CN101587072B - Method of detecting Se in high-purity arsenic trioxide - Google Patents
Method of detecting Se in high-purity arsenic trioxide Download PDFInfo
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- CN101587072B CN101587072B CN2009100329291A CN200910032929A CN101587072B CN 101587072 B CN101587072 B CN 101587072B CN 2009100329291 A CN2009100329291 A CN 2009100329291A CN 200910032929 A CN200910032929 A CN 200910032929A CN 101587072 B CN101587072 B CN 101587072B
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- arsenic trioxide
- filtrate
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- solution
- purity arsenic
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- HJTAZXHBEBIQQX-UHFFFAOYSA-N 1,5-bis(chloromethyl)naphthalene Chemical compound C1=CC=C2C(CCl)=CC=CC2=C1CCl HJTAZXHBEBIQQX-UHFFFAOYSA-N 0.000 title claims abstract description 30
- GOLCXWYRSKYTSP-UHFFFAOYSA-N arsenic trioxide Inorganic materials O1[As]2O[As]1O2 GOLCXWYRSKYTSP-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000706 filtrate Substances 0.000 claims abstract description 16
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 15
- 238000001514 detection method Methods 0.000 claims abstract description 10
- 239000012498 ultrapure water Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 229910002651 NO3 Inorganic materials 0.000 claims description 5
- 229910052785 arsenic Inorganic materials 0.000 claims description 5
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 7
- 238000001036 glow-discharge mass spectrometry Methods 0.000 abstract description 4
- 238000004458 analytical method Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000001704 evaporation Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000011669 selenium Substances 0.000 description 24
- 239000000243 solution Substances 0.000 description 21
- 229910052711 selenium Inorganic materials 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 4
- 239000012086 standard solution Substances 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 2
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 2
- 239000002210 silicon-based material Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 208000030208 low-grade fever Diseases 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
Method of detecing Se in high-purity arsenic trioxide, relates to material analysis technology field, dissolving the high-purity arsenic trioxide into high-purity water, evaporating to remove water and then cooling to separate out the arsenic trioxide, keeping the filtrate, using the filtrate to prepare hydrochloric acid solution of 20% volume concentration, using potassium hydroxide and potassiumborohydride to react with the hydrochloric acid solution, taking a solution containing Se[+4] to detect Se content in the filtrate via hydrogenation-flame atomic fluorescence spectrophotometer, and then calculating Se content in high-purity arsenic trioxide according to Se content in filtrate. The invention can eliminate interference of As and has small investment in equipment (less than 200 thousands), and has better accuracy by comparing detection data with GD-MS detection data repeatedly.
Description
Technical field
The present invention relates to the detection method of selenium in the species analysis technical field, particularly high-purity arsenic trioxide.
Background technology
High-purity arsenic trioxide is starting material of making high purity arsenic, and high purity arsenic is as photoelectric material, and third generation semiconductor material especially is with its superior physicochemical property, by being doped in the silicon materials and being combined to forms such as gallium arsenide, the information capacity that has broken through silicon materials is limited.Arithmetic speed is limited, the work energy consumption is big, high capacity needs undesirable or the like the limit of large volume, brightness and color, be widely used in information, communication, photoelectron, large scale integrated circuit, the highlighted large screen display of high definition. remote sensing, detection, far infrared, control, intellectuality automatically, sulfuration optical fiber, alloy material, medicine, Medical Devices, space equipment, space flight and aviation, military equipment or the like industrial field. and orientated as the great strategic basic material that supports high-tech industry, modernization construction and intelligent war industry development by countries in the world.The production of high purity arsenic and application are continue the semiconductor electronic pipe. and second generation semiconductor material " silicon " replacement first generation semiconductor material " germanium " another the semiconductor new material revolution after this. its market outlook are quite wide.
The detection method of high-purity arsenic trioxide selenium adopts methods such as GD-MS, ICP-MS usually at present, but GD-MS, ICP-MS apparatus expensive (more than 1,000,000).
Summary of the invention
The object of the invention be to provide a kind of equipment investment little, detect the data detection method of Se in the high-purity arsenic trioxide accurately.
The present invention includes following steps: high-purity arsenic trioxide is dissolved in the high purity water more than 16 megaohms fully, cooling, filter, filtrate evaporated under temperature conditions below 100 ℃ remove moisture content, be cooled to below 20 ℃ again and separate out arsenic trioxide, leave and take filtrate, getting filtrate, to be mixed with volumetric concentration be 20% hydrochloric acid solution, with potassium hydroxide and potassium borohydride and the reaction of described hydrochloric acid solution, get and contain Se
+ 4Solution; Simultaneously, respectively with mass concentration be 0,2,5,10, the Se solution of 20ng/ml sets up hydrogenation-NITRATE BY FLAME ATOMIC fluorescence spectrophotometer multipoint method typical curve; Get the described Se of containing
+ 4Solution detect the content of Se in the filtrate through hydrogenation-NITRATE BY FLAME ATOMIC fluorophotometric instrument, again according to the content of cubage Se in high-purity arsenic trioxide of Se in the filtrate.
In order to dissolve high-purity arsenic trioxide fast, heat to 30～80 ℃.
In addition, after sample dissolves fully, be cooled to below 20 ℃ and filter.
The present invention is poor according to solubility of substances, adopts high purity water to remove principal goods matter arsenic trioxide, and moisture content is removed in evaporation, and arsenic trioxide is separated out in cooling, eliminates the interference of As, with SeO
2The trace SeO that form exists
2All stay in the filtrate.Being mixed with 20% hydrochloric acid solution, is that reductive agent makes element generate SeH with potassium hydroxide and potassium borohydride
4, set up typical curve through hydrogenation-NITRATE BY FLAME ATOMIC fluorescence spectrophotometer multipoint method and detect Se
+ 4Concentration, and go out the content of Se impurity at high-purity arsenic trioxide according to the Mass Calculation of high-purity arsenic trioxide.Present device investment little (below 200,000) repeatedly relatively detects data relatively with GD-MS by detecting data, and its accuracy is better.
Description of drawings
Fig. 1 is for entering the multipoint method typical curve that hydrogenation-atomic fluorescence spectrometer is set up with the Se standard solution for preparing.
Embodiment
Operation steps:
(1) will take by weighing certain mass (m
Arsenic trioxide) high-purity arsenic trioxide, be heated to 30～80 ℃, make it be dissolved in the above high purity water of 16 megaohms fully; Cool to 20 ℃ to room temperature.
(2) filter, filtrate A is evaporated under temperature conditions below 100 ℃ remove moisture content.
(3) be cooled to again below 20 ℃ and separate out arsenic trioxide, leave and take liquor B.
(4) getting liquor B, to be mixed with 50ml, hydrochloric acid volumetric concentration be 20% hydrochloric acid solution, specific operation process is as follows: get liquor B in the 50ml volumetric flask, adding sub-boiling distillation, to cross volumetric concentration be 30%～38% hydrochloric acid 20ml, be diluted to 50ml with high purity water, shake up, the hydrochloric acid volumetric concentration is 20% in this solution to be checked.
(5) with potassium hydroxide and potassium borohydride and hydrochloric acid solution reaction, get and contain Se
+ 4Solution to be checked.
(6) prepare respectively that mass concentration is 0,2,5,10, the Se standard solution of 20ng/ml.Specific operation process is as follows:
1. take by weighing the high-purity Se powder of 1.0000g, adding 20mL volumetric concentration is 50% HNO
3Aqueous solution, the low-grade fever dissolving moves in the 1000mL volumetric flask, adds 200mLHCl again, and cooling, shakes up to scale with distilled water diluting, and this solution S e concentration is 1000 μ g/mL storing solutions 1.
2. draw in the 1.00mL storing solution 1 immigration 100mL volumetric flask that upward step makes, be diluted to 100mL with 20%HCl (v/v), shake up, this solution S e concentration is 10.0 μ g/mL storing solutions 2.
3. draw 1.00mL storing solution 2 and move in the 100mL volumetric flask, be diluted to 100mL with 20%HCl (v/v), shake up, this solution S e concentration is 100ng/mL storing solution 3.
4. be that the storing solution 3 of 100ng/mL joins that concentration is respectively 0,2,5,10, the standard solution 1,2,3,4,5 (seeing the following form) of 20ng/ml with Se concentration respectively again:
| Standard No. | Add 100ng/mL standard volume (mL) | Add HCl volume (mL) | Final volume (mL) | Normal concentration ng/mL |
| 1? | 0.00? | 20? | 100? | 0.0? |
| 2? | 2.00? | 20? | 100? | 2.0? |
| 3? | 5.00? | 20? | 100? | 5.0? |
| 4? | 10.00? | 20? | 100? | 10.0? |
| 5? | 20.00? | 20? | 100? | 20.0? |
(7) enter hydrogenation-atomic fluorescence spectrometer with the standard solution 1,2,3,4,5 for preparing and set up the multipoint method typical curve, as shown in Figure 1.
Fitting formula: y=158.2393x+308.2899
r＝0.999926
Test condition: lamp current: 80mA, negative high voltage :-350V, integral time: 5S, revolution speed: 100 rev/mins.
Method of testing: multipoint method.
(8) set up typical curve after, get and contain Se
+ 4Solution to be checked measure Se content C with hydrogenation-atom fluorescent luminosity instrument.
(9) result of calculation: C
Selenium=50 * C/m
Arsenic trioxide
In the formula:
C
Sulphur---Se content ng/ml
m
Arsenic trioxide---the arsenic trioxide quality
C---Se content in the solution to be checked
50---selenium element liquor capacity to be measured.
Selenium check and analysis result in the high-purity arsenic trioxide:
Claims (3)
1. the detection method of Se in the high-purity arsenic trioxide is got and is contained Se
+ 4Solution detect the content of Se in the filtrate through hydrogenation-NITRATE BY FLAME ATOMIC fluorophotometric instrument, again according to the content of cubage Se in high-purity arsenic trioxide of Se in the filtrate, it is characterized in that producing and contain Se
+ 4The method of solution may further comprise the steps: high-purity arsenic trioxide is dissolved in the high purity water more than 16 megaohms fully, cooling, filter, filtrate evaporated under temperature conditions below 100 ℃ remove moisture content, be cooled to below 20 ℃ again and separate out arsenic trioxide, leave and take filtrate, getting filtrate, to be mixed with volumetric concentration be 20% hydrochloric acid solution, with potassium hydroxide and potassium borohydride and the reaction of described hydrochloric acid solution, get and contain Se
+ 4Solution; Simultaneously, respectively with mass concentration be 0,2,5,10, the Se solution of 20ng/ml sets up hydrogenation-NITRATE BY FLAME ATOMIC fluorescence spectrophotometer multipoint method typical curve.
2. according to the detection method of Se in the described high-purity arsenic trioxide of claim 1, it is characterized in that: during the dissolving high-purity arsenic trioxide, heat to 30～80 ℃.
3. according to the detection method of Se in claim 1 or the 2 described high-purity arsenic trioxides, it is characterized in that: after sample dissolves fully, be cooled to below 20 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009100329291A CN101587072B (en) | 2009-06-09 | 2009-06-09 | Method of detecting Se in high-purity arsenic trioxide |
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| CN2009100329291A CN101587072B (en) | 2009-06-09 | 2009-06-09 | Method of detecting Se in high-purity arsenic trioxide |
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| CN101587072A CN101587072A (en) | 2009-11-25 |
| CN101587072B true CN101587072B (en) | 2010-12-29 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102519933A (en) * | 2011-12-20 | 2012-06-27 | 苏州硒谷科技有限公司 | Method for determining form of selenium in selenium-enriched edible fungi |
| CN104422672B (en) * | 2013-08-21 | 2018-08-17 | 上海宝钢工业技术服务有限公司 | Using the method for Se content in micro-wave digestion-In Soil With Atomic Fluorescence |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1120018A (en) * | 1994-05-07 | 1996-04-10 | 湖南大学 | Method of wet-extraction for arsenic |
| CN101412538A (en) * | 2008-11-10 | 2009-04-22 | 江苏康洁环境工程有限公司 | Method for extracting arsenic trioxide from roasting dust of arsenic-containing gold concentrate powder |
-
2009
- 2009-06-09 CN CN2009100329291A patent/CN101587072B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1120018A (en) * | 1994-05-07 | 1996-04-10 | 湖南大学 | Method of wet-extraction for arsenic |
| CN101412538A (en) * | 2008-11-10 | 2009-04-22 | 江苏康洁环境工程有限公司 | Method for extracting arsenic trioxide from roasting dust of arsenic-containing gold concentrate powder |
Non-Patent Citations (3)
| Title |
|---|
| 吴东华 等.锑及三氧化二锑化学分析方法 硒量的测定 原子荧光光谱法.GB/T 3253.6-2008 锑及三氧化二锑化学分析方法 硒量的测定 原子荧光光谱法.2008,第1页第2段,第2页第4-6段,第7页第1段. |
| 吴东华等.锑及三氧化二锑化学分析方法 硒量的测定 原子荧光光谱法.GB/T 3253.6-2008 锑及三氧化二锑化学分析方法 硒量的测定 原子荧光光谱法.2008,第1页第2段,第2页第4-6段,第7页第1段. * |
| 陈莉.砒霜的无害化处理方法研究.应用科技.2009,(2),全文. * |
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