING
• The O-rings are parts for periodic replacement.
If an O-ring is damaged or deformed it must be replaced. Failure to do so could cause accidents.
NOTE
The O-rings, which have to be replaced as maintenance parts, are provided in a set.
For details on the chemicals that can be used with each type of O-ring, see 10.1.2 "Flame Specifications".
8-12 AA-7000
8.2 Burner Maintenance (AA-7000F)
WARNING
• Wear protective goggles and protective gloves to maintain the parts.
If chemicals get into the eyes, there is a risk of loss of sight.
For details, see "Precautions on Handling Chemicals and Samples" in the Introductory section.
• Do NOT remove the joint between the chamber and the U-tube.
This could cause a gas leak.
Do NOT disconnect
CAUTION
• If you spill any waste liquid on the instrument, wipe it up immediately.
It could cause rusting or instrument failure.
Burner head
Burner socket
Drain tank
Connector
U-tube
Drain tube
Hose clamp
Cap
Drain sensor
AA-7000 8-13
Chapter 8 Maintenance
(1) In order to deal with the waste liquid in the drain tank and the U-tube, prepare a container with chemical
resistance to the waste liquid (such as a beaker).
(2) Remove the burner head.
(3) Remove the drain sensor's connector.
(4) Open the cap on the drain tank and take out the drain sensor.
(5) So as not to break the U-tube, tilt the drain tank forward gently while draining all of the waste liquid in the
drain tank into the waste liquid container.
NOTE
If there is heavy soiling, remove it with a plastic brush.
(9) Pour in distilled water through the burner socket and fill the U-tube.
(10) While pressing a clean rag against the U-tube's outlet, drain the liquid from the U-tube by bending it gently
so that it will not break.
8-14 AA-7000
8.2 Burner Maintenance (AA-7000F)
(11) Repeat the operations in steps (9) and (10) to clean the U-tube.
NOTE
If there is heavy soiling, remove it with a plastic brush.
(12) When the cleaning work is finished, return all the parts to their original situations.
NOTE
If you spill any waste liquid, wipe it up with a clean rag.
AA-7000 8-15
Chapter 8 Maintenance
8.3 Atomizer Positioning Adjustment
(1) Select an element that you usually use in the flame continuous method.
(2) In the [Optics Parameters] page, set the lamp mode to [NON-BGC] and turn on the lamp to perform the line
search.
(3) Check that the burner head is mounted securely, then adjust the burner to the 10 mm position by using the
burner up/down position adjusting knobs. Set the burner angle to 0°.
(4) Set the burner height checking card provided as an accessory at the center of the burner head so that the
scale on it faces the lamp.
Adjust the forward/backward position of the burner with the burner forward/backward adjusting knobs so
that the light beam shines directly above the burner slot.
(5) Move the burner height checking card to the right end of the burner head and, while turning the burner
head little by little by using the burner head angle adjusting lever, ensure that the light beam shines directly
above the burner slot.
(6) Set the burner height checking card at the center of the burner head again and check that the light beam is
directly above the burner slot.
The burner is now set at the most sensitive position in the forward/backward direction.
You should adjust the burner height in accordance with the measurement conditions.
(1) Select an element, which you usually use in flame continuous method.
(2) In the [Optics Parameters] page, set the lamp mode to [NON-BGC] and light on the lamp to perform the
line search.
(3) Select [Instrument]-[Maintenance]-[Burner Origin Position Adjustment] from the menu.
Then [Burner Origin Position Adjustment] dialog box opens.
(4) Verify that the burner head is securely mounted. Then click on [Up] and [Down] buttons to set the burner
height to about 10 mm. In addition, set the burner angle to 0°.
(5) Set the burner height checking card provided as an accessory at the center of the burner head so that the
scale on it faces the lamp.
(6) Using the [Forward] and [Backward] buttons, adjust the forward/backward position of the burner so that the
light beam shines directly over the burner slot.
(7) Move the burner height checking card to the right end of the burner head without changing the direction in
which it is facing and, while turning the burner head little by little by using the burner head angle adjusting
lever, ensure that the light beam shines directly above the burner slot.
(8) Set the burner height checking card at the center of the burner head again and check that the light beam is
directly above the burner slot.
(9) Click on the [Up] and [Down] buttons to set the burner height to 10 mm. Set the check card on the burner.
Adjust the burner height so that the beam spot on the paper is semicircular as shown in Fig. 8.6.
8-16 AA-7000
8.3 Atomizer Positioning Adjustment
Beam spot
10 mm
Burner head
AA-7000 8-17
Chapter 8 Maintenance
8.3.2.1 AA-7000G
(1) Select an element that you usually use in the furnace method.
(2) On the [Optics Parameters] page, set the lamp mode to [NON-BGC].
Press [Cancel] in response to the message "Line Search/Beam Balance is necessary" in this procedure.
(3) From the Menu, select [Instrument]-[Maintenance]-[Furnace Origin Position Adjustment].
This opens the [Furnace Origin Position Adjustment] dialog box.
(4) Click on [Line Search] to open [Line Search/Beam Balance] and execute Line Search/Beam Balance.
(5) After both Line Search and Beam Balance have been completed successfully, click on the [Close] button.
(6) Using the manual control knob, adjust the horizontal and vertical positions to minimize the measured value
in the [Furnace Origin Position Adjustment] dialog box.
NOTE
Immediately after the lamp has been on the baseline may not be stable. If this is the case, wait until the
baseline has stabilized and then carry out position adjustment.
NOTE
Immediately after the lamp has been on the baseline may not be stable. If this is the case, wait until the
baseline has stabilized and then carry out position adjustment.
(7) After adjusting the position, click on [Origin Memory]. The current furnace position is memorized as
"Forward/Backward=0" and "Up/Down=0".
8-18 AA-7000
8.4 Checking the Pilot Flame Unit
8.4 Checking the Pilot Flame Unit
With extended use of the instrument, soot may accumulate on the electrode in the pilot flame unit. When soot
builds up in this area, it may obstruct the pilot flame, making it difficult to ignite the burner. In the worst case, the
pilot flame may remain lit inside the instrument, causing a fire hazard.
(4) If soot has accumulated on the electrode, scrape it off with a slender, rigid object, such as the tip of a
flathead screwdriver. Not much force is needed to remove the soot.
Soot
Flathead screwdriver
Electrode
AA-7000 8-19
Chapter 8 Maintenance
8.5 Checking for Gas Leaks
A constant check is conducted for gas leakage from the fuel gas tube inside the gas control unit.
This section describes the method for inspecting for leakage from the gas piping (customer's equipment), the
gas hose (standard accessory), and the gas piping that includes the gas control section inside the instrument.
WARNING
• If a gas leak occurs, stop using the instrument immediately and request your Shimadzu
representative to inspect the instrument.
Continuing to use the instrument without taking action could lead to an accident.
Carry out an inspection at least once a month by following the procedure below. Note that the gas leakage
inspection described here is based on the recommended piping example in 10.6.3 (3) "Gas piping".
For details, see 10.6.3 (3) "Gas piping".
(1) Turn the power switch of the AA-7000 OFF. Also start the compressor.
(2) Open the main valves on the gas cylinder and compressor, and all the stop cocks.
(3) Verify that the gas pressure is set correctly.
(4) Wait for at least 5 seconds, then close the main valves.
(5) Read the indications of the pressure gauge between the main valve and the instrument in each case.
(6) Read the indication of each pressure gauge after an interval of 30 minutes.
If the drop in pressure over 30 minutes at the fuel gas side is greater than 0.01 MPa, or if the drop in
pressure at the assist gas side is greater than 0.02 MPa, it is judged that there is a gas leak.
NOTE
• If it is judged that there is a gas leak, apply soapy water or leak detection fluid (optional) at each
connection between the gas cylinder or compressor and the gas control unit and burner to check the
location of the leak.
• If a gas leak has occurred at a connection, make the connection again. If it is judged that there is a gas
leak inside the gas control unit, stop using the instrument and contact your Shimadzu representative.
8-20 AA-7000
8.6 Checking for Leaks of Pressure Regulators (Optional)
8.6 Checking for Leaks of Pressure Regulators
(Optional)
WARNING
1. If a mistake is made in the piping, it may cause flashback on ignition.
2. Always set the gas supply pressures at the specified values.
3. Never use a broken regulator. This may result in gas leaks.
4. If nitrous oxide is used, use the dedicated pressure regulator.
AA-7000 8-21
Chapter 8 Maintenance
Stop cock
Connecting nut
8-22 AA-7000
8.7 Replacing the Drain Tube
8.7 Replacing the Drain Tube
When the drain tube becomes old it may rupture, allowing drain to leak out. Replace the drain tube by following
the procedure below.
(1) Remove the old polythene tube connected to the outlet of the drain tank.
(2) Connect the new polythene tube.
(3) Prepare a container to receive the drain from the instrument.
(4) Cut the polythene tube to the appropriate length.
Make sure that the end of the tube is not submerged in the waste liquid in the container.
(5) Supply water a little at a time through the burner socket until water overflows from the drain tank. If the
water level is too low the liquid level sensor actuates and ignition will not be possible.
Drain tank
Drain tube
CAUTION
• Be sure to lower the drain tube as smoothly as possible. Also ensure that the end of the tube is
not submerged in the waste liquid in the container.
If the waste liquid cannot flow smoothly the level of noise will be increased and this may have an
adverse affect on repeatability.
AA-7000 8-23
Chapter 8 Maintenance
8.8 Replacing the Deuterium Lamp
Part No 062-65055-05
Type L6380
WARNING
• Wait at least 30 minutes after turning the D2 lamp off before replacing the lamp.
Otherwise you could be burned.
CAUTION
1. Handle the new lamp using gloves so as not to leave fingerprints on the light beam window. Otherwise,
the window is stained with the fingerprints when it is hot, and as the result the light transmission will be
reduced. If contaminated, clean it with alcohol or the like.
2. When detaching or attaching the cover of the deuterium lamp house, be very careful not to hit the
protruding upper edge of the deuterium lamp against the cover rear side. It may cause a vacuum leak of
the bulb.
8-24 AA-7000
8.8 Replacing the Deuterium Lamp
AA-7000 8-25
Chapter 8 Maintenance
(5) When the message "The operator is about to set lamp usage time to zero. Are you sure?" is displayed,
click [Yes].
(6) Check that the [Used Time] of the changed lamp is [0], then click [OK] on the [Lamp History] dialog box.
(7) As shown below, remove the two screws to detach the lamp cover. When the cover is removed, the
deuterium lamp will appear as shown in Fig. 8.11.
(8) Pull the deuterium lamp slowly upward and out of its socket.
(9) Insert a new deuterium lamp into the socket. Check that the plastic part of the electrode makes tight
contact with that of the lamp socket.
8-26 AA-7000
8.8 Replacing the Deuterium Lamp
Adjusting screw
Fixing screw
NOTE
Immediately after the lamp has been on, the baseline may not be stable. If this is the case, wait until the
baseline has stabilized and then carry out position adjustment.
(9) Tighten the 2 deuterium lamp fixing screws, and click on [OK] to close the [D2 Lamp Adjustment] dialog
box.
NOTE
After replacing the deuterium lamp, exit the PC software and turn off the power to the instrument.
AA-7000 8-27
Chapter 8 Maintenance
8.9 Method for Replacing the Hollow Cathode
Lamp
8-28 AA-7000
8.9 Method for Replacing the Hollow Cathode Lamp
(8) When the message "The operator is about to set lamp usage time to zero. Are you sure?" is displayed,
click [Yes].
AA-7000 8-29
Chapter 8 Maintenance
(9) Check that the [Used Time] of the changed lamp is "0", then click [OK] on the [Lamp History] dialog box.
8-30 AA-7000
8.9 Method for Replacing the Hollow Cathode Lamp
AA-7000 8-31
Chapter 8 Maintenance
8.10 Maintenance Parts
The parts for periodic replacement are indicated below. All parts for periodic replacement are consumable
parts.
NOTE
Parts listed below relate to the safety of the product. Be sure to replace the parts periodically.
Standard
Part Name Part No. Remarks Replacement
Interval
Standard
Part Name Part No. Remarks Replacement
Interval
8-32 AA-7000
8.11 Repair Parts
8.11 Repair Parts
Power cable (for 100 V, 120 V) 071-60816-12 For Japan and North America
AA-7000 8-33
Chapter 8 Maintenance
8-34 AA-7000
Chapter 9
Troubleshooting
CONTENTS
AA-7000 9-1
Chapter 9 Troubleshooting
9.1 Failure to Ignite
When it is not possible to ignite the flame of the AA-7000F, take the following corrective action in accordance
with the symptoms as follows.
Nothing happens in Either communications Check the power switch Turn the power switch
response to the ignition between the instrument and indicator at the ON. Select [Instrument]
operation. No error and the PC are OFF or bottom right of the front - [Connect] from the
message is displayed. the instrument's power of the instrument. WizAArd menu to
is OFF. complete initialization.
See 2.1.1 "Activation".
Gas leakage detection The status on the [Gas Wait until the gas
is being executed. Controller Status] dialog leakage inspection is
box is [Checking]. completed.
The remaining time for See 2.7 "Checking the
gas leakage detection is Gas Controller Status
indicated by the status (AA-7000F)".
bar display.
The pilot flame The supply pressure of Ignition will be possible Check if the supply
establishes, but the burner the fuel gas is actually if the supply pressure of pressure of the fuel gas
goes out immediately after low. the fuel gas is is 0.09 MPa. It is
igniting. Only the following increased. necessary that this set
error message is pressure is maintained
displayed: [Fuel gas while the gas is flowing.
pressure is too low].
The pilot flame establishes The ratio of fuel gas in Ignition will be possible Increase the flow rate of
but it is difficult to get the the mixture is too low if the flow rate of fuel the fuel gas, ignite the
burner to ignite. When and the flame blows gas is increased. flame, then decrease
ignition fails, the message out. the flow rate later.
"Flame has been See 3.1.8 "Atomizer/
extinguished." is Gas Flow Rate Setup".
displayed.
The pilot flame is too The flame is actually too Adjust the pilot flame.
small to reach the small.
burner.
The pilot flame fails to The igniter has failed. The igniter does not Repair the igniter.
establish. Gas is flowing. discharge.
When ignition fails, the
The electromagnetic The igniter does Repair the
message "Flame has been
valve for the pilot has discharge but no pilot electromagnetic valve
extinguished." is
failed. flame is generated. for the pilot.
displayed.
9-2 AA-7000
9.2 Responding to Trouble
9.2 Responding to Trouble
This section describes the types of trouble that could occur while using an AA-7000 series instrument, and the
corrective actions to take against them.
When any kind of trouble occurs, first see Chapter 8 "Maintenance" and Chapter 9 "Troubleshooting". If this
does not resolve the trouble, contact your Shimadzu representative.
The indicator does not The power plug or power cable is Plug in the power plug and power
light when the power disconnected. cable.
switch is turned ON.
A wavelength origin error There is something blocking the light If there is something blocking the light
occurs at initialization. path in the atomizer. path, remove it.
The position of the deuterium lamp is Adjust the position of the deuterium
not adjusted appropriately. lamp.
See 8.8.2.2 "Adjusting Position of
Deuterium Lamp".
The lit time of the deuterium lamp has Replace the deuterium lamp.
exceeded the cumulative life time of See 8.8 "Replacing the Deuterium
the lamp. Lamp".
The ASC-7000 or GFA- The power switch of the ASC-7000 or Turn the power switch ON.
7000 is not connected at GFA-7000 is OFF. See 2.1.1 "Activation".
initialization.
The ASC-7000 or GFA-7000 Connect the communications cable.
communications cable is See 1.4.1 "Operation Switches/
disconnected. Connectors".
The signal-to-noise ratio is Either the hollow cathode lamp for the Correctly install the hollow cathode
bad (there is a lot of target element has not been installed, lamp for the target element.
baseline noise). or it has been installed in a socket See 1.4.4 "Hollow Cathode Lamp
that differs from the analysis Turret" and 8.9 "Method for Replacing
conditions. the Hollow Cathode Lamp".
The window plates at left and right of Wipe off the soiling with a soft cloth
the burner compartment are soiled. moistened with alcohol.
The slit width setting is not Change the slit width to suit the target
appropriate. element by referring to the standard
analysis conditions.
See 10.2 "Measurement Conditions
Table for Flame Atomic Absorption
Analysis".
For furnace analysis, refer to 6.2
"Standard Analysis Conditions" in
GFA-7000 Instruction Manual.
The lit time of the deuterium lamp has Replace the deuterium lamp.
exceeded the cumulative life time of See 8.8 "Replacing the Deuterium
the lamp. Lamp".
AA-7000 9-3
Chapter 9 Troubleshooting
The signal-to-noise ratio is The lit time of the hollow cathode Replace the hollow cathode lamp.
bad (there is a lot of lamp has exceeded the cumulative See 8.9 "Method for Replacing the
baseline noise). life time of the lamp. Hollow Cathode Lamp".
The line search / beam There is something blocking the light If there is something blocking the light
balancing failed. path in the atomizer. path, remove it.
Either the hollow cathode lamp for the Correctly install the hollow cathode
target element has not been installed, lamp for the target element.
or it has been installed in a socket See 1.4.4 "Hollow Cathode Lamp
that differs from the analysis Turret" and 8.9 "Method for Replacing
conditions. the Hollow Cathode Lamp".
The window plates at left and right of Wipe off the soiling with a soft cloth
the burner compartment are soiled. moistened with alcohol.
The slit width setting is not Change the slit width to suit the target
appropriate. element by referring to the standard
analysis conditions.
See 10.2 "Measurement Conditions
Table for Flame Atomic Absorption
Analysis".
For furnace analysis, refer to 6.2
"Standard Analysis Conditions" in
GFA-7000 Instruction Manual.
The lamp current value setting is not Set the lamp current value that is
appropriate. appropriate for the target element by
referring to the standard analysis
conditions.
See 10.2 "Measurement Conditions
Table for Flame Atomic Absorption
Analysis".
For furnace analysis, refer to 6.2
"Standard Analysis Conditions" in
GFA-7000 Instruction Manual.
The lamp mode has been set to BGC- Set the lamp mode to NON-BGC or
D2 for an element that does not have BGC-SR (a hollow cathode tube
an analysis line in the wavelength compatible with the SR method is
range for which background required).
compensation using the deuterium
lamp is possible (185 to 430 nm).
The lit time of the hollow cathode Replace the deuterium lamp.
lamp has exceeded the cumulative See 8.8 "Replacing the Deuterium
life time of the lamp. Lamp".
9-4 AA-7000
9.2 Responding to Trouble
The line search / beam The lit time of the hollow cathode Replace the hollow cathode lamp.
balancing failed. lamp has exceeded the cumulative See 8.9 "Method for Replacing the
life time of the lamp. Hollow Cathode Lamp".
The absorbance is −1 The light paths of the hollow cathode Adjust the position of the deuterium
(minus one). lamp and the deuterium lamp do not lamp.
coincide. See 8.8.2.2 "Adjusting Position of
(When the BGC-D2 mode is set) Deuterium Lamp".
AA-7000 9-5
Chapter 9 Troubleshooting
9.2.2 AA-7000F
The absorbance or energy Either the hollow cathode lamp for the Correctly install the hollow cathode
value has fallen very target element has not been installed, lamp for the target element.
considerably, or it does not or it has been installed in a socket See 1.4.4 "Hollow Cathode Lamp
move from zero. that differs from the analysis Turret".
conditions.
The [AUTO ZERO] button has been Press the [AUTO ZERO] button while
pressed by mistake during spraying the solvent instead of the
measurement. sample. Then resume measurement.
The lit time of the deuterium lamp has Replace the deuterium lamp.
exceeded the cumulative life time of See 8.8 "Replacing the Deuterium
the lamp. Lamp".
The lit time of the hollow cathode Replace the hollow cathode lamp.
lamp has exceeded the cumulative See 8.9 "Method for Replacing the
life time of the lamp. Hollow Cathode Lamp".
The slot of the burner head is not on Adjust the position of the atomizer in
the optical axis. the forward/backward direction or the
up/down direction to adjust the
positional relationship between the
burner slot and the optical axis.
See 3.1.8 "Atomizer/Gas Flow Rate
Setup".
The flame is not stable. Deposits have become attached to Wash the burner head.
the slot in the burner head. See 8.2.1 "Burner Head
Maintenance".
The volume of gas remaining in the Replace the cylinder with a new one.
dissolved acetylene cylinder is low.
9-6 AA-7000
9.2 Responding to Trouble
When using the high- N2O gas is not being supplied. Open the main valve on the N2O gas
temperature burner head cylinder and supply N2O gas at the
(option), the instrument will stipulated pressure.
not change from an air- See 10.6.3 "Gas Requirements".
acetylene (Air-C2H2) flame
The flame type is set to Air-C2H2. Set the flame type to N2O-C2H2 on
to a nitrous oxide-
the gas condition setting screen.
acetylene (N2O-C2H2)
flame.
The absorbance is −1 Light radiation derived from the flame Carry out a line search while spraying
(minus one). or sample is exerting an influence. the blank solution.
AA-7000 9-7
Chapter 9 Troubleshooting
9.3 When the Buzzer Sounds
The events that cause the buzzer to sound while using an AA-7000 series unit, and the action to take in each
case, are described below.
NOTE
When the power to the instrument is turned ON, the buzzer sounds briefly once: "pip". After that, self
diagnosis is performed and if an abnormality is found the buzzer sounds three times: "pip pip pip".
WARNING
• When a gas leak has been detected, stop using the instrument immediately.
Leaked gas could be ignited, causing a fire.
NOTE
If no gas leak is detected as the result of a gas leakage inspection, the message shown below is displayed.
Click [OK] and you will be able to ignite the flame.
9-8 AA-7000
9.3 When the Buzzer Sounds
• If this error occurs even though fuel gas is being supplied to the instrument, stop using the instrument and
contact your Shimadzu representative.
• If this error occurs even when the drain tank is topped up with water, stop using the instrument and contact
your Shimadzu representative.
9.3.3 When the Buzzer Sounds Four Times (beep, beep, beep, beep)
A flashback has occurred.
AA-7000 9-9
Chapter 9 Troubleshooting
• After confirming safety in the vicinity, display the [Gas Controller Status] dialog box and click the [Reset]
button.
• If this error occurs even though assist gas is being supplied to the instrument and the flame ignites, stop
using the instrument and contact your Shimadzu representative.
• If this error occurs even though there is nothing obstructing the flame monitor, stop using the instrument
and contact your Shimadzu representative.
9-10 AA-7000
9.3 When the Buzzer Sounds
• Lessen the amount of external light and illumination entering the burner compartment to make the inside of
the chamber dark.
• If this error occurs even though the inside of the burner compartment has been made dark, stop using the
instrument and contact your Shimadzu representative.
AA-7000 9-11
Chapter 9 Troubleshooting
9.4 Error Messages
NOTE
Before contacting your Shimadzu representative, record the following items.
1. Content of error message
2. Status in which the error message is displayed (indication screen, performed operation, measurement
file, etc.)
3. Instrument information displayed at the upper in the initialization screen (model names of AA/ASC/GFA,
ROM version and serial No.)
4. AA software version No. ([Help]-[About Wizard] menu)
9-12 AA-7000
9.4 Error Messages
AA-7000 9-13
Chapter 9 Troubleshooting
9-14 AA-7000
9.4 Error Messages
AA-7000 9-15
Chapter 9 Troubleshooting
9-16 AA-7000
9.4 Error Messages
AA-7000 9-17
Chapter 9 Troubleshooting
9-18 AA-7000
9.4 Error Messages
AA-7000 9-19
Chapter 9 Troubleshooting
9-20 AA-7000
9.4 Error Messages
AA-7000 9-21
Chapter 9 Troubleshooting
9-22 AA-7000
9.4 Error Messages
(4) The light intensity becomes • Increase the hollow cathode lamp
smaller because of the exhaustion current (Low) (pay attention to the
of hollow cathode lamp. max. current).
• Widen the slit width (pay attention
to neighboring lines).
(3) Set [Wavelength] correctly in
[Optics Parameters] page.
(4) Change the hollow cathode lamp.
AA-7000 9-23
Chapter 9 Troubleshooting
9-24 AA-7000
9.4 Error Messages
AA-7000 9-25
Chapter 9 Troubleshooting
9-26 AA-7000
9.4 Error Messages
AA-7000 9-27
Chapter 9 Troubleshooting
9-28 AA-7000
9.4 Error Messages
AA-7000 9-29
Chapter 9 Troubleshooting
9-30 AA-7000
9.4 Error Messages
AA-7000 9-31
Chapter 9 Troubleshooting
9-32 AA-7000
9.4 Error Messages
AA-7000 9-33
Chapter 9 Troubleshooting
9-34 AA-7000
9.4 Error Messages
AA-7000 9-35
Chapter 9 Troubleshooting
9-36 AA-7000
Chapter 10
Technical Data
CONTENTS
AA-7000 10-1
Chapter 10 Technical Data
10.1 Specifications
The specifications of the AA-7000 series are as follows. The AA-7000 series does not conform to IEC60601.
10-2 AA-7000
10.1 Specifications
Peak data processing range Peak data processing range can be changed with
peak height and peak area mode.
Table Data Processing Functions Actual concentration calculation using Weight factor,
Dilution factor, Volume factor and Correction factor.
AA-7000 10-3
Chapter 10 Technical Data
Power Requirements AC100, 120, 220, 230 V selectable, 230 VA, 50/60 Hz
Additional power for PC is necessary.
Burner Head 10 cm slot made of Titanium (5 cm slot made of Titanium for N2O-
C2H2 flame is optional item.)
Positioning AA-7000F
• Manual Adjustment for back-for and up-down positions
AA-7000F (when equipped with Auto Atomizer Changer (optional))
• Automatic switching between burner and furnace by motor drive
• Automatic search for optimum burner height
Gas Controller Flow Rate Control • Automatic flow rate setting for fuel gas (0.1 L/min increments)
• Manual flow rate setting for support gas (when equipped with
optional instruments)
• Automatic searching for optimum gas flow rate
10-4 AA-7000
10.1 Specifications
WARNING
• Check that the parts of the atomizer are resistant to the chemicals to be used.
Using such chemicals will cause accidents.
• Replace each part at the specified intervals.
The chemical resistance and conditions of use of the materials used in the atomizer of AA-7000F instruments
are as follows.
Before making a measurement, check that there is resistance to the chemicals to be used by referring to the
table below.
The chemical resistance stated is that when the chemical is at room temperature.
Water *1
Ethanol
Hydrochloric acid
Nitric acid
Sulfuric acid
Hydrofluoric acid
Perchloric acid
AA-7000 10-5
Chapter 10 Technical Data
CAUTION
Chemicals that are not covered in the table above cannot be used.
NOTE
When a mixture of two or more types of chemical is used, abide by the stricter conditions.
Heating Control Method Drying: Current control method (with automatic temperature calibration
function)
Ashing/Atomizing: Optical temperature control method
Positioning AA-7000G
• Manual Adjustment for back-for and up-down positions
AA-7000F (when equipped with Auto Atomizer Changer (optional))
• Automatic switching between the burner and furnace by motor drive
10-6 AA-7000
10.1 Specifications
Repeatability ≤ 2.00 %
(No. of repetition 5 times, confidence coefficient 95%)
Stability ≤ 6.0%
Repeatability ≤ 2.5 %
(No. of repetition 5 times, confidence coefficient 95%)
NOTE
The performance is premised on the following conditions.
• At least 30 minutes has elapsed since the power to the instrument that includes the option was turned
ON.
• Each of the lamps used have been lit for at least 10 minutes in preparation.
• The cumulative operation time of each of the lamps is within the guaranteed service life.
AA-7000 10-7
Chapter 10 Technical Data
Specifications
Peripherals Monitor
Keyboard
Printer
NOTE
The AA-7000 series software does not support "switching users".
10-8 AA-7000
10.2 Measurement Conditions Table for Flame Atomic
10.2 Measurement Conditions Table for Flame
Absorption Analysis
Atomic Absorption Analysis
NOTE
1. Most of these measurement conditions are included in the software as standard analysis conditions, but
the optimal measurement conditions vary depending upon the properties of the sample. (A single
element each is assumed as a standard condition. Therefore, if there are multiple conditions, one of
them is included in the software.)
2. <HVG-1> represents the Hydride Vapor Generator (optional).
Wave
L233 L2433 Slit Flow Burner. H
Element length Flame Type
(mA) (mA) (nm) (L/min) (mm)
(nm)
Ag 328.1 10 10/400 0.7 Air-C2H2 2.2 7
Al 309.3 10 10/600 0.7 N2O-C2H2 7.0 11
As (H) 193.7 12 12/500 0.7 Air-C2H2 2.0 <HVG-1>
Au 242.8 10 10/400 0.7 Air-C2H2 1.8 7
B 249.7 16 10/500 0.2 N2O-C2H2 7.7 11
Ba 553.5 16 12/600 0.2 N2O-C2H2 6.7 11
Be 234.9 16 10/600 0.7 N2O-C2H2 7.0 11
Bi (H) 223.1 10 10/300 0.7 Air-C2H2 2.0 <HVG-1>
Bi 223.1 10 10/300 0.7 Air-C2H2 2.2 7
Ca (1) 422.7 10 10/600 0.7 Air-C2H2 2.0 7
Ca (2) 422.7 10 10/600 0.7 N2O-C2H2 6.5 11
Cd 228.8 8 8/100 0.7 Air-C2H2 1.8 7
Co 240.7 12 12/400 0.2 Air-C2H2 1.6 7
Cr 357.9 10 10/600 0.7 Air-C2H2 2.8 9
Cs 852.1 16 0.7 Air-C2H2 1.8 7
Cu 324.8 8 10/500 0.7 Air-C2H2 1.8 7
Dy 421.2 14 15/600 0.2 N2O-C2H2 7.0 11
Er 400.8 14 15/500 0.7 N2O-C2H2 7.0 11
Eu 459.4 14 10/600 0.7 N2O-C2H2 7.0 11
Fe 248.3 12 12/400 0.2 Air-C2H2 2.2 9
Ga 287.4 4 4/400 0.2 Air-C2H2 1.8 7
Gd 368.4 12 0.2 N2O-C2H2 7.0 11
Ge 265.2 18 20/500 0.2 N2O-C2H2 7.8 11
Hf 307.3 24 20/600 0.2 N2O-C2H2 7.0 11
Hg 253.7 4 0.7 By the cold vapor mercury
technique
Ho 410.4 14 10/600 0.2 N2O-C2H2 7.0 11
Ir 208.8 20 0.2 Air-C2H2 2.2 7
K 766.5 10 8/600 0.7 Air-C2H2 2.0 7
La 550.1 18 18/600 0.7 N2O-C2H2 7.5 11
Li 670.8 8 8/500 0.7 Air-C2H2 1.8 7
Lu 360.0 14 0.7 N2O-C2H2 7.0 11
AA-7000 10-9
Chapter 10 Technical Data
Wave
L233 L2433 Slit Flow Burner. H
Element length Flame Type
(mA) (mA) (nm) (L/min) (mm)
(nm)
Mg 285.2 8 8/500 0.7 Air-C2H2 1.8 7
Mn 279.5 10 10/600 0.2 Air-C2H2 2.0 7
Mo 313.3 10 10/500 0.7 N2O-C2H2 7.0 11
Na 589.0 12 8/600 0.2 Air-C2H2 1.8 7
Nb 334.9 24 0.2 N2O-C2H2 7.0 11
Ni 232.0 12 10/400 0.2 Air-C2H2 1.6 7
Os 290.9 14 0.2 N2O-C2H2 7.0 11
Pb (1) 217.0 12 8/300 0.7 Air-C2H2 2.0 7
Pb (2) 283.3 10 8/300 0.7 Air-C2H2 2.0 7
Pd 247.6 10 10/300 0.7 Air-C2H2 1.8 7
Pr 495.1 14 0.7 N2O-C2H2 7.0 11
Pt 265.9 14 10/300 0.7 Air-C2H2 1.8 7
Rb 780.0 14 0.2 Air-C2H2 1.8 7
Re 346.0 20 0.2 N2O-C2H2 7.0 11
Ru 349.9 20 20/600 0.2 Air-C2H2 1.8 7
Sb (H) 217.6 13 15/500 0.7 Air-C2H2 2.0 <HVG-1>
Sb 217.6 13 15/500 0.7 Air-C2H2 2.0 7
Sc 391.2 10 0.2 N2O-C2H2 7.0 11
Se (H) 196.0 23 15/300 0.7 Air-C2H2 2.0 <HVG-1>
Se 196.0 23 15/300 0.7 Ar-H2 [3.7] 15
Si 251.6 15 10/500 0.7 N2O-C2H2 7.7 11
Sm 429.7 14 15/600 0.2 N2O-C2H2 7.0 11
Sn (H) 286.3 10 20/500 0.7 Air-C2H2 2.0 <HVG-1>
Sn (1) 224.6 10 20/500 0.7 Air-C2H2 3.0 9
Sn (2) 286.3 10 20/500 0.7 Air-C2H2 3.0 9
Sn (3) 224.6 10 20/500 0.7 N2O-C2H2 6.8 11
Sn (4) 286.3 10 20/500 0.7 N2O-C2H2 6.8 11
Sr 460.7 8 6/500 0.7 Air-C2H2 1.8 7
Ta 271.5 18 0.2 N2O-C2H2 7.0 11
Tb 432.6 10 0.2 N2O-C2H2 7.0 11
Te (H) 214.3 14 15/400 0.2 Air-C2H2 2.0 <HVG-1>
Te 214.3 14 15/400 0.2 Air-C2H2 1.8 7
Ti 364.3 12 10/600 0.7 N2O-C2H2 7.8 11
Tl 276.8 6 0.7 Air-C2H2 1.8 7
V 318.4 10 10/600 0.7 N2O-C2H2 7.5 11
W 255.1 24 0.2 N2O-C2H2 7.7 11
Y 410.2 14 10/600 0.7 N2O-C2H2 7.5 11
Yb 398.8 10 5/200 0.7 N2O-C2H2 7.5 11
Zn 213.9 8 10/300 0.7 Air-C2H2 2.0 7
Zr 360.1 18 0.2 N2O-C2H2 7.5 11
10-10 AA-7000
10.3 Analysis Line Wavelength Table for Flame Emission
10.3 Analysis Line Wavelength Table for Flame Analysis
Emission Analysis
Element Wave length (nm) Element Wave length (nm) Element Wave length (nm)
Ag 328.1 Hf 531.2 Re 346.1
Al 396.2 Hg 253.7 Rh 343.5
As 193.7 In 451.1 Ru 372.8
Au 267.6 Ho 410.4 Sc 402.4
B 518.0* Ir 550.0 Si 251.6
Ba 455.4 K 766.5 Sm 476.0
Be 234.9 La 442.0 Sn 317.5
Bi 306.8 Li 670.8 Sr 460.7
Ca 422.7 Lu 451.9 Ta 474.0
Cd 326.1 Mg 285.2 Tb 534.0*
Ce 494.0* Mn 403.3 Te 486.6
Co 345.4 Mo 390.3 Ti 334.9
Cr 425.4 Na 589.0 Th 492.0
Cs 455.5 Nb 405.9 Tl 377.6
Cu 324.8 Nd 492.5 U 544.8
Dy 404.6 Ni 352.5 V 437.9
Er 400.8 Os 442.1 W 430.2
Eu 459.4 Pb 405.8 Y 597.2
Fe 372.0 Pd 363.5 Yb 398.8
Ga 417.2 Pr 495.1 Zn 636.2
Gd 622.0 Pt 265.9 Zr 360.1
Ge 265.1 Rb 794.8
* Band spectrum
Since the adsorption wavelength range is wide, the analysis line is partially set within that range.
AA-7000 10-11
Chapter 10 Technical Data
10.4 Optional Parts
The optional parts available for this instrument are listed below.
High temperature burner head 206-77530-91 Titanium, N2O-C2H2 5 cm slot for flame
Flow meter kit 206-77617-91 Float type flow meter for assist gas
Mist separator kit 206-52458-91 Required at the time of using a different air
compressor described above.
Microsampling kit 206-77540-91 This is a kit that makes it possible to use the
flame micro sampling method. An ASC-7000 or
ASK-7000 unit (or the ASC stand kit) is required
separately.
O-ring set 206-77620-92 Set of O-rings for use with organic solvents
For details, see 10.1.2.1 "Chemicals That can
be Used".
Waste liquid hook 206-77565-91 Clamps the drain tube to the waste liquid
container.
Gas leak detection fluid 670-11514 Used for gas leak test
10-12 AA-7000
10.4 Optional Parts
Cooling water circulating unit CA- 044-01809-03 Operating temperature range: −20 to +30°C
1112
Tube ASSY for cooling water 206-51028-91 Used when the cooling water is drawn from tap
water
Regulator ASSY 206-86147-91 Pressure reducing valve for cooling water, used
when the cooling water is drawn from tap water
10.4.3 Autosampler
Extended unit for furnace analysis 206-77550-91 For both flame and furnace analyses
ASK-7000
Nozzle ASSY, HVG 206-67563 Required when using ASC-6100F with HVG-1
AA-7000 10-13
Chapter 10 Technical Data
NOTE
This lamp cannot be used for the high-speed self reversal method.
10-14 AA-7000
10.4 Optional Parts
AA-7000 10-15
Chapter 10 Technical Data
10-16 AA-7000
10.4 Optional Parts
NOTE
This lamp cannot be used for the high-speed self reversal method.
AA-7000 10-17
Chapter 10 Technical Data
10-18 AA-7000
10.5 Instrument Placement and Site Requirements
10.5 Instrument Placement and Site Requirements
WARNING
• Take the weight of the entire measuring system into account when installing the product.
Install this product on a desk or stand that can easily bear the weight of the entire measuring system
and is flat and stable. If these conditions are not met, accidents in which the product topples over or falls
may occur.
CAUTION
• Make sure that it is not exposed to strong outdoor daylight.
The AA-7000 series are equipped with a safety system using an optical sensor. Exposure to strong
outdoor daylight may interfere with normal operation of the flame extinction safety system for monitoring
flame combustion (Flame Monitor). When using incandescent lamp or other heat light sources near the
main unit, select the installation site where the luminous intensity by the light source only is below
400 Lx. If not available, don't allow the direct light from the light source to come into the burner
compartment.
• If the temperature changes by 1 °C, the absorbance may change by 0.010 Abs maximum.
To carry out such long-hour measurement as may be affected by temperature changes, execute AUTO
ZERO during the measurement if necessary.
In the case of manual flame measurement (not using ASC), you can execute AUTO ZERO at any time
by clicking on [AUTO ZERO] button on the left lower of the main window. In the case of automatic flame
measurement (using ASC), if set "AUTO ZERO" or "RINSE" in [Action] field on the MRT work sheet,
AUTO ZERO can be executed during the nozzle rinsing. In the case of furnace measurement, setting is
not necessary because the instrument automatically execute AUTO ZERO just before measurement.
AA-7000 10-19
Chapter 10 Technical Data
• Since gas and water pipes cables are connected at the back of the AA main unit, there must be a space of
about 15 to 20 cm from the back of the AA main unit to a wall.
• There must be more than 30 cm of space from the right side of the AA main unit so that the HCL cover on
the right side of the AA-7000 series can be opened/closed.
Wall
150 to 200
588
870
280
AA-7000
714
GFA-7000
ASC-7000
390
340
(Unit: mm)
960
10-20 AA-7000
10.6 Equipment Requirements
10.6 Equipment Requirements
Allowable voltage range Within ± 10% (Free from sudden voltage change)
NOTE
The power requirement for a PC system is not shown in the table.
The points to note when supplying the cooling water from the city water are given below.
• A water outlet with sink must be located within 7 m of the instrument.
• A flow rate of 0.6 to 1.5 L/min is required. Use a water pressure of 0.08 to 0.15 MPa. If this flow rate is not
met, the safety device is actuated to stop operation.
If the water pressure exceeds 0.17 MPa, use the specially provided pressure reducing valve (regulator
assembly, P/N 206-86147-91).
• Maintain the water temperature in the range between 10 °C and 30 °C. If the water temperature is less
than 10 °C or more than 30 °C, use a cooling water circulating unit (optional) rather than piped water. If the
water temperature is greatly different from the room temperature, condensation may occur in the graphite
furnace. If the water temperature drifts out of this range, the safety device is actuated to stop operation.
CAUTION
To be prepared in case there is water leakage, the water outlet must be equipped with a sink.
If there is no sink, the equipment may be caused to fail by outflowing water. There is also the possibility of
material damage at the installation site.
NOTE
When using a cooling water circulating unit (optional), be sure to use a cooler connecting kit.
AA-7000 10-21
Chapter 10 Technical Data
Air 0.35 ± 0.03 17.5 Free from oil, moisture and dust
WARNING
• Do NOT use oxygen gas.
Otherwise, fire or malfunction could result.
CAUTION
• Take care about fluctuations in gas pressure during analysis operations.
If the gas supply pressure changes during the analysis, resultant changes in flame combustion will
adversely affect measurement reproducibility. The supply pressure shown in Table 10.3 must be
maintained during flame combustion.
WARNING
• Place the cylinders outdoors.
Otherwise, fire or accidents could result.
a. Not exposed to heat sources such as direct sunlight, furnaces, and heaters: Always keep the cylinders
at a temperature below 40 °C
b. Away from spark sources such as switchboards, ground wires, and high voltage power sources
c. Away from flammable materials such as oil, gasoline, and organic solvents
d. Sufficiently ventilated
e. If outdoors, not exposed to wind and rain
(3) Gas piping
If the cylinders are placed outdoors, piping must be performed separately within 5 m of the instrument.
In this case, be sure follow the precautionary measures listed below.
a. Use stainless steel pipes for the piping. Do not use of pipes that contain over 62% copper for
acetylene piping.
b. Ensure that the pipe diameters are not too small to supply gas at the pressures indicated in Table
10.3. A pipe diameter of at least 7 mm will be sufficient.
10-22 AA-7000
10.6 Equipment Requirements
c. Place a mist separator in the air piping system at the location indicated in Fig. 10.2. If a sufficiently dry
air supply source is used, a drain separator is unnecessary.
d. Install the stopcock and pressure regulator at a point within 5 meters of the instrument, in the analysis
room.
e. Provide a hose nipple with an outside diameter of 8.4 to 8.9 mm so that the provided gas supply hose
(inside diameter 7.9 mm) can be connected to the end of the gas piping.
Argon gas
AA-7000 10-23
Chapter 10 Technical Data
CAUTION
(1) Install the gas cylinders in the airy outdoors where they are not exposed to direct sunlight.
(2) Take care that gas cylinders become no hotter than 40 °C, and do NOT allow any flame within 2 meters
of the gas cylinders.
(3) When using high pressure gas, make sure that there is sufficient ventilation. At the start of work
inspection, check for gas leakage with soapy water or by other means. With regard to the use of
flammable gases (e.g. acetylene) and gases that increase the susceptibility of substances to burn (e.g.
nitrous oxide) in particular, smoking and the use of fire is prohibited within 5 meters of the equipment
that is using these gases. Install a fire extinguisher to be prepared in the event of an accident.
(4) Secure gas cylinders in a vertical position so that they cannot drop or fall over. Always keep liquefied
gas cylinders (acetylene, nitrous oxide, etc.) in a vertical position and do NOT allow them to fall to a
horizontal position.
(5) Be sure to use oil-free pressure reducing valves. Also use ones that have no oil adhering to the inside of
the pipes, etc., where high-pressure gas comes into contact.
(6) Use approved pressure regulators and connectors. For details, contact your Shimadzu representative.
(7) When installing the pressure regulator on a cylinder, be sure to wipe the dust off the outlet of the
cylinder. Dust at the outlet of the cylinder could cause gas leakage.
10-24 AA-7000
10.6 Equipment Requirements
WARNING
Be sure to provide a duct made of metal for the expulsion of combustible gas above the atomic absorption
spectrophotometer.
If you use a duct made of plastic it will burn due to the heat of the flame.
A ventilator with an airflow rate of 600 to 1200 m3/h is appropriate for flame analysis, while one with an airflow
rate of 10 to 180 m3/h is appropriate for furnace analysis. Too much suction force will affect measurement.
Placement of a damper in the duct system is ideal for setting the optimum airflow.
φ150 to φ200
Fan
Damper
φ150 to φ200
Damper
About 500 × About 500
415 415
1100 to 1200
900 to 1000
AA-7000
714
GFA-7000
ASC-7000
390
340
700
960 960
(Unit: mm)
AA-7000 10-25
Chapter 10 Technical Data
10-26 AA-7000
Index
Symbols B
%R ..................................................................... 3-92 Bandwidth ......................................................... 10-2
%RSD ................................................................ 3-92 Baseline drift ....................................................... 7-4
%TV ..................................................................... 6-6 Beam balance ................................3-23, 3-50, 3-73
.aa ....................................................................... 4-7 BG ..................................................................... 3-91
.taa .................................................................... 3-77 BGC-D2 ............................................................ 10-2
.vld ..................................................................... 7-23 BGC-D2 mode .................................................. 1-16
^ ......................................................................... 3-86 BGC-D2 noise level ............................................ 7-4
BGC-SR ............................................................ 10-2
Numerics BGC-SR mode .................................................. 1-16
BLANK .............................................................. 3-88
21 CFR P11 ....................................................... 5-13 Blank Preparation Parameters .......3-10, 3-36, 3-63
21 CFR Part 11 ................................................... 5-2 BLK ................................................................... 3-93
Burner head ............................... 1-8, 1-9, 8-6, 10-4
A Burner head angle adjustment lever ................... 1-8
Burner position adjustment
Abs .................................................................... 3-86
(When equipped with AAC-7000) ..................... 8-16
Abs. ................................................................... 3-91
Burner positioning adjustment .......................... 8-16
Absorbance and repeatability
Burner Select Sensor Check ............................. 2-17
(In the case of flame analysis) ............................. 7-5
Absorbance and repeatability BURNER SELECT switch ................1-6, 3-17, 3-44
(In the case of furnace analysis) ......................... 7-6 Burner socket ...............................................1-9, 8-6
Absorbance digital display ................................. 3-80 BUSY ................................................................ 3-89
Acceptance Criteria ............................................. 6-5
Acrobat Distiller ................................................. 5-32 C
Actual Conc. ...................................................... 3-92
C# ..................................................................... 3-93
Actual Conc. Unit ............................................... 3-92
C2H2 .........................................................4-11, 4-13
Adjusting position of deuterium lamp ................ 8-27
CAL-CHK .......................................................... 3-94
Admin .................................................................. 5-4
Calibration curve display ................................... 3-85
Administrator ............................................. 5-4, 5-19
Calibration Curve Setup ...................3-9, 3-34, 3-61
Adobe PDFWrite ............................................... 5-32
Capillary .............................................................. 8-9
Air ...................................................................... 4-11
CCB ...........................................................6-8, 6-16
Air-C2H2 ............................................................ 4-11
CCV ...........................................................6-8, 6-16
ANALOG OUT ..................................................... 1-6
CF ..................................................................... 3-92
Analog output .......................................... 1-17, 10-3
Chamber ........................ 1-9, 8-6, 8-11, 8-32, 10-4
ASC connector .................................................... 1-6
Change Database ............................................. 5-34
ASC DF ............................................................. 3-92
Change Graphite Tube ..................................... 3-76
Atomizer position indicator scale ......................... 1-7
Check result ...................................................... 7-17
Atomizer/Gas Flow Rate Setup ............... 3-24, 3-51
Chemicals that can be used .............................. 10-5
Audit Trail .......................................................... 5-14
Chimney .....................................................1-8, 2-11
Audit trail ................................................... 5-3, 5-26
Circuit protector ................................................... 2-3
AUTO ZERO ..................................................... 3-88
CLASS-Agent ...................................................... 5-3
Auto Zero ........................................................... 3-76
CLEANING ........................................................ 3-94
Automatic inspection points ........... 3-15, 3-42, 3-70
Cleaning ............................................................ 3-75
AUTOZERO ...................................................... 3-94
Coating .............................................................. 3-62
AA-7000 IX-1
Coating/Boost Cycle ..........................................3-75 Event log ........................................................... 5-21
COMMAND ........................................................3-94 EXTINGUISH button ........................................... 1-6
Conc. ....................................................... 3-86, 3-91
Conc. Unit ........................................ 3-9, 3-34, 3-61 F
Continuing Calibration Blank ...............................6-8
Continuing Calibration Verification ......................6-8 Fan Stop Sensor ............................................... 2-17
Cooling water supply requirement ...................10-21 Fan stop sensor ................................................ 1-19
Copy ................................................................3-100 FDA 21 CFR Part 11 ..........................5-2, 5-3, 5-23
CORR ..................................................................6-6 File Management .............................................. 5-15
CRA ........................................................... 6-9, 6-16 FILEEXPORT .................................................... 3-94
CRDL ......................................................... 6-4, 6-16 FILESAVE ......................................................... 3-94
Cross Hair ...................................... 3-82, 3-84, 3-87 Flame emission analysis ................................... 4-24
Current user display ..........................................5-24 Flame monitor ........................................... 1-8, 1-19
Flame shield (chimney door) ............................... 1-8
Flashback Monitor ............................................. 2-17
D
Flashback monitor device ................................. 1-19
D .............................................................. 6-15, 6-16 Forward/backward adjusting knob ...................... 1-7
Data administration ............................................5-32 Front panel .................................................. 1-7, 2-8
Data Processing Range (sec) ............................3-92 Fuel gas .................................................. 4-11, 4-13
Database Maintenance Fuel gas pressure monitor ................................ 1-19
Change Database .......................................5-34 Fuel Gas Pressure Monitor Check .................... 2-17
Network .......................................................5-34
Fuel Gas Pressure Monitor Level ...................... 2-16
Repair Database .........................................5-34
Delete Log .........................................................5-21 Function buttons ................................................ 3-88
Designing a system administration policy ............5-9 Furnace position adjustment ............................. 8-18
Furnace position adjustment
Detection limit (In the case of flame analysis) .....7-5
(When equipped with AAC-7000) ...................... 8-18
Detection limit (In the case of furnace analysis) ..7-6
Furnace program ............................................... 3-74
Deuterium lamp ....................................... 1-12, 1-14
Furnace program graph .................................... 3-81
DF ......................................................................3-92
Diffraction grating ..............................................1-14
Diluent ...............................................................3-92
G
Disperser ................................................... 8-8, 8-11 Gas Controller Status .............................. 2-16, 9-10
Drain ..................................................................8-32 Gas Leak Check ................................................ 2-16
Drain Level ........................................................2-16 Gas leaks .......................................................... 8-20
Drain level sensor ..............................................1-19 Gas piping ....................................................... 10-22
Drain Level Sensor Check .................................2-17 Gas requirements ............................................ 10-22
Drain sensor ......................................................8-13 GFA connector .................................................... 1-6
Drain tank ................................................ 2-18, 8-13 GLP/GMP ............................................................ 5-3
Draw BG Line ....................................................3-83 Good Laboratory Practice ................................... 5-2
DUP ...................................................................6-15 Good Manufacturing Practice .............................. 5-2
Duplicate sample analysis .................................6-15 Graph ................................................................ 3-91
GxP support functions ................................. 5-2, 5-3
E
E ........................................................................3-86
H
e .........................................................................3-86 Hardware Validation ............................................ 7-8
Element Selection ............................ 3-4, 3-29, 3-56 Hardware validation ............................................ 7-2
EMISSION .........................................................10-2 Help ................................................................... 2-13
EMISSION mode ...............................................1-15 High temperature burner head .......................... 4-10
EPA ........................................................... 6-2, 6-17 History of system changes ................................ 5-27
IX-2 AA-7000
Hollow cathode lamp ................................. 1-14, 2-6 Mixer ..................................................1-9, 8-6, 8-32
Hollow cathode lamps ............... 1-10, 10-14, 10-16 Mixing ON/OFF ........................................3-36, 3-63
Monochrometer ........................................1-14, 10-2
I Monthly inspection .............................................. 8-3
Mounting the chimney ....................................... 2-11
ICB ............................................................ 6-7, 6-16 Mounting the front panel ..................................... 2-9
ICV ............................................................ 6-7, 6-16 MRT .................................................................. 3-90
ICVS .................................................................. 6-17 MRT work sheet .......................................3-87, 3-90
IDL ..................................................................... 6-16 MSA .........................................................3-94, 4-22
IGNITE button ............................................. 1-6, 1-8 MSA-RES .................................................3-94, 4-22
Igniting and extinguishing the flame .................. 4-10
Initial Calibration Blank ........................................ 6-7
N
Initial Calibration Verification ............................... 6-7
Initializing the instrument ............... 3-15, 3-42, 3-70 N2O ................................................................... 4-13
Instrument Check List for Flame Analysis N2O-C2H2 ......................................................... 4-13
.................................................................. 3-21, 3-48 Nebulizer .......................... 1-9, 8-6, 8-7, 8-32, 10-4
Instrument Detection Limit Determination ......... 6-16 Network ............................................................. 5-34
Instrument information ................... 3-15, 3-42, 3-70 Noise level .......................................................... 7-4
NON-BGC ......................................................... 10-2
L NON-BGC mode ............................................... 1-15
NON-BGC noise level ......................................... 7-4
Laboratory Control Samples .............................. 6-12
Lamp Pos. Setup ............................. 3-7, 3-32, 3-59
O
Lamp Turret ....................................................... 1-10
LCS ............................................... 3-94, 6-12, 6-16 Optical system .................................................. 1-14
Level .................................................................. 5-13 Optics Parameters .........................3-22, 3-49, 3-72
21 CFR P11 ................................................ 5-13 Order ................................................3-9, 3-34, 3-61
Level 1 ........................................................ 5-13
Organic solvent samples ................................... 4-16
Level 2 ........................................................ 5-13
Level 3 ........................................................ 5-13 O-ring SET ........................................................ 8-32
Line search .................................... 3-23, 3-50, 3-73 Out of Control Action ........................................... 6-5
Log Browser ...................................................... 5-11
Logging in WizAArd ......................... 3-2, 3-27, 3-54 P
Login authentication .......................................... 5-23
Password ....................... 3-3, 3-28, 3-55, 5-7, 5-23
Login ID ..................................3-3, 3-28, 3-55, 5-23
Change ....................................................... 5-21
Paste ............................................................... 3-100
M PAUSE .............................................................. 3-94
M ....................................................................... 3-91 PB ............................................................6-10, 6-16
Main screen (Hardware validation) .................... 7-25 PC connector ...................................................... 1-6
Main window ...................................................... 3-78 PDF ................................................................... 5-32
Manual inspection points ......................... 3-15, 3-42 PDS ..........................................................6-13, 6-17
Maximum Password Age ................................... 5-13 Peak profile ....................................................... 3-83
Measurement element tool bar .......................... 3-80 Photo multiplier ................................................. 10-2
Measurement Sequence for Calibration Curve Photo multiplier tube ......................................... 1-14
........................................................ 3-10, 3-36, 3-63 Pilot flame ........................................................... 1-8
Menu bar ........................................................... 3-79 Pilot flame unit .................................................. 8-19
Method for replacing the hollow cathode lamp Polyethylene tube ............................................... 8-9
............................................................................ 8-28 Portable Document Format ............................... 5-32
Minimum Password Length ............................... 5-13 Power requirements ........................................ 10-21
POWER switch ................................................... 1-6
AA-7000 IX-3
Preparation Blank ..............................................6-10 Routine inspections ............................................. 8-2
Pressure regulators ...........................................8-21 RPD ................................................................... 6-17
Print Data/Parameters .........................................4-9
Print Measured Data ..........................................7-26 S
Print Setup .........................................................7-26
Print Table Data ...................................................4-9 S .............................................................. 6-13, 6-17
Printing the data ..................................................4-8 Sample beam .................................................... 1-14
Purge Air .................................................. 3-16, 3-43 Sample Group Setup ......................3-11, 3-38, 3-66
PURGE button ............................................. 1-6, 1-8 Sample ID ......................................................... 3-90
Purge C2H2 .............................................. 3-16, 3-43 Sample ID Collective Setup ...........3-13, 3-40, 3-68
Save calibration curve setup information
Purge N2O ............................................... 3-16, 3-43
................................................................. 3-37, 3-65
Saving the data ................................................... 4-7
Q
SD ..................................................................... 3-92
Q ........................................................................3-91 Security support functions ................................. 5-23
QA/QC ............................................. 6-2, 6-17, 10-3 Current user display ................................... 5-24
Login authentication ................................... 5-23
QC Blank/QC Standard Setup .............................6-4
Restricting the operations
according to user rights .............................. 5-24
R Self-determined true value .................................. 6-4
Setting the optimum condition of burner height
r ............................................................... 3-86, 6-17 ........................................................................... 4-31
Radar ............................................. 3-82, 3-84, 3-87 Setting the optimum condition of fuel gas flow rate
READY ..............................................................3-89 ........................................................................... 4-32
Reagent ................................................... 3-35, 3-62 SG# ................................................................... 3-93
Reagent 1 ..........................................................3-92 Simple standard addition method ...................... 4-17
Reagent 2 ..........................................................3-92 SMSA ...................................................... 3-94, 4-22
Reagent 3 ..........................................................3-92 Software validation ............................................ 5-29
Real time graph .................................................3-81 Spike ................................................................. 6-13
Red feather ........................................................4-15 Spike test .......................................................... 6-13
Reference beam ................................................1-14 SPK ................................................3-94, 6-13, 6-16
Registration Spray unit .................................................. 8-8, 8-10
Rights group ...............................................5-15
Stability (In the case of flame analysis) ............... 7-5
User ............................................................5-18
Standard addition method ................................. 4-17
Removing the chimney ......................................2-11
Standard tool bar ............................................... 3-79
Removing the front panel ....................................2-8
START .............................................................. 3-88
Repair Database ................................................5-34
Start Leak Check ..................................... 3-15, 3-42
Repeat Conditions ......................... 3-10, 3-35, 3-62
Status bar .......................................................... 3-89
Replacing deuterium lamp .................................8-25
STD ................................................................... 3-94
Replacing O-rings ..............................................8-12
Support gas ............................................. 4-11, 4-13
Replacing the drain tube ....................................8-23
Support gas flow meter ..................................... 1-13
RESLOPE ..........................................................3-94
Support gas flow rate adjusting knob ................ 1-13
Reslope Preparation Parameters .. 3-10, 3-36, 3-63
Support gas pressure monitor ........................... 1-19
Restricting the operations according to user rights
............................................................................5-24 Support Gas Pressure Monitor Check (Air) ....... 2-17
Retry ....................................................................6-5 Support Gas Pressure Monitor Check (N2O) .... 2-17
Rights ..................................................................5-5 Support Gas Pressure Monitor Level ................ 2-16
Rights (Group) .....................................................5-5 System administration ................................. 5-3, 5-4
Rights group System Policy .................................................... 5-11
Registration .................................................5-15
RINSE ...................................................... 3-88, 3-94
IX-4 AA-7000
T
Temp. Search .................................................... 3-76
Template ........................................................... 3-77
TEST MEAS. ..................................................... 3-88
Test Meas. ......................................................... 3-75
True Value ......................................................... 3-91
TV .............................................................. 6-4, 6-17
U
U.S. Environmental Protection Agency ............... 6-2
UNK ................................................................... 3-94
Upward/downward adjusting knob ...................... 1-7
USEPA .............................................................. 6-17
User
Registration ................................................ 5-18
User Administration ........................................... 5-11
User ID ...................................................... 5-4, 5-19
User Name ................................................ 5-4, 5-19
U-tube ................................................ 1-9, 8-6, 8-13
V
Validation ............................................................. 5-3
Ventilation system ........................................... 10-25
VF ...................................................................... 3-92
Vibration Sensor ................................................ 2-17
Vibration sensor ................................................ 1-19
W
WAIT ................................................................. 3-94
Wavelength accuracy .......................................... 7-4
Wavelength shift ................................................ 4-30
Weight Correction Factors ............. 3-11, 3-38, 3-66
WF ..................................................................... 3-92
WizAArd launcher .............................................. 1-18
X
X ........................................................................ 3-91
Z
Zero Intercept .................................. 3-9, 3-34, 3-61
AA-7000 IX-5
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IX-6 AA-7000