CN103592197A - Method for analyzing selenium content in crude selenium - Google Patents
Method for analyzing selenium content in crude selenium Download PDFInfo
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- CN103592197A CN103592197A CN201310545957.XA CN201310545957A CN103592197A CN 103592197 A CN103592197 A CN 103592197A CN 201310545957 A CN201310545957 A CN 201310545957A CN 103592197 A CN103592197 A CN 103592197A
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Abstract
The invention discloses a method for analyzing selenium content in crude selenium. The method comprises the following steps: dissolving sample acid, filtering, separating interference of acid-insoluble elements, reducing by using hydrazine hydrate, filtering, separating partial interference elements, precipitating, further dissolving in acid, testing tellurium by using a spectrograph, eliminating main interference elements, testing the selenium content of the filtrate by using the spectrograph, and modifying the analysis result. According to the method, a classical weight method is adopted for measurement, main interference elements are eliminated, loss of selenium in the filtrate is compensated, the result of the method is accurate and reliable, the analysis range is wide, not only is the crude selenium tested, but also pure selenium with the selenium content less than 99.9% can be tested, and great popularization values are achieved.
Description
Technical field
The present invention relates to a kind of method of analyzing Se content in thick selenium.
Background technology
Selenium is a kind of important raw material of industry, is also one of necessary trace element of animal and human's body.Selenium is rare at occurring in nature, dispersion, seldom has concentrated mineral deposit, and the content in the earth's crust is 1/100000000th.Due to selenium, there is the characteristics such as photaesthesia, semiconductor, so be commonly used to manufacture light activated element, optical instrument, electric elements etc.At industrial circles such as metallurgy, glass, chemistry, selenium is widely used; In nutrition, medical science, life science, it is the trace element that body weight for humans is wanted.20 beginnings of the century, have started the production of selenium in the world, but due to the impact of the factors such as selenium resource scarcity, content are extremely low, extraction process is complicated, expensive, cause its commercial Application to be greatly affected.Along with scientific and technical progress and the fast development of world economy, the continuous expansion in especially current hard-core technology field, the application of selenium constantly expands, its application mainly concentrates on the fields such as oil, chemical industry, electronics, electrical equipment, glass, metallurgy, pottery, medical industry, and is penetrated into gradually other association areas.The application of selenium constantly has new development, and semiconductor refrigerating element, thermoelectric material and solar cell are the current and following developing direction of selenium.Therefore, selenium is modern industry high development, the indispensable material of especially following high-end development in science and technology.
The primary raw material that extracts selenium is the earth of positive pole of electrolytic non-ferrous metal output, and what wherein occupy first place is the earth of positive pole of cupric electrolysis, is secondly the earth of positive pole of nickel and plumbous electrolysis, and the sour mud in nonferrous smelting and chemical plant.In the earth of positive pole and sour mud, be rich in selenium and the tellurium of high level, by in advance preliminary and smelting, making containing selenium is that (general to claim to be greater than 75%, to be less than 98% selenium product containing selenium be thick selenium for more than 75% thick selenium, in thick selenium, also contain the tellurium below 5%), through further Refining, become pure selenium, high-purity selenium.The consumption of domestic annual pure selenium, high-purity selenium is 1000～2000t, 80% mode with the thick selenium marketing at home of total amount selenium, and as the raw material of pure selenium, high-purity selenium processing factory, trading volume is larger.
At present, general coloured industry standard < < YS/T 226.12-2009 selenium chemical analysis method the 12nd part that adopts of Selenium Contents: the mensuration sodium thiosulfate volumetric method > > of selenium amount, its principle is: after test portion decomposes with acid mixture, in sulfuric acid medium, with sodium thiosulfate standard solution, carry out titration.While closing on terminal, add potassium iodide, the iodine that reaction is separated out be take starch as indicator, continues to carry out titration with sodium thiosulfate titrand, blue disappearance for terminal.The measurement range that it is applicable: 98.0%-99.0%.Thick selenium does not have corresponding, unified analytical approach, mostly use for reference coloured industry standard < < YS/T 226.12-2009 selenium chemical analysis method the 12nd part: the mensuration sodium thiosulfate volumetric method > > of selenium amount, but thick selenium is not in its scope of application, and the tellurium in thick selenium has a strong impact on measurement result, leads to controversy and dispute.
Summary of the invention
The technical problem to be solved in the present invention is the analytical approach that the existing analysis to Se content in thick selenium does not have standard, and the tellurium in thick selenium has a strong impact on measurement result, and a kind of method of analyzing Se content in thick selenium is provided for this reason.
Technical scheme of the present invention is: a kind of method of analyzing Se content in thick selenium, and it comprises the following steps:
(1), dry sample, get sample dry 2h in 100 ℃～105 ℃ baking ovens that granularity is not more than 0.098mm, and be placed in exsiccator and be cooled to room temperature;
(2), claim sample, the sample taking in 2.0g step (1) is designated as m
0, be accurate to 0.0001g;
(3), measure, sample in step (2) is placed in to 500mL conical flask, add 7mL nitric acid, in 70 ℃～80 ℃ water-baths, clear up completely, then add the hydrochloric acid of 21mL, to be dissolved completely after, take down nature cooling, cooled solution is moved in 200mL volumetric flask, with water constant volume, to 200.00mL, shake up;
(4), by the dry conical beaker that is filled into clean dry of the solution in step (3), discard initial 20mL filtrate, pipette 100.00mL filtrate in the conical beaker of 500mL, the hydrochloric acid that adds again 60mL, shake up, slowly drip the hydrazine hydrate of 50mL, on low temperature, be slowly heated to solution clarification, place and treat that it is naturally cooling;
(5), in 100 ℃～105 ℃ baking ovens dry glass core crucible constant weight, then be positioned in exsiccator after cool to room temperature, take out glass core crucible and on electronic balance, weigh and be designated as m
1, be accurate to 0.0001g;
(6), install suction filtration device, with the solution finally obtaining in glass core crucible suction filtration step (4), the precipitation first obtaining with suction filtration in distilled water cleaning glass core crucible 3～5 times, with pH test paper, measure filtrate and be neutral, with 5mL absolute ethyl alcohol, clean again, after absolute ethanol volatilizes, glass core crucible is placed in 100 ℃～105 ℃ baking ovens and is dried and constant weight, and be placed in exsiccator and be cooled to room temperature, on electronic balance, weigh, be accurate to 0.0001g, must precipitate with core crucible and close and be heavily designated as m
2;
(7), the filtrate of collecting after the suction filtration in step (6) puts into 250mL volumetric flask, adds 5mL nitric acid, with water constant volume, to 250mL, shakes up, and with the content of Se in ICP-AES spectrographic determination filtrate, is designated as c
se;
(8), the glass core crucible that precipitation is housed in step (6) is put into 100mL flat bottom beaker, add 50mL hydrochloric acid, add again 10mL nitric acid, be placed in 70 ℃～80 ℃ water-baths heating and make to precipitate dissolve complete, take off cooling after, move in 200mL volumetric flask, with water washing glass core crucible and flat bottom beaker 3～5 times, with water constant volume, to 200mL, shake up, with the content of Te in ICP-AES spectrographic determination filtrate, be designated as c
te;
(9), calculate the massfraction (%) of selenium,
M wherein
0, m
1and m
2unit is gram, c
seand c
teunit is mcg/ml.
The invention has the beneficial effects as follows that sample dissolves through acid, filter, the insoluble element of separating acid disturbs; Hydrazine hydrate reduction, filters separating part interference element; Precipitation is dissolved through acid again, and spectrophotometer tellurium, gets rid of main interference element; Filtrate, through spectrophotometer Se content, is carried out revisal to analysis result.Method adopts classical gravimetric determination, eliminates main interference element, the loss of ICP-AES spectroscopic methodology revisal filtrate selenium, accurately and reliably, analyst coverage is wide for methods and results, not only can measure thick selenium, can also measure Se content at the pure selenium below 99.9%, there is larger promotional value.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1:(1), dry sample, get sample dry 2h in 100 ℃ of baking ovens of granularity 0.098mm, and be placed in exsiccator and be cooled to room temperature;
(2), claim sample, the sample taking in 2.0g step (1) is designated as m
0, be accurate to 0.0001g;
(3), measure, sample in step (2) is placed in to 500mL conical flask, add 7mL nitric acid, in 70 ℃ of water-baths, clear up completely, then add the hydrochloric acid of 21mL, to be dissolved completely after, take down nature cooling, cooled solution is moved in 200mL volumetric flask, with water constant volume, to 200.00mL, shake up;
(4), by the dry conical beaker that is filled into clean dry of the solution in step (3), discard initial 20mL filtrate, pipette 100.00mL filtrate in the conical beaker of 500mL, the hydrochloric acid that adds again 60mL, shake up, slowly drip the hydrazine hydrate of 50mL, on low temperature, be slowly heated to solution clarification, place and treat that it is naturally cooling;
(5), in 100 ℃ of baking ovens dry glass core crucible constant weight, then be positioned in exsiccator after cool to room temperature, take out glass core crucible and on electronic balance, weigh and be designated as m
1, be accurate to 0.0001g;
(6), install suction filtration device, with the solution finally obtaining in glass core crucible suction filtration step (4), the precipitation first obtaining with suction filtration in distilled water cleaning glass core crucible 3 times, measures filtrate with pH test paper and is neutral, then clean with 5mL absolute ethyl alcohol, after absolute ethanol volatilizes, glass core crucible is placed in 100 ℃ of baking ovens and is dried and constant weight, and be placed in exsiccator and be cooled to room temperature, on electronic balance, weigh, be accurate to 0.0001g, must precipitate with core crucible and close and be heavily designated as m
2;
(7), the filtrate of collecting after the suction filtration in step (6) puts into 250mL volumetric flask, adds 5mL nitric acid, with water constant volume, to 250mL, shakes up, and with the content of Se in ICP-AES spectrographic determination filtrate, is designated as c
se;
(8), the glass core crucible that precipitation is housed in step (6) is put into 100mL flat bottom beaker, add 50mL hydrochloric acid, add again 10mL nitric acid, be placed in 70 ℃ of water-baths heating and make to precipitate dissolve complete, take off cooling after, move in 200mL volumetric flask, with water washing glass core crucible and flat bottom beaker 3 times, with water constant volume, to 200mL, shake up, with the content of Te in ICP-AES spectrographic determination filtrate, be designated as c
te;
(9), calculate the massfraction (%) of selenium,
M wherein
0, m
1and m
2unit is gram, c
seand c
teunit is mcg/ml.
Embodiment 2:(1), dry sample, getting granularity is sample dry 2h in 105 ℃ of baking ovens of 0.090mm, and is placed in exsiccator and is cooled to room temperature;
(2), claim sample, the sample taking in 2.0g step (1) is designated as m
0, be accurate to 0.0001g;
(3), measure, sample in step (2) is placed in to 500mL conical flask, add 7mL nitric acid, in 80 ℃ of water-baths, clear up completely, then add the hydrochloric acid of 21mL, to be dissolved completely after, take down nature cooling, cooled solution is moved in 200mL volumetric flask, with water constant volume, to 200.00mL, shake up;
(4), by the dry conical beaker that is filled into clean dry of the solution in step (3), discard initial 20mL filtrate, pipette 100.00mL filtrate in the conical beaker of 500mL, the hydrochloric acid that adds again 60mL, shake up, slowly drip the hydrazine hydrate of 50mL, on low temperature, be slowly heated to solution clarification, place and treat that it is naturally cooling;
(5), in 105 ℃ of baking ovens dry glass core crucible constant weight, then be positioned in exsiccator after cool to room temperature, take out glass core crucible and on electronic balance, weigh and be designated as m
1, be accurate to 0.0001g;
(6), install suction filtration device, with the solution finally obtaining in glass core crucible suction filtration step (4), the precipitation first obtaining with suction filtration in distilled water cleaning glass core crucible 5 times, measures filtrate with pH test paper and is neutral, then clean with 5mL absolute ethyl alcohol, after absolute ethanol volatilizes, glass core crucible is placed in 105 ℃ of baking ovens and is dried and constant weight, and be placed in exsiccator and be cooled to room temperature, on electronic balance, weigh, be accurate to 0.0001g, must precipitate with core crucible and close and be heavily designated as m
2;
(7), the filtrate of collecting after the suction filtration in step (6) puts into 250mL volumetric flask, adds 5mL nitric acid, with water constant volume, to 250mL, shakes up, and with the content of Se in ICP-AES spectrographic determination filtrate, is designated as c
se;
(8), the glass core crucible that precipitation is housed in step (6) is put into 100mL flat bottom beaker, add 50mL hydrochloric acid, add again 10mL nitric acid, be placed in 80 ℃ of water-baths heating and make to precipitate dissolve complete, take off cooling after, move in 200mL volumetric flask, with water washing glass core crucible and flat bottom beaker 5 times, with water constant volume, to 200mL, shake up, with the content of Te in ICP-AES spectrographic determination filtrate, be designated as c
te;
(9), calculate the massfraction (%) of selenium,
M wherein
0, m
1and m
2unit is gram, c
seand c
teunit is mcg/ml.
The present invention is exemplarily described above in conjunction with the embodiments; obviously specific implementation of the present invention is not subject to the restrictions described above; as long as adopted the improvement of the various unsubstantialities that method of the present invention design and technical scheme carry out; or without improving, design of the present invention and technical scheme are directly applied to other occasion, all within protection scope of the present invention.
Claims (1)
1. analyze a method for Se content in thick selenium, it is characterized in that it comprises the following steps:
(1), dry sample, get sample dry 2h in 100 ℃～105 ℃ baking ovens that granularity is not more than 0.098mm, and be placed in exsiccator and be cooled to room temperature;
(2), claim sample, the sample taking in 2.0g step (1) is designated as m
0, be accurate to 0.0001g;
(3), measure, sample in step (2) is placed in to 500mL conical flask, add 7mL nitric acid, in 70 ℃～80 ℃ water-baths, clear up completely, then add the hydrochloric acid of 21mL, to be dissolved completely after, take down nature cooling, cooled solution is moved in 200mL volumetric flask, with water constant volume, to 200.00mL, shake up;
(4), by the dry conical beaker that is filled into clean dry of the solution in step (3), discard initial 20mL filtrate, pipette 100.00mL filtrate in the conical beaker of 500mL, the hydrochloric acid that adds again 60mL, shake up, slowly drip the hydrazine hydrate of 50mL, on low temperature, be slowly heated to solution clarification, place and treat that it is naturally cooling;
(5), in 100 ℃～105 ℃ baking ovens dry glass core crucible constant weight, then be positioned in exsiccator after cool to room temperature, take out glass core crucible and on electronic balance, weigh and be designated as m
1, be accurate to 0.0001g;
(6), install suction filtration device, with the solution finally obtaining in glass core crucible suction filtration step (4), the precipitation first obtaining with suction filtration in distilled water cleaning glass core crucible 3～5 times, with pH test paper, measure filtrate and be neutral, with 5mL absolute ethyl alcohol, clean again, after absolute ethanol volatilizes, glass core crucible is placed in 100 ℃～105 ℃ baking ovens and is dried and constant weight, and be placed in exsiccator and be cooled to room temperature, on electronic balance, weigh, be accurate to 0.0001g, must precipitate with core crucible and close and be heavily designated as m
2;
(7), the filtrate of collecting after the suction filtration in step (6) puts into 250mL volumetric flask, adds 5mL nitric acid, with water constant volume, to 250mL, shakes up, and with the content of Se in ICP-AES spectrographic determination filtrate, is designated as c
se;
(8), the glass core crucible that precipitation is housed in step (6) is put into 100mL flat bottom beaker, add 50mL hydrochloric acid, add again 10mL nitric acid, be placed in 70 ℃～80 ℃ water-baths heating and make to precipitate dissolve complete, take off cooling after, move in 200mL volumetric flask, with water washing glass core crucible and flat bottom beaker 3～5 times, with water constant volume, to 200mL, shake up, with the content of Te in ICP-AES spectrographic determination filtrate, be designated as c
te;
(9), calculate the massfraction (%) of selenium,
M wherein
0, m
1and m
2unit is gram, c
seand c
teunit is mcg/ml.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107101905A (en) * | 2017-04-24 | 2017-08-29 | 阳谷祥光铜业有限公司 | A kind of method of Se content in measure impure selenium |
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2013
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| US4913878A (en) * | 1988-02-05 | 1990-04-03 | General Signal Corporation | Method of testing the magnesium content of magnesium-treated cast iron |
| US20090236544A1 (en) * | 2004-12-14 | 2009-09-24 | National Research Council Of Canada | Uv reactive spray chamber for enhanced sample introduction efficiency |
| CN102200500A (en) * | 2010-03-24 | 2011-09-28 | 上海宝钢工业检测公司 | Pretreatment method for inductively coupled plasma-atomic emission spectrometry (ICP-AES) test of content of elements in quaternary alloy |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107101905A (en) * | 2017-04-24 | 2017-08-29 | 阳谷祥光铜业有限公司 | A kind of method of Se content in measure impure selenium |
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