CN103499536A - Method for measuring indium content in exhaust gas by utilizing flame atomic absorption spectrometry - Google Patents
Method for measuring indium content in exhaust gas by utilizing flame atomic absorption spectrometry Download PDFInfo
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- CN103499536A CN103499536A CN201310443239.1A CN201310443239A CN103499536A CN 103499536 A CN103499536 A CN 103499536A CN 201310443239 A CN201310443239 A CN 201310443239A CN 103499536 A CN103499536 A CN 103499536A
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Abstract
The invention provides a method for measuring the indium content in exhaust gas by utilizing a flame atomic absorption spectrometry. According to the method, a solvent prepared by proportioning high-grade pure nitric acid with deionized water according to a volume ratio of 1:1 is taken as a digestion solvent of a to-be-measured sample, wherein the nitric acid in the proportion is low in boiling point and strong in oxidability and can rapidly digest indium in the to-be-measured sample without easily generating a carbonization phenomenon; as the heating-digestion temperature is controlled at 90-110 DEG C, the digestion speed of the indium is increased, and the time of the whole test is shortened. Meanwhile, the method provided by the invention has the advantages that the detection limit is low, and the test is simple and is easy to operate.
Description
Technical field
The present invention relates to a kind of method that contains the indium amount in the waste gas discharged welding shop of measuring, be specifically related to a kind of method based on the content of indium in Flame Atomic Absorption Spectrometry Determination waste gas.
Background technology
With the indium tin solder, carry out containing the Trace Indium element in the waste gas of workshop electric welding discharge, the atomic number 49 of indium, atomic weight 114.82, flammable, there is pungency, belong to heavy metal, toxic, the Exposed limit value that the U.S. and Britain have announced indium is 0.1mg/m
3, and these two the plumbous standards of country are 0.15mg/m
3, as can be seen here, the toxicity of indium is also larger than plumbous, is not sneezed at, and environment is had to harm, to water body, can pollute.Therefore, the detection that detects indium content in the discharging waste gas of welding shop be environmental monitoring must survey project.
At present, the method that detects indium content is mainly GFAAS (graphite furnace atomic absorption spectrometry), and that GFAAS (graphite furnace atomic absorption spectrometry) has is highly sensitive, the few sample utilization factor of consumption is high, is suitable for the solution that analytical solution concentration is the ppb level, but the composition unevenness of the method is larger, repeatable poor.Be not less than 0.5%mg/L according to the content of indium in indium tin waste gas, meeting under the prerequisite of precision flame atomic absorption spectrometry more accurately and reliably, and convenient fast, favorable repeatability.Need in flame atomic absorption spectrometry to use and clear up solvent element to be measured in testing sample is cleared up, at present, commonly used clear up solvent be according to certain volume match well than sulfuric acid and hydrogen peroxide, there is following drawback in this kind of solvent: 1, hydrogen peroxide is easily blasted in heating process, hazard test personnel's personal safety; 2, the boiling point of sulfuric acid is high, and in the hot digestion process, easily charing, affect testing result.
Summary of the invention
In order to solve the deficiency in background technology, the object of the invention is to overcome the defect of background technology, provide that a kind of test period is shorter, be difficult for the method for indium content in the Flame Atomic Absorption Spectrometry Determination waste gas of charing in handling safety, course of reaction.
For achieving the above object, the technical solution used in the present invention is:
A kind of method of indium content in Flame Atomic Absorption Spectrometry Determination waste gas is characterized in that: comprise the following steps:
A. the collection of sample: gather waste gas with filter cylinder, the described filter cylinder that gathered the waste gas sample is shredded with the stainless steel scissors, obtain the testing sample with described phosphide element, be placed in exsiccator stand-by;
B. Specimen eliminating is processed: accurately take testing sample, be placed in reaction vessel, add quantitative salpeter solution in reaction vessel, being placed on low-temperature heat in electric furnace after reaction vessel is sealed clears up, until test solution is as clear as crystal, and the volume that is evaporated to test solution be salpeter solution add volume 1/4th, filter after test solution is cooled to room temperature and obtain filtrate and be placed in volumetric flask stand-by;
C. sample solution preparation: add deionized water to be settled to scale in volumetric flask, be mixed with testing sample solution;
D. reagent blank liquid preparation: will be diluted to the volume identical with testing sample solution with deionized water with the salpeter solution of step b moderate, and then do dilution for the second time and obtain blank reagent solution, stand-by, the multiple of dilution is 10 times for the second time;
E. standard solution preparation: take deionized water as thinning agent, the indium titer of 100mg/L is mixed with to the standard solution of variable concentrations;
F. indium content in Instrument measuring waste gas, described instrument comprises: flame atomic absorption spectrophotometer, phosphide atom spectrum lamp, design parameter arranges as follows:
Lamp current: 6.0mA
Spectral band-width: 0.5nm
Combustion gas height: 7mm
Air mass flow 8.0mL/min
Acetylene gas flow 2.0L/min
G. with reagent blank liquid calibration flame atomic absorption spectrophotometer zero point, the absorbance of bioassay standard solution and sample solution, the drawing standard curve, measure the content of indium.
In a preferred embodiment of the present invention, further comprise that reaction vessel in described step b is placed on heating and decompose in electric furnace temperature after sealing is 90 ~ 110 ℃.
In a preferred embodiment of the present invention, further comprise that the constituent of described salpeter solution and volume ratio thereof are: the pure nitric acid 1 of top grade, described deionized water 1, described deionized water is 18M Ω cm deionized water.
In a preferred embodiment of the present invention, further comprise that described reaction vessel is the high type glass beaker with scale.
In a preferred embodiment of the present invention, further comprise that in step b, testing sample is 1:13.5 with the volume mass of salpeter solution than g/mL.
In a preferred embodiment of the present invention, further comprise that the measurement of concetration scope of described indium is: 0 ~ 5mg/L.
Usefulness of the present invention is: adopting the pure nitric acid of top grade and deionized water is solvent after the 1:1 proportioning solvent of clearing up as testing sample according to volume ratio, nitric acid boiling point under this kind of proportioning is low, oxidisability is strong, can make the indium in testing sample be difficult for producing the charing phenomenon in rapid-digestion; The temperature of heating and decompose is controlled at 90 ~ 110 ℃, accelerates the oxidation rate of indium, shortens the time of whole test; Method of the present invention also has advantages of that detection limit is low, it is simple to operation to test simultaneously.
Embodiment
In order to make those skilled in the art person understand better the present invention program, and above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with embodiment, the present invention is further detailed explanation.
A kind of method of indium content in Flame Atomic Absorption Spectrometry Determination waste gas is characterized in that: comprise the following steps:
A. the collection of sample: gather waste gas with filter cylinder, the described filter cylinder that gathered the waste gas sample is shredded with the stainless steel scissors, obtain the testing sample with described phosphide element, be placed in exsiccator stand-by;
B. Specimen eliminating is processed: accurately take testing sample, be placed in reaction vessel, add quantitative salpeter solution in reaction vessel, being placed on low-temperature heat in electric furnace after reaction vessel is sealed clears up, until test solution is as clear as crystal, and the volume that is evaporated to test solution be salpeter solution add volume 1/4th, filter after test solution is cooled to room temperature and obtain filtrate and be placed in volumetric flask stand-by;
C. sample solution preparation: add deionized water to be settled to scale in volumetric flask, be mixed with testing sample solution;
D. reagent blank liquid preparation: will be diluted to the volume identical with testing sample solution with deionized water with the salpeter solution of step b moderate, and then do dilution for the second time and obtain blank reagent solution, stand-by, the multiple of dilution is 10 times for the second time;
E. standard solution preparation: take deionized water as thinning agent, the indium titer of 100mg/L is mixed with to the standard solution of variable concentrations;
F. indium content in Instrument measuring waste gas, described instrument comprises: flame atomic absorption spectrophotometer, phosphide atom spectrum lamp, design parameter arranges as follows:
Lamp current: 6.0mA
Spectral band-width: 0.5nm
Combustion gas height: 7mm
Air mass flow 8.0mL/min
Acetylene gas flow 2.0L/min
G. with reagent blank liquid calibration flame atomic absorption spectrophotometer zero point, the absorbance of bioassay standard solution and sample solution, the drawing standard curve, measure the content of indium.
Preferably, the temperature that in step b, reaction vessel is placed on heating and decompose in electric furnace after sealing is 90 ~ 110 ℃.
Preferably, the constituent of salpeter solution and volume ratio thereof are: the pure nitric acid 1 of top grade, described deionized water 1, described deionized water is 18M Ω cm deionized water.
Preferably, reaction vessel is the high type glass beaker with scale.
Preferably, in step b, testing sample is 1:13.5 with the volume mass of salpeter solution than g/mL.
Preferably, the measurement of concetration scope of indium is: 0 ~ 5mg/L.
Embodiment 1:
Gather the waste gas of 400L with the Mount Taishan glue-free filter cylinder of 3 flint glass F fiber, the filter cylinder that gathered the waste gas sample is shredded with the stainless steel scissors, obtain the testing sample with indium, take the high type glass beaker that the 1.481g testing sample is placed in 50mL, adding salpeter solution 20mL(is that 1:13.5 get with the volume mass of salpeter solution than g/mL according to testing sample again), wherein the constituent of salpeter solution and volume ratio thereof are: the pure nitric acid 1 of top grade, the deionized water 1 of 18M Ω cm, the nitric acid of sufficient and specific proportioning is the indium in dissolution sample fast, be difficult for producing the charing phenomenon simultaneously, the surface plate sealing that adds beaker on the salpeter solution bonnet, after adding a cover the surface plate sealing, steam forms backflow, be unfavorable for producing the talk phenomenon, be placed in electric furnace with 100 ℃ of heating and decomposes, until test solution is as clear as crystal, digestion time is 318s, and to be evaporated to test solution be 5mL, take out to filter after test solution is cooled to room temperature and obtain in volumetric flask that filtrate is placed in 50mL, in the 50mL volumetric flask, add deionized water to be settled to scale again, be mixed with testing sample solution.
The preparation of reagent blank liquid, by the 20mL salpeter solution, (volume ratio nitric acid: deionized water=1:1) with deionized water, dilute, be settled to 50mL, do dilution for the second time after shaking up and obtain reagent blank liquid, stand-by, the multiple of dilution is 10 times for the second time.
Preparing standard solution is also drawn the mark working curve: take deionized water as thinning agent, the indium titer (being provided by State center for standard matter) of 100mg/L is mixed with respectively to concentration A is 0,1.0,2.0,3.0,4.0, the series standard solution of 5.0mg/L.
The mentioned reagent blank solution is measured according to above-mentioned set parameter with Japanese Shimadzu 6800 type flame atomic absorption spectrophotometers (attached computing machine and printer), proofread and correct spectrometer zero point, sequentially determining series standard solution again, the instrument automatic data processing, and the display standard curve, the absorbance result recorded is as follows: C=0.0063,23.26,46.52,69.79,93.06,116.33.
According to the corresponding relation of A and C, obtain an equation of linear regression by Mathematical Fitting, as follows:
A=0.04298C+0.00027, related coefficient is r=0.9999, so the concentration of indium is linear in 0 ~ 5mg/L scope.
Under arranging, above-mentioned same parameters carries out the mensuration of testing sample solution, parallel METHOD FOR CONTINUOUS DETERMINATION six times, show that according to working curve measurement result is: 0.036mg/L, 0.031 mg/L, 0.038 mg/L, 0.042 mg/L, 0.038 mg/L, 0.043 mg/L, calculating mean value is 0.038 mg/L, the content that draws indium in waste gas is 0.038mg/L, is qualified discharge.
Embodiment 2
With the difference of the condition of embodiment 1, be, after the sealing of beaker cover upper surface ware, be placed in electric furnace with 90 ℃ of heating and decomposes, until test solution is as clear as crystal, digestion time is 352s;
Other test condition is consistent with embodiment 1, testing sample solution is done to parallel METHOD FOR CONTINUOUS DETERMINATION six times, show that according to working curve measurement result is: 0.028 mg/L, 0.023 mg/L, 0.024 mg/L, 0.020 mg/L, 0.029 mg/L, 0.020 mg/L, calculating mean value is 0.024 mg/L, with embodiment 1, compare, the content of indium is lower, after analysis-by-synthesis, draws: when digestion condition is 90 ℃, indium is not cleared up fully.
Embodiment 3
With the difference of the condition of embodiment 1, be, after the sealing of beaker cover upper surface ware, be placed in electric furnace with 110 ℃ of heating and decomposes, until test solution is as clear as crystal, digestion time is 315s;
Other test condition is consistent with embodiment 1, testing sample solution is done to parallel METHOD FOR CONTINUOUS DETERMINATION six times, show that according to working curve measurement result is: 0.030 mg/L, 0.031 mg/L, 0.034 mg/L, 0.028 mg/L, 0.028 mg/L, 0.035 mg/L, calculating mean value is 0.031 mg/L, with embodiment 1, compare, the content of indium is lower, after analysis-by-synthesis, draws: when digestion condition is 110 ℃, indium runs off with the boiling of nitric acid.
Embodiment 4
With unique difference of embodiment 1, be, the solvent of clearing up of embodiment 1 is salpeter solution, the solvent of clearing up of embodiment 4 is to be the sulfuric acid of 1:3 and hydrogen peroxide by volume, testing sample solution is done to parallel METHOD FOR CONTINUOUS DETERMINATION six times, show that measurement result is: 0.052 mg/L, 0.045 mg/L, 0.047 mg/L, 0.045 mg/L, 0.047 mg/L, 0.046 mg/L, calculating mean value is 0.047 mg/L, with embodiment 1, compare, the content of indium is higher, sulfuric acid produces the charing phenomenon in heating process, affect measurement result, after analysis-by-synthesis, draw: with salpeter solution in specific proportions of the present invention as clearing up solvent, measure not only accurately and reliably, and convenient quick.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not limited by the examples; other any do not deviate from change, the modification done under Spirit Essence of the present invention and principle, substitutes, combination, simplify and all should be equivalent substitute mode, within being included in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain that claim was defined.
Claims (6)
1. the method for indium content in a Flame Atomic Absorption Spectrometry Determination waste gas is characterized in that: comprise the following steps:
A. the collection of sample: gather waste gas with filter cylinder, the described filter cylinder that gathered the waste gas sample is shredded with the stainless steel scissors, obtain the testing sample with described phosphide element, be placed in exsiccator stand-by;
B. Specimen eliminating is processed: accurately take testing sample, be placed in reaction vessel, add quantitative salpeter solution in reaction vessel, being placed on low-temperature heat in electric furnace after reaction vessel is sealed clears up, until test solution is as clear as crystal, and the volume that is evaporated to test solution be salpeter solution add volume 1/4th, filter after test solution is cooled to room temperature and obtain filtrate and be placed in volumetric flask stand-by;
C. sample solution preparation: add deionized water to be settled to scale in volumetric flask, be mixed with testing sample solution;
D. reagent blank liquid preparation: will be diluted to the volume identical with testing sample solution with deionized water with the salpeter solution of step b moderate, and then do dilution for the second time and obtain blank reagent solution, stand-by, the multiple of dilution is 10 times for the second time;
E. standard solution preparation: take deionized water as thinning agent, the indium titer of 100mg/L is mixed with to the standard solution of variable concentrations;
F. indium content in Instrument measuring waste gas, described instrument comprises: flame atomic absorption spectrophotometer, phosphide atom spectrum lamp, design parameter arranges as follows:
Lamp current: 6.0mA
Spectral band-width: 0.5nm
Combustion gas height: 7mm
Air mass flow 8.0mL/min
Acetylene gas flow 2.0L/min
G. with reagent blank liquid calibration flame atomic absorption spectrophotometer zero point, the absorbance of bioassay standard solution and sample solution, the drawing standard curve, measure the content of indium.
2. the method for indium content in Flame Atomic Absorption Spectrometry Determination waste gas according to claim 1 is characterized in that: in described step b, to be placed on the temperature of heating and decompose in electric furnace after sealing be 90 ~ 110 ℃ to reaction vessel.
3. the method for indium content in Flame Atomic Absorption Spectrometry Determination waste gas according to claim 1 and 2, it is characterized in that: the constituent of described salpeter solution and volume ratio thereof are: the pure nitric acid 1 of top grade, described deionized water 1, described deionized water is 18M Ω cm deionized water.
4. the method for indium content in Flame Atomic Absorption Spectrometry Determination waste gas according to claim 2, it is characterized in that: described reaction vessel is the high type glass beaker with scale.
5. the method for indium content in Flame Atomic Absorption Spectrometry Determination waste gas according to claim 1, it is characterized in that: in step b, testing sample is 1:13.5 with the volume mass of salpeter solution than g/mL.
6. the method for indium content in Flame Atomic Absorption Spectrometry Determination waste gas according to claim 1, it is characterized in that: the measurement of concetration scope of described indium is: 0 ~ 5mg/L.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107677616A (en) * | 2017-08-14 | 2018-02-09 | 广西德邦科技有限公司 | The method of cobalt content in Flame Atomic Absorption Spectrometry Determination product indium |
| CN107677617A (en) * | 2017-08-14 | 2018-02-09 | 广西德邦科技有限公司 | The method of silver content in Flame Atomic Absorption Spectrometry Determination product indium |
| CN107703119A (en) * | 2017-08-14 | 2018-02-16 | 广西德邦科技有限公司 | The method of nickel content in Flame Atomic Absorption Spectrometry Determination product indium |
| CN110426358A (en) * | 2019-08-09 | 2019-11-08 | 南通化学环境监测站有限公司 | The Flame Atomic Absorption Spectrometry in Determining of barium in a kind of water quality |
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2013
- 2013-09-26 CN CN201310443239.1A patent/CN103499536A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107677616A (en) * | 2017-08-14 | 2018-02-09 | 广西德邦科技有限公司 | The method of cobalt content in Flame Atomic Absorption Spectrometry Determination product indium |
| CN107677617A (en) * | 2017-08-14 | 2018-02-09 | 广西德邦科技有限公司 | The method of silver content in Flame Atomic Absorption Spectrometry Determination product indium |
| CN107703119A (en) * | 2017-08-14 | 2018-02-16 | 广西德邦科技有限公司 | The method of nickel content in Flame Atomic Absorption Spectrometry Determination product indium |
| CN110426358A (en) * | 2019-08-09 | 2019-11-08 | 南通化学环境监测站有限公司 | The Flame Atomic Absorption Spectrometry in Determining of barium in a kind of water quality |
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Application publication date: 20140108 |