CN102072833A - Sample preparation method for measuring impurity element in high-purity arsenic by ICP-MS method - Google Patents
Sample preparation method for measuring impurity element in high-purity arsenic by ICP-MS method Download PDFInfo
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- CN102072833A CN102072833A CN201010593568.0A CN201010593568A CN102072833A CN 102072833 A CN102072833 A CN 102072833A CN 201010593568 A CN201010593568 A CN 201010593568A CN 102072833 A CN102072833 A CN 102072833A
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- arsenic
- high purity
- purity arsenic
- icp
- impurity element
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Links
- 229910052785 arsenic Inorganic materials 0.000 title claims abstract description 30
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000012535 impurity Substances 0.000 title claims abstract description 15
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 title claims abstract 5
- 238000005464 sample preparation method Methods 0.000 title abstract 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 4
- 239000001301 oxygen Substances 0.000 claims abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 39
- 239000003708 ampul Substances 0.000 claims description 14
- 239000010453 quartz Substances 0.000 claims description 14
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 3
- JRIGVWDKYXCHMG-UHFFFAOYSA-N (5-arsoroso-2-hydroxyphenyl)azanium;chloride Chemical compound Cl.NC1=CC([As]=O)=CC=C1O JRIGVWDKYXCHMG-UHFFFAOYSA-N 0.000 claims description 2
- 229910000413 arsenic oxide Inorganic materials 0.000 claims description 2
- 229960002594 arsenic trioxide Drugs 0.000 claims description 2
- 230000001186 cumulative effect Effects 0.000 claims description 2
- KTTMEOWBIWLMSE-UHFFFAOYSA-N diarsenic trioxide Chemical compound O1[As](O2)O[As]3O[As]1O[As]2O3 KTTMEOWBIWLMSE-UHFFFAOYSA-N 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 229950008475 oxophenarsine Drugs 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 4
- 238000001514 detection method Methods 0.000 abstract description 3
- 238000001036 glow-discharge mass spectrometry Methods 0.000 abstract description 3
- 238000004458 analytical method Methods 0.000 abstract description 2
- HJTAZXHBEBIQQX-UHFFFAOYSA-N 1,5-bis(chloromethyl)naphthalene Chemical compound C1=CC=C2C(CCl)=CC=CC2=C1CCl HJTAZXHBEBIQQX-UHFFFAOYSA-N 0.000 abstract 1
- GOLCXWYRSKYTSP-UHFFFAOYSA-N arsenic trioxide Inorganic materials O1[As]2O[As]1O2 GOLCXWYRSKYTSP-UHFFFAOYSA-N 0.000 abstract 1
- 239000004065 semiconductor Substances 0.000 description 4
- 239000002210 silicon-based material Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 229910052732 germanium Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 241000692870 Inachis io Species 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000003969 polarography Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a sample preparation method for measuring an impurity element in high-purity arsenic by an inductively coupled plasma-mass spectrometry (ICP-MS) method, and relates to the technical field of material analysis. The method comprises the following steps of: putting the high-purity arsenic into a special container; introducing oxygen at a certain temperature to form arsenic trioxide and sublimating to remove the arsenic; remaining the impurity element with low steam pressure in the container; resolving the remaining solution through electronic-grade nitric acid; and fixing the volume by using dilute nitric acid. By the method, the interference to the matrix element arsenic can be completely eliminated. Compared with glow discharge-mass spectrometry (GD-MS) detection data, the detection data of a sample prepared by the ICP-MS method has the characteristics of high precision and high accuracy, and is practical and feasible.
Description
Technical field
The present invention relates to the species analysis technical field, particularly detect the method for making sample of high purity arsenic with ICP-MS.
Background technology
High purity arsenic, as third generation semiconductor material, with its superior physicochemical property. by being doped in the silicon materials and being combined to forms such as gallium arsenide. the limited arithmetic speed of information capacity that has broken through silicon materials is limited, the big high capacity of work energy consumption needs undesirable or the like the limit of large volume brightness and color, be widely used in the information communication photoelectron, large scale integrated circuit, the highlighted large screen display of high definition, remote sensing, survey, far infrared, automatically control, intelligent, sulfuration optical fiber, alloy material, the 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 Semiconducting Silicon Materials replaces another the semiconductor new material revolution of first generation semiconductor material germanium after this. and its market outlook are quite wide.
At present, the assay method of impurity element is respectively and uses polarography determination Se in the domestic high purity arsenic, peacock green spectrophotometry Sb, and chemical spectroscopy is measured Co, Zn, Ag, Cu, Ca, AL, Ni, Cr, elements such as Pb, Fe.Above method sample preparation is loaded down with trivial details, and the checked for impurities element is incomplete.
Summary of the invention
The object of the invention is to design a kind of impurity and detects comprehensively, and process is measured the method for making sample of impurity element in the high purity arsenic simply, fast with the ICP-MS method.
The inventive method is: take by weighing high purity arsenic, obtain quality m
High purity arsenic , the high purity arsenic that takes by weighing is all placed in the quartz ampoule, under 300～350 ℃ of conditions,, treat that high purity arsenic after oxidation generates arsenic oxide arsenoxide distillation removal, makes quartz ampoule reduce to normal temperature to feeding quartz ampoule oxygen, take out the silica crucible that leaves residue in the quartz ampoule; The nitric acid that adds electron level in silica crucible, after clearing up fully after being heated on 150 ℃ the heating plate, adding mass percent concentration again in crucible is to be not more than 10% dilute nitric acid solution constant volume, obtains the cumulative volume V of constant volume.
More than, mixed liquor behind the constant volume is placed ICP-MS (inductance coupled plasma mass spectrometer), can accurately measure the quality of each impurity element, promptly obtain C for to measure the method for making sample of each impurity content with ICP-MS (inductance coupled plasma mass spectrometer) method
Survey, by each constituent content C=V * C of formula
Survey /m
High purity arsenic , can calculate following impurity element: Li in the high purity arsenic respectively, Be, B, Na, Mg, Al, Si, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, Sr, Y, Zr, Nb, Mo, Ru, Rh, Pd, Ag, Cd, In, Sn, Sb, Te, I, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, Ta, W, Re, Os, Ir, Pt, Au, Hg, Tl, Pb, Bi, Th, the content of U.Detected value of the present invention and GD-MS relative error are less than 10%, and sample preparation is convenient and swift, detection elements is many, can thoroughly eliminate matrix and disturb, and are particularly suitable for adopting ICP-MS ICP-MS (inductance coupled plasma mass spectrometer) method to detect containing of high purity arsenic of assorted situation.
Embodiment
(1) temperature adjustment: in advance furnace temp is transferred between 300～350 ℃ in (heating furnace with program control table temperature control).
(2) claim sample: take by weighing the high purity arsenic of 5～10g, and recording quality m
High purity arsenic , then the high purity arsenic that takes by weighing is all inserted silica crucible.
(3) shove charge: put silica crucible into quartz ampoule, again quartz ampoule is put in the heating furnace that mixes up temperature, carry out the sealing insulation at the gap location of heating furnace fire door and quartz ampoule.
(4) ventilation row arsenic (is eliminated matrix A
sDisturb): import (plastic flexible pipe inserts the following 5mm of the water surface) in the glass container that fills aqueous solution in the quartz ampoule gas outlet with the silica gel plastics flexible pipe, at the air intake opening aerating oxygen of quartz ampoule, according to steam pressure difference, the compd A s of matrix element As
2O
3Because of vapour pressure is removed 300～350 ℃ of distillations greatly, and the little impurity element of vapour pressure remains in the silica crucible.
(5) come out of the stove: take out quartz ampoule after 18 hours, the silica crucible that has the residual impurity element is taken out in cooling naturally after 30 minutes.
(6) clear up: in silica crucible, add electron level nitric acid 5ml, the crucible that has added nitric acid was put on 150 ℃ the heating plate heating 60 minutes, the interior residue of former silica crucible is cleared up fully.
(7) constant volume: the crucible mass concentration of taking off the residual impurity element is that rare nitric acid of 5% is settled to 50ml.Above process is done blank simultaneously.
(8) detect: the mixed liquor of constant volume is detected through ICP-MS (inductance coupled plasma mass spectrometer), obtain each element detected value C
Survey
(9) result of calculation: C=V * C
Survey /m
High purity arsenic
In the formula:
C---each constituent content
C
Survey ---each element instrument displayed value
V---constant volume
m
High purity arsenic ---the high purity arsenic quality
Claims (1)
1. measure the method for making sample of impurity element in the high purity arsenic with the ICP-MS method, it is characterized in that taking by weighing high purity arsenic, obtain quality m
High purity arsenic The high purity arsenic that takes by weighing is all placed silica crucible, again silica crucible is put into quartz ampoule, under 300～350 ℃ of conditions, to the quartz ampoule aerating oxygen, after treating that the high purity arsenic oxidation generates arsenic oxide arsenoxide distillation removal, make quartz ampoule reduce to normal temperature, take out the silica crucible that stays residue in the quartz ampoule, the nitric acid that in silica crucible, adds electron level, in be heated on 150 ℃ the heating plate clear up fully after, adding mass percent concentration again in crucible is to be not more than 10% dilute nitric acid solution constant volume, obtains the cumulative volume V of constant volume.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105935680A CN102072833B (en) | 2010-12-17 | 2010-12-17 | Sample preparation method for measuring impurity element in high-purity arsenic by ICP-MS method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105935680A CN102072833B (en) | 2010-12-17 | 2010-12-17 | Sample preparation method for measuring impurity element in high-purity arsenic by ICP-MS method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102072833A true CN102072833A (en) | 2011-05-25 |
| CN102072833B CN102072833B (en) | 2012-07-25 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010105935680A Active CN102072833B (en) | 2010-12-17 | 2010-12-17 | Sample preparation method for measuring impurity element in high-purity arsenic by ICP-MS method |
Country Status (1)
| Country | Link |
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| CN (1) | CN102072833B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102830155A (en) * | 2012-08-16 | 2012-12-19 | 四川鑫龙碲业科技开发有限责任公司 | Method for determining content of trace impurity element in cadmium telluride |
| CN103163120A (en) * | 2013-04-02 | 2013-06-19 | 中国兵器工业集团第五三研究所 | Method for measuring contents of Al, K, Na, Zn, Ce and Ti in irradiation-resistant glass |
| CN103308508A (en) * | 2013-05-23 | 2013-09-18 | 扬州高能新材料有限公司 | Method of detecting impurity elements in high-purity alumina frit |
| CN106442050A (en) * | 2016-09-18 | 2017-02-22 | 广东先导稀材股份有限公司 | Method for preparing sample for measuring content of impurity in high purity arsenic |
| CN113686980A (en) * | 2021-06-24 | 2021-11-23 | 上海市食品药品包装材料测试所 | Method for simultaneously determining content of 24 element impurities in hydroxyethyl starch sodium chloride injection |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU1297188A (en) * | 1987-02-12 | 1988-09-14 | Allied-Signal Inc. | Manufacture of high purity low arsenic anhydrous hydrogen fluoride |
| US6635231B2 (en) * | 2001-03-06 | 2003-10-21 | Lithdyne International | Preparation of arsenic pentafluoride |
| CN101054168A (en) * | 2006-04-13 | 2007-10-17 | 张世才 | Method for producing high-purity arsenic |
| CN101096726A (en) * | 2006-06-30 | 2008-01-02 | 杨华民 | Production method for high-purity arsenic and its equipment |
-
2010
- 2010-12-17 CN CN2010105935680A patent/CN102072833B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU1297188A (en) * | 1987-02-12 | 1988-09-14 | Allied-Signal Inc. | Manufacture of high purity low arsenic anhydrous hydrogen fluoride |
| US6635231B2 (en) * | 2001-03-06 | 2003-10-21 | Lithdyne International | Preparation of arsenic pentafluoride |
| CN101054168A (en) * | 2006-04-13 | 2007-10-17 | 张世才 | Method for producing high-purity arsenic |
| CN101096726A (en) * | 2006-06-30 | 2008-01-02 | 杨华民 | Production method for high-purity arsenic and its equipment |
Non-Patent Citations (1)
| Title |
|---|
| 《中华人民共和国有色金属行业标准》 19920313 中国有色金属工业总公司 高纯砷化学分析方法 中国有色金属工业总公司 第1版，325－327 1 , 1 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102830155A (en) * | 2012-08-16 | 2012-12-19 | 四川鑫龙碲业科技开发有限责任公司 | Method for determining content of trace impurity element in cadmium telluride |
| CN103163120A (en) * | 2013-04-02 | 2013-06-19 | 中国兵器工业集团第五三研究所 | Method for measuring contents of Al, K, Na, Zn, Ce and Ti in irradiation-resistant glass |
| CN103308508A (en) * | 2013-05-23 | 2013-09-18 | 扬州高能新材料有限公司 | Method of detecting impurity elements in high-purity alumina frit |
| CN106442050A (en) * | 2016-09-18 | 2017-02-22 | 广东先导稀材股份有限公司 | Method for preparing sample for measuring content of impurity in high purity arsenic |
| CN113686980A (en) * | 2021-06-24 | 2021-11-23 | 上海市食品药品包装材料测试所 | Method for simultaneously determining content of 24 element impurities in hydroxyethyl starch sodium chloride injection |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102072833B (en) | 2012-07-25 |
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