CN105954262A - {0><}0{>ICP-AES method for measuring sulfur content of lead sulfate in waste storage battery - Google Patents
{0><}0{>ICP-AES method for measuring sulfur content of lead sulfate in waste storage battery Download PDFInfo
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- CN105954262A CN105954262A CN201610545405.2A CN201610545405A CN105954262A CN 105954262 A CN105954262 A CN 105954262A CN 201610545405 A CN201610545405 A CN 201610545405A CN 105954262 A CN105954262 A CN 105954262A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
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Abstract
{0><}0{>The invention discloses an ICP-AES method for measuring sulfur content of lead sulfate in a waste storage battery. The method comprises six steps of sample treatment, preparation of a to-be-tested sample solution and a blank solution, preparation of a standard working solution, drawing of a standard working curve, measurement on sulfur contents of the to-be-tested sample solution and the blank solution and calculation on sulfur content of a sample. <0}{0><}0{>The method disclosed by the invention is simple and rapid, accurate in result, and good in repeatability and reproducibility.
Description
Technical field
The invention belongs to technical field of measurement and test, relate to chemical composition quantitative analysis tech, be specifically related to
ICP-AES method measures sulfur content in scrap battery lead sulfate.
Background technology
Along with constantly riseing of lead metal price, Some Enterprises is had to use scrap battery to reclaim metallic lead at present,
Gained precipitate after the sulfur content that the most typically will measure before processing in scrap battery and process
Middle sulfur content, sinks so as to most lead sulfate the most having become ceruse etc. in inspection processing procedure
Shallow lake thing.
In lead sulfate, the mensuration of sulfur content generally uses barium sulfategravimetry and burning-acid base titration neutralisation,
Barium sulfategravimetry whole analysis process formality is loaded down with trivial details, and analysis time is tediously long, and needs high-temperature fusion and high temperature
Calcination and precipitating for a long time, burning-acid base titration neutralisation is relatively inaccessible to the temperature of more than 1250 DEG C sometimes
Degree so that the SO in lead sulfate4 2-It is difficult to be fully converted to SO2Escape and often result in Lower result, and
Analyzing operation the most loaded down with trivial details, analysis time is longer.
Summary of the invention
For above-mentioned, it is an object of the invention to provide a kind of inductively coupled plasma atomic emission spectrum (letter
Claim ICP-AES) measure the method for sulfur content in scrap battery lead sulfate, sample, after clearing up, uses inductance coupling
Close plasma atomic emission spectrometer and measure the characteristic spectral line intensity of element to be measured in sample solution, by mark
Directrix curve method calculates the content of sulfur in sample.
The concrete technical scheme that the present invention takes is:
The assay method of sulfur content in a kind of scrap battery lead sulfate, its step includes:
(1) sample treatment: weigh sample in high type conical beaker, uses a small amount of water-wet, adds appropriate
Salpeter solution and hydrochloric acid solution A, cap upper surface ware, heating for dissolving on electric hot plate, temperature be 160 DEG C～
180 DEG C, treat that sample steams near dry, take off the coldest, add appropriate hydrochloric acid B solution and move in volumetric flask, use
Water is diluted to scale, shakes up, and stands, clarification, measures, obtain sample to be tested molten after taking supernatant solution or filtering
Liquid, makees blank assay simultaneously；
(2) preparation of standard working solution: weigh 4.4303g and dry to constant weight in 105 DEG C～110 DEG C
Benchmark anhydrous sodium sulfate, is placed in 300mL beaker, after dissolving by suitable quantity of water, moves into 1000mL capacity
In Ping, it is diluted with water to scale, shakes up, obtain sulfur Standard Stock solutions；Pipette sulfur Standard Stock solutions respectively
Each 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL are in 6 50mL
In volumetric flask, each addition 2.5mL hydrochloric acid, it is diluted with water to scale, shakes up, obtain standard working solution；
This series standard solution 1mL sulfur-bearing be respectively 0.00 μ g, 10.0 μ g, 20.0 μ g, 40.0 μ g, 60.0 μ g,
80.0μg；
(3) mensuration of standard working curve: according to the substantially concentration range of element to be measured in test solution, imports
Standard working solution, with the spectral line of inductively coupled plasma atomic emission spectrometer metric works curve
Intensity, with element sulphur concentration as abscissa, the intensity of spectral line is vertical coordinate, draws standard working curve；
(4) blank solution and the mensuration of sample to be tested solution: after standard working curve measures, electricity consumption
Sense coupled plasma-atomic emission spectrometer measures sample blank solution and the intensity of spectral line of sample solution, logical
Cross standard working curve and calculate blank solution and the concentration of element sulphur in sample to be tested solution；
(5) calculating of the content of sulfur in sample:
In formula:
The content of sulfur in X sample, unit is percentage ratio (%)；
The content of sulfur in the sample to be tested solution that c obtains from standard working curve, unit is the every milli of microgram
Rise (μ g/mL)；
c0The content of sulfur in the blank solution obtained from standard working curve, unit is micrograms per millilitre
(μg/mL)；
V sample solution constant volume, unit is milliliter (mL)；
The quality of m sample, unit is gram (g).
In said determination method, sample granularity should≤150 μm.
In said determination method, the mass fraction of sulfur is between 0.50%～8.00%, and weighing sample quality is
0.2g, is accurate to 0.0001g.
In said determination method, high type conical beaker used by step (1) is 125ml, and volumetric flask is 250ml,
Described salpeter solution volume is 9ml, and density is 1.42g/mL；The volume of hydrochloric acid solution A is 3ml,
Density is 1.19g/mL；Hydrochloric acid B solution volume is 12.5ml, and density is 1.19g/mL.
In said determination method, detection is limited to 0.002g/100g.
In said determination method, the analysis spectral line of described element sulphur is: 180.7nm or 182.0nm.
The invention has the beneficial effects as follows: the inventive method simple and fast, result is accurate, Repeatability and Reproducibility
Good.
Detailed description of the invention
Below embodiments of the invention are described in detail, so that advantages and features of the invention can be easier to
It is readily appreciated by one skilled in the art, thus protection scope of the present invention is made apparent clear and definite defining.
Instrument and equipment:
Electronic balance: sensibility reciprocal 0.1mg.
Sub-sieve: 150 μm.
Adjustable temperature control electric hot plate.
Inductively coupled plasma atomic emission spectrometer: first start preheating 40min～60 before starting to measure
Min, simultaneously by argon purging light path to drive away the gas molecules such as light room air, to improve ultraviolet signal
Sensitivity and stability.
Experiment material:
Sample granularity should≤150 μm；
Salpeter solution: density is 1.42g/mL；
Hydrochloric acid solution: density is 1.19g/mL；
Anhydrous sodium sulfate (standard reagent).
Embodiment 1
The assay method of sulfur content in a kind of scrap battery lead sulfate, its step includes:
(1) sample treatment: weigh about 0.2g scrap battery sample in 125mL high type conical beaker,
Use a small amount of water-wet, add 9mL nitric acid and 3mL hydrochloric acid, cap upper surface ware, electric hot plate adds thermosol
Solving, temperature is 160 DEG C～180 DEG C, treats that sample steams near dry, takes off the coldest, add 12.5mL hydrochloric acid,
Rinsing surface plate and wall of cup by little water, warm dissolves salt in beaker, moves in 250mL volumetric flask,
It is diluted with water to scale, shakes up, stand, clarification, measure after taking supernatant solution or filtering, make blank simultaneously
Test；
(2) preparation of standard working solution: weigh 4.4303g and dry to constant weight in 105 DEG C～110 DEG C
Benchmark anhydrous sodium sulfate, is placed in 300mL beaker, after dissolving by suitable quantity of water, moves into 1000mL capacity
In Ping, it is diluted with water to scale, shakes up, obtain sulfur Standard Stock solutions；Pipette sulfur Standard Stock solutions respectively
Each 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL are in 6 50mL
In volumetric flask, each addition 2.5mL hydrochloric acid, it is diluted with water to scale, shakes up, obtain standard working solution；
This series standard solution 1mL sulfur-bearing be respectively 0.00 μ g, 10.0 μ g, 20.0 μ g, 40.0 μ g, 60.0 μ g,
80.0μg；
(3) mensuration of standard working curve: according to the substantially concentration range of element to be measured in test solution, imports
Standard working solution, with the spectral line of inductively coupled plasma atomic emission spectrometer metric works curve
Intensity, with element sulphur concentration as abscissa, the intensity of spectral line is vertical coordinate, draws standard working curve；
(4) blank solution and the mensuration of sample to be tested solution: after standard working curve measures, electricity consumption
Sense coupled plasma-atomic emission spectrometer measures sample blank solution and the intensity of spectral line of sample solution, logical
Cross standard working curve and calculate blank solution and the concentration of element sulphur in sample to be tested solution；
(5) calculating of the content of sulfur in sample:
The measured value of the twice independent test result obtained under the conditions of repeatability, in meansigma methods given below
In the range of, the absolute difference of the two test result is less than repeatability limit (r), exceedes repeatability limit (r)
Situation less than 5%, repeatability limit (r) is obtained by table 1 data acquisition linear interpolation:
Table 1 repeatability limit
| wGa/ % | 0.80 | 1.50 | 7.00 |
| R/% | 0.07 | 0.14 | 0.26 |
The absolute difference of the twice independent test result obtained under the conditions of repeatability is not more than repeatability limit
(R), the situation exceeding repeatability limit (R) is less than 5%, and repeatability limit (R) presses table 2 data acquisition
Try to achieve by linear interpolation.
Table 2 repeatability limits
| wGa/ % | 0.80 | 1.50 | 7.00 |
| R/% | 0.08 | 0.16 | 0.29 |
Inductively coupled plasma atomic emission spectrometer working condition
Claims (6)
1. the assay method of sulfur content in a scrap battery lead sulfate, it is characterised in that its step includes:
(1) sample treatment: weigh sample in high type conical beaker, uses a small amount of water-wet, adds appropriate
Salpeter solution and hydrochloric acid solution A, cap upper surface ware, heating for dissolving on electric hot plate, temperature be 160 DEG C～
180 DEG C, treat that sample steams near dry, take off the coldest, add appropriate hydrochloric acid B solution and move in volumetric flask, use
Water is diluted to scale, shakes up, and stands, clarification, measures, obtain sample to be tested molten after taking supernatant solution or filtering
Liquid, makees blank assay simultaneously；
(2) preparation of standard working solution: weigh 4.4303g and dry to constant weight in 105 DEG C～110 DEG C
Benchmark anhydrous sodium sulfate, is placed in 300mL beaker, after dissolving by suitable quantity of water, moves into 1000mL capacity
In Ping, it is diluted with water to scale, shakes up, obtain sulfur Standard Stock solutions；Pipette sulfur Standard Stock solutions respectively
Each 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL are in 6 50mL
In volumetric flask, each addition 2.5mL hydrochloric acid, it is diluted with water to scale, shakes up, obtain standard working solution；
This series standard solution 1mL sulfur-bearing be respectively 0.00 μ g, 5.0 μ g, 10.0 μ g, 20.0 μ g, 40.0 μ g,
60.0μg、80.0μg；
(3) mensuration of standard working curve: according to the substantially concentration range of element to be measured in test solution, imports
Standard working solution, with the spectral line of inductively coupled plasma atomic emission spectrometer metric works curve
Intensity, with element sulphur concentration as abscissa, the intensity of spectral line is vertical coordinate, draws standard working curve；
(4) blank solution and the mensuration of sample to be tested solution: after standard working curve measures, electricity consumption
Sense coupled plasma-atomic emission spectrometer measures sample blank solution and the intensity of spectral line of sample solution, logical
Cross standard working curve and calculate blank solution and the concentration of element sulphur in sample to be tested solution；
(5) calculating of the content of sulfur in sample:
In formula:
The content of sulfur in X sample, unit is %；
The content of sulfur in the sample to be tested solution that c obtains from standard working curve, unit is μ g/mL；
c0The content of sulfur in the blank solution obtained from standard working curve, unit is μ g/mL；
V sample solution constant volume, unit is mL；
The quality of m sample, unit is g.
In assay method the most according to claim 1, it is characterised in that its sample granularity should≤150 μm.
In assay method the most according to claim 1, it is characterised in that the mass fraction of sulfur exists
Between 0.50%～8.00%, weighing sample quality is 0.2g, is accurate to 0.0001g.
In assay method the most according to claim 1, it is characterised in that high type three used by step (1)
Angle beaker is 125ml, and volumetric flask is 250ml, and described salpeter solution volume is 9ml, and density is 1.42
g/mL；The volume of hydrochloric acid solution A is 3ml, and density is 1.19g/mL；Hydrochloric acid B solution volume is 12.5ml,
Density is 1.19g/mL.
In assay method the most according to claim 1, it is characterised in that the method detection is limited to
0.002g/100g。
In assay method the most according to claim 1, it is characterised in that the analytical spectra of described element sulphur
Line is: 180.7nm or 182.0nm.
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| CN201610545405.2A CN105954262A (en) | 2016-07-12 | 2016-07-12 | {0><}0{>ICP-AES method for measuring sulfur content of lead sulfate in waste storage battery |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106645099A (en) * | 2016-12-10 | 2017-05-10 | 金堆城钼业股份有限公司 | Method for measuring content of sulphur in ammonium molybdate through ICP |
| CN113176252A (en) * | 2021-04-23 | 2021-07-27 | 广东佳纳能源科技有限公司 | Method for measuring sulfur content in ternary precursor |
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2016
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| CN101793830A (en) * | 2010-03-16 | 2010-08-04 | 武汉钢铁(集团)公司 | Method for measuring sulfur content in iron ore |
| CN104007101A (en) * | 2014-05-26 | 2014-08-27 | 中国兵器工业集团第五三研究所 | Method for measuring sulfur content in fuel oil through inductively coupled plasma-atomic emission spectrometry (ICP-AES) method |
| CN105319202A (en) * | 2015-07-10 | 2016-02-10 | 贵州航天精工制造有限公司 | Method for measuring indissolvable nickel-base superalloy multielement content with microwave digestion ICP method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106645099A (en) * | 2016-12-10 | 2017-05-10 | 金堆城钼业股份有限公司 | Method for measuring content of sulphur in ammonium molybdate through ICP |
| CN113176252A (en) * | 2021-04-23 | 2021-07-27 | 广东佳纳能源科技有限公司 | Method for measuring sulfur content in ternary precursor |
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