CN107843709A - Integrated portable heavy metal quick analytic instrument and its analyzing detecting method - Google Patents
Integrated portable heavy metal quick analytic instrument and its analyzing detecting method Download PDFInfo
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- CN107843709A CN107843709A CN201711376461.9A CN201711376461A CN107843709A CN 107843709 A CN107843709 A CN 107843709A CN 201711376461 A CN201711376461 A CN 201711376461A CN 107843709 A CN107843709 A CN 107843709A
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- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 11
- 239000007789 gas Substances 0.000 claims abstract description 76
- 239000007788 liquid Substances 0.000 claims abstract description 41
- 239000012159 carrier gas Substances 0.000 claims abstract description 24
- 239000012530 fluid Substances 0.000 claims abstract description 24
- 238000012360 testing method Methods 0.000 claims abstract description 24
- 238000000889 atomisation Methods 0.000 claims abstract description 22
- 238000005070 sampling Methods 0.000 claims abstract description 14
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 34
- 229910052697 platinum Inorganic materials 0.000 claims description 17
- 210000002381 plasma Anatomy 0.000 claims description 16
- 239000013307 optical fiber Substances 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 238000004458 analytical method Methods 0.000 claims description 11
- 239000000835 fiber Substances 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 239000010453 quartz Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000001228 spectrum Methods 0.000 claims description 9
- 239000007921 spray Substances 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052737 gold Inorganic materials 0.000 claims description 6
- 239000010931 gold Substances 0.000 claims description 6
- 229910052709 silver Inorganic materials 0.000 claims description 6
- 239000004332 silver Substances 0.000 claims description 6
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 6
- 229910052721 tungsten Inorganic materials 0.000 claims description 6
- 239000010937 tungsten Substances 0.000 claims description 6
- 239000000446 fuel Substances 0.000 claims description 5
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 230000019491 signal transduction Effects 0.000 claims description 4
- 230000003595 spectral effect Effects 0.000 claims description 3
- 210000004209 hair Anatomy 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 14
- 150000002500 ions Chemical class 0.000 abstract description 4
- 238000004445 quantitative analysis Methods 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 238000005507 spraying Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 239000002689 soil Substances 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- -1 are opened Substances 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 240000005373 Panax quinquefolius Species 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000003891 environmental analysis Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000000918 plasma mass spectrometry Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/20—Metals
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The present invention provides a kind of integrated portable heavy metal quick analytic instrument and its analyzing detecting method, including：Liquid sampling device (1), pneumatic micro- atomization system (2,3,4,5,6,8,9,10), corona discharge systems (7,11,12,13) and spectroscopic system (14,15,16), pneumatic micro- atomization system include：The airborne gas cylinder of sheath (2), auxiliary airborne gas cylinder (3), threeway a (4), threeway b (5), threeway c (6), fluid passage (8), sheath gas passage (9) and auxiliary gas passage (10)；Centronics port of the testing liquid through threeway a (4) in the liquid sampling device (1) enters the fluid passage (8)；Carrier gas is passed into the sheath gas passage (9) by the airborne gas cylinder of sheath (2) through threeway b (5) Centronics ports；Auxiliary gas is passed into the auxiliary gas passage (10) by the auxiliary airborne gas cylinder (3) through threeway c (6) Centronics ports；The fluid passage (8), the sheath gas passage (9) and the auxiliary gas passage (10) are coaxially arranged.The analyzer of the application adds a carrier gas passage, while ensureing that heavy metal sample fast and effeciently carries out quantitative analysis, reduces the loss of sample ions beam, improves the accuracy and precision of instrument detection.
Description
Technical field
The present invention relates to the portable inspection of a kind of corona discharge and content of beary metal in the integrated emission spectrographic analysis liquid of spraying
Survey device, and in particular to a kind of integrated portable heavy metal quick analytic instrument and its analyzing detecting method, belong to environmental analysis
Learn technical field.
Background technology
Heavy metal pollution is one of the problem of contaminated area is most wide, harm is maximum in current environmental pollution.A huge sum of money in environment
Waste gas, waste water and the waste residue of industrial and mining enterprises' discharges such as the source of category pollution is mainly dug up mine, smelting, the fossil fuel such as coal and oil
Burning and agriculture chemical be excessively used, wherein mainly include Hg, Cd, Pb, Cr, Zn, Cu, Ni and metalloid As etc..Extensively
General sources of heavy metal causes big gas and water and Mobility of Heavy Metals In Soil Environment to pollute and increasingly aggravate.Rainfall can be by air, soil
Heavy metal is transferred in water body in earth and road dust；Irrational sewage irrigation etc. can cause Heavy Metals in Waters for a long time
Into soil.After heavy metal is entered in environment, it is difficult to be biodegradable, the transfer of form and phase can only occur.By heavy metal
After the water body and soil of pollution are bioavailable, it can accumulate in vivo, and as food chain is communicated up, to the mankind and Sheng
State system produces immeasurable harm.Therefore, heavy metal present in environment for human survival is carried out close, easily real
When detection be particularly important.
The common detection methods of content of beary metal at present, as Atomic absorption-AAS, inductively coupled plasma-
Atomic emission spectrometry etc., the limitation that detection means is larger, is difficult to movement etc. is suffered from, it is quick to be difficult to realize heavy metal in water
Sensitive monitoring in real time in situ.Therefore, it is very urgent to design, develop sensitive, accurate portable water heavy metal analysis device
Cut.
Non-thermal microplasma (such as dielectric barrier discharge DBD) can be entered by pneumatic mode to heavy metal in solution
Row is directly atomized, and is plasma by the heavy metal ionization of atomization, then received by spectrometer and treat check weighing in a manner of energization
The characteristic spectrum signal of metal simultaneously carries out analysis measure.Instrument build needed for this method is smaller and heavy metal in solution is carried out
Directly it is atomized and excites the sensitivity that can significantly improve this method, it is possible to achieve the portable inspectiont of heavy metal in water.
Present inventor has found that existing portable detector only designs a carrier gas passage and is used for mist under study for action
Change fluid sample, caused spraying is inevitable must to occur loss, so as to cause the dirt of the loss of test substance and lens mirror
Dye so that deviation occurs in testing result；Existing portable detector is using conventional platinum filament coil electrode, platinum filament coil electricity
Pole and testing liquid contact surface are smaller, it is impossible to are effectively ionized, influence the ionizing efficiency of testing sample, reduce device inspection
The accuracy of survey.
The content of the invention
The present invention is the loss realized the in situ detection of heavy metal in fluid sample, reduce atomized sample ion beam, is proposed
A kind of integrated portable heavy metal quick analytic instrument and its analyzing detecting method, the analyzer add a carrier gas passage,
While ensureing that heavy metal sample fast and effeciently carries out quantitative analysis, the loss of sample ions beam is reduced, is substantially increased
The accuracy and precision of instrument detection.
On the one hand, a kind of integrated portable heavy metal quick analytic instrument of the invention, including：
Liquid sampling device, pneumatic micro- atomization system, corona discharge systems and spectroscopic system,
Pneumatic micro- atomization system includes：The airborne gas cylinder of sheath, auxiliary airborne gas cylinder, threeway a, threeway b, threeway c, liquid lead to
Road, sheath gas passage and auxiliary gas passage；Centronics port of the testing liquid through threeway a in the liquid sampling device enters described
Fluid passage；Carrier gas is passed into the sheath gas passage by the airborne gas cylinder of sheath through threeway b Centronics ports；The auxiliary airborne gas cylinder
Auxiliary gas is passed into the auxiliary gas passage through threeway c Centronics ports；
The fluid passage, the sheath gas passage and the auxiliary gas passage are coaxially arranged.
Further, the corona discharge systems include：
Electrode a, electrode b and power supply；The both ends of power electrically connects with electrode a and electrode b respectively；The electrode crosses institute
State fluid passage and be coaxially disposed with the fluid passage.
Further, the spectroscopic system includes：
Lens, optical fiber and fiber spectrometer；The lens are connected through the optical fiber with the fiber spectrometer.
Further, the flow rate of liquid of the liquid sampling device is 1-80 μ l/s；Sample frequency is 0-60 times/h.
Further, the fluid passage is made of quartz capillary, 200 μm of internal diameter, 360 μm of external diameter, length 10cm；
The sheath gas passage is made of quartz capillary, 530 μm of internal diameter, 670 μm of external diameter, length 8cm；
The auxiliary gas passage is made of quartz capillary, 750 μm, external diameter 1.59mm, length 6cm of internal diameter.
Further, the sheath gas is argon gas or helium, flow velocity 1-600ml/min；The auxiliary gas is argon gas or helium,
Flow velocity is 1-500ml/min.
Further, the electrode a length is 12-15cm, a diameter of 50-80 μm；The distance of the electrode a and electrode b
For 5-15mm；The conducting metal of the electrode a is platinum, gold, silver or tungsten；The conducting metal of the electrode b is platinum, gold, silver or tungsten；
The electrode b is square, length of side 2-4cm, thickness 0.02-0.6mm.
Further, the voltage of the power supply is 3.5-5.0KV, frequency 40-50KHz.
Further, the lens are arranged in electrode side, distance electrode 10-15cm；The internal diameter of the lens is 600-
1000 μm, length 10-20cm；The core diameter of the optical fiber is 90 μm, length 20cm；
The slit width of the fiber spectrometer is 25 μm, and grating is 1600/mm, spectral resolution 0.2nm.
On the other hand, according to the analyzing detecting method of above-mentioned analyzer, comprise the following steps：
(1) the sheath gas passage and the auxiliary gas passage carrier gas, are opened, carrier gas is gone out by pneumatic micro- atomization system
Mouth is continual and steady to be sprayed, and is opened power supply, is made the sustainable generation DBD plasmas of corona discharge systems；
(2) sample introduction is started after plasma stability generation；Injected a sample into by the liquid sampling device pneumatic micro-
Atomization system, it is liquid little particle to be atomized in atomization system outlet by the airborne gas of sheath, and will be atomized by auxiliary airborne gas
Liquid is grouped as the relatively regular fuel spray of shape, while enters in DBD plasma exciatiaons source and excite plasma, produces special
Levy emission spectrum；
(3) using lens collect test substance characteristic spectrum, by optical fiber by signal transduction into spectrometer, go forward side by side
Row record analysis.
Compared with prior art, integrated portable heavy metal quick analytic instrument of the invention, has：
1st, integrating device build of the present invention it is smaller, can be portable, sample detection frequency is higher, suitable for the original position of actual sample
Detection；
2nd, double carrier gas passages design of integrating device of the present invention can concentrate liquid spray Shu Gengjia, on the one hand improve
The accuracy and precision of testing result, on the other hand reduce spraying loss polluted to caused by device.
3rd, platinum electrode runs through whole fluid passage, increases the contact area with testing liquid, can improve determinand
The ionizing efficiency of matter, so as to improve the accuracy of instrument detection.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are this hairs
Some bright embodiments, for those of ordinary skill in the art, on the premise of not paying creative work, can be with root
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is the schematic diagram of integrated portable heavy metal quick analytic instrument embodiment of the embodiment of the present invention；
Fig. 2 embodiment of the present invention obtains the micro- gram per liter lead solution canonical plottings of 0-20.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention
In accompanying drawing, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is
Part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art
The every other embodiment obtained under the premise of creative work is not made, belongs to the scope of protection of the invention.
As shown in figure 1, integrated portable heavy metal quick analytic instrument of the present invention, including：It is liquid sampling device 1, pneumatic micro-
Atomization system, corona discharge systems and spectroscopic system.Pneumatic micro- atomization system includes carrier gas bottle 2 and carrier gas bottle 3, threeway 4,
Threeway 5 and threeway 6, fluid passage 8, sheath gas passage 9 and auxiliary gas passage 10, and three pipelines are coaxial；Liquid sampling device 1 and threeway
4 Centronics ports are connected, for by testing liquid through being injected into fluid passage 8；Carrier gas bottle 2 is connected with the Centronics port of threeway 5, is used for
Carrier gas is passed through sheath gas passage 9, so as to be atomized testing liquid, carrier gas bottle 3 is connected through the Centronics port of threeway 6, for carrier gas to be led to
Enter auxiliary gas passage 10, so as to concentrate fuel spray, the embodiment of the present invention, can be with by way of increasing a carrier gas passage in outside
Spray shapes are corrected, reduce the loss probability of spraying, so as to improve the accuracy of device detection.The corona discharge systems include
Platinum electrode 7 (or gold, silver or tungsten), AC power 11, platinum plate electrode 12 (also can be gold, silver or tungsten) and wire 13；Platinum
Silk electrode 7 crosses the fluid passage 8, and coaxial in it, and the embodiment of the present invention is to be measured by the way that elongated platinum electrode is crossed
Fluid passage, increase both contacts area, the ionizing efficiency of testing sample can be greatly improved, improve the accurate of device detection
Property.AC power 11 is connected with platinum electrode 7 and platinum plate electrode 12 respectively by wire 13, for by atomized liquid ionization for etc.
Gas ions, and launch the characteristic spectrum of test substance；The spectral collection device includes lens 14, optical fiber 15 and fiber spectrum
Instrument 16；Lens 14 are connected by optical fiber 15 with fiber spectrometer 16, for characteristic spectrum to be collected, and pass through fiber coupling
And conduct and recorded and analyzed into fiber spectrometer.
Fluid passage 8 is made of quartz capillary, 200 μm of internal diameter, 360 μm of external diameter, length 10cm；Sheath gas passage 9 is adopted
It is made of quartz capillary, 530 μm of internal diameter, 670 μm of external diameter, length 8cm；Auxiliary gas passage 10 is made of quartz capillary, interior
750 μm, external diameter 1.59mm, length 6cm of footpath；Sheath gas is argon gas, flow velocity 600ml/min；Auxiliary gas is argon gas, flow velocity 300ml/
min；The length of platinum electrode 7 is 12cm, a diameter of 60 μm；The platinum electrode 7 and distance 5mm of platinum plate electrode 12；The side of platinum plate electrode 12
A length of 2cm, thickness 0.3mm；The voltage of AC power 11 is 3.9KV, frequency 40KHz；Lens 14 are distributed in electrode side,
Distance electrode 10cm；The internal diameter of the lens 14 is 950 μm, length 20cm.
In embodiments of the present invention, Liquid sample introduction system can be FIA lab Instruments Inc.；CCD type number can be
The Tristan-5 of German Mut companies.
The analyzing detecting method of the analyzer of the embodiment of the present invention, comprises the following steps：
(1) the sheath gas passage and the auxiliary gas passage carrier gas, are opened, carrier gas is gone out by pneumatic micro- atomization system
Mouth is continual and steady to be sprayed, and is opened power supply, is made the sustainable generation DBD plasmas of corona discharge systems；
(2) sample introduction is started after plasma stability generation；Injected a sample into by the liquid sampling device pneumatic micro-
Atomization system, it is liquid little particle to be atomized in atomization system outlet by the airborne gas of sheath, and will be atomized by auxiliary airborne gas
Liquid is grouped as the relatively regular fuel spray of shape, while enters in DBD plasma exciatiaons source and excite plasma, produces special
Levy emission spectrum；
(3) using lens collect test substance characteristic spectrum, by optical fiber by signal transduction into spectrometer, go forward side by side
Row record analysis.
Exemplified by determining Pb, the integrated portable heavy metal analysis device measure Pb's of the present invention comprises the following steps that：
(1) two passage carrier gas are opened, sheath gas and auxiliary gas velocity are respectively set to 600 and 300ml/min；Treat carrier gas by mist
After changing the continual and steady ejection of system outlet, power-on, in electrode both ends loading 2.9kV high-frequency ac voltage, put corona
The sustainable generation DBD plasmas of electric system；
(2) sample introduction is started after plasma can be stablized and produce；By Liquid sample introduction system by 50 μ L samples containing Pb2+ with
The 5 μ L/s pneumatic micro- atomization system of flow velocity injection, it is liquid to be atomized in atomization system outlet by inner side carrier gas (sheath gas)
Little particle, and atomized liquid is grouped as by the relatively regular fuel spray of shape by outside carrier gas (auxiliary gas), while enter DBD etc.
Plasma is excited in gas ions excitaton source, produces characteristic emission spectrum；
(3) using lens collect test substance characteristic spectrum, by optical fiber by signal transduction into spectrometer, go forward side by side
Row record analysis；
(4) after the completion of testing, the fluid passage in cleaning liquid sampling system and pneumatic micro- atomization system, for next time
Sample introduction is prepared；
The Pb2+ linear detection ranges of apparatus of the present invention are 10-1000 μ g/L, and canonical plotting is as shown in Figure 2.
Three kinds of representative water body examples (including river, seawater and underground water) of collection are subjected to simple pre- place
(after 0.45 μm of membrane filtration, a certain proportion of hydrochloric acid extraction sample is added after reason extraction experiment), is collected respectively through the present invention
Into portable unit and icp mses (ICP-MS) quantitative analysis, and the testing result of stream oriented device is carried out
Contrast.
Analysis result is as shown in table 1.The result show the present apparatus analyze a variety of environmental water sample results and inductive etc. from
Daughter mass spectrometry results are consistent, it was demonstrated that this method reliable results, accurate.
The inductivity coupled plasma mass spectrometry of table 1 and apparatus of the present invention analysis environments water sample and pedotheque Pb content balances
The sensitivity of lead element is less than 3% up to 20ng/L, precision in the bright device detection water sample of we, and analysis time is not
More than 1min, device gross weight is no more than 10Kg, the metal member in plurality of liquid sample in-site detecting actual environment
Element.When in use, testing liquid is in pneumatically pair through sheath gas and auxiliary gas at micro- atomization system nozzle for the analytical equipment of such scheme
Under recast is used, testing liquid is converted into the spray cone beam for comparing concentration, avoids loss of spraying.The spray cone beam is on the one hand
The loss of test substance is reduced, the accuracy of instrument is improved, on the other hand can reduce dirt of the spraying to lens mirror of loss
Dye.Electrode metal silk runs through whole fluid passage, increases the contact area with testing liquid, can improve the electricity of test substance
From efficiency, so as to improve the accuracy of instrument detection.
Finally it should be noted that：The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
The present invention is described in detail with reference to the foregoing embodiments, it will be understood by those within the art that：It still may be used
To be modified to the technical scheme described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic；
And these modification or replace, do not make appropriate technical solution essence depart from various embodiments of the present invention technical scheme spirit and
Scope.
Claims (10)
- A kind of 1. integrated portable heavy metal quick analytic instrument, it is characterised in that including：Liquid sampling device (1), pneumatic micro- atomization system (2,3,4,5,6,8,9,10), corona discharge systems (7,11,12,13) With spectroscopic system (14,15,16),Pneumatic micro- atomization system includes：The airborne gas cylinder of sheath (2), auxiliary airborne gas cylinder (3), threeway a (4), threeway b (5), threeway C (6), fluid passage (8), sheath gas passage (9) and auxiliary gas passage (10)；Testing liquid warp in the liquid sampling device (1) Threeway a (4) Centronics port enters the fluid passage (8)；The airborne gas cylinder of sheath (2) will through threeway b (5) Centronics port Carrier gas is passed into the sheath gas passage (9)；Auxiliary gas is passed into described by the auxiliary airborne gas cylinder (3) through threeway c (6) Centronics ports Auxiliary gas passage (10)；The fluid passage (8), the sheath gas passage (9) and the auxiliary gas passage (10) are coaxially arranged.
- 2. analyzer according to claim 1, it is characterised in that the corona discharge systems include：Electrode a (7), electrode b (12) and power supply (11)；Power supply (11) both ends are electric with electrode a (7) and electrode b (12) respectively Connection；The electrode (7) is crossed the fluid passage (8) and is coaxially disposed with the fluid passage (8).
- 3. analyzer according to claim 1, it is characterised in that the spectroscopic system includes：Lens (14), optical fiber (15) and fiber spectrometer (16)；The lens (14) are through the optical fiber (15) and the optical fiber light Spectrometer (16) is connected.
- 4. analyzer according to claim 1, it is characterised in that the flow rate of liquid of the liquid sampling device (1) is 1-80 μ l/s；Sample frequency is 0-60 times/h.
- 5. analyzer according to claim 1 or claim 2, it is characterised in that the fluid passage (8) uses quartz capillary system Into, 200 μm of internal diameter, 360 μm of external diameter, length 10cm；The sheath gas passage (9) is made of quartz capillary, 530 μm of internal diameter, 670 μm of external diameter, length 8cm；The auxiliary gas passage (10) is made of quartz capillary, 750 μm, external diameter 1.59mm, length 6cm of internal diameter.
- 6. analyzer according to claim 1 or claim 2, it is characterised in that the sheath gas is argon gas or helium, flow velocity 1- 600ml/min；The auxiliary gas is argon gas or helium, flow velocity 1-500ml/min.
- 7. analyzer according to claim 3, it is characterised in that electrode a (7) length is 12-15cm, a diameter of 50- 80μm；The electrode a (7) and electrode b (12) distance are 5-15mm；The conducting metal of the electrode a (7) be platinum, gold, silver or Tungsten；The conducting metal of the electrode b (12) is platinum, gold, silver or tungsten；The electrode b (12) is square, and length of side 2-4cm is electric Pole thickness is 0.02-0.6mm.
- 8. analyzer according to claim 3, it is characterised in that the voltage of the power supply (11) is 3.5-5.0KV, and frequency is 40-50KHz。
- 9. according to the analyzer of claim 4 or 5, it is characterised in that the lens (14) are arranged in electrode side, distance electrode 10-15cm；The internal diameter of the lens (14) is 600-1000 μm, length 10-20cm；The core diameter of the optical fiber (15) is 90 μm, length 20cm；The slit width of the fiber spectrometer (16) is 25 μm, and grating is 1600/mm, spectral resolution 0.2nm.
- 10. according to the analyzing detecting method of one of the claim 1-9 analyzers, it is characterised in that comprise the following steps：(1) the sheath gas passage (9) and auxiliary gas passage (10) carrier gas, are opened, makes carrier gas by pneumatic micro- atomization system Outlet is continual and steady to be sprayed, and is opened power supply, is made the sustainable generation DBD plasmas of corona discharge systems；(2) sample introduction is started after plasma stability generation；Pneumatic micro- atomization is injected a sample into by the liquid sampling device System, in atomization system outlet, to be atomized by the airborne gas of sheath be liquid little particle, and by auxiliary airborne gas by atomized liquid The relatively regular fuel spray of shape is grouped as, while enters in DBD plasma exciatiaons source and excites plasma, produces feature hair Penetrate spectrum；(3) characteristic spectrum of test substance is collected using lens, by optical fiber by signal transduction into spectrometer, and remembered Record analysis.
Priority Applications (1)
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