CN103645241A - Determination method for impurity arsenic in trichlorosilane - Google Patents
Determination method for impurity arsenic in trichlorosilane Download PDFInfo
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- CN103645241A CN103645241A CN201310720900.9A CN201310720900A CN103645241A CN 103645241 A CN103645241 A CN 103645241A CN 201310720900 A CN201310720900 A CN 201310720900A CN 103645241 A CN103645241 A CN 103645241A
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Abstract
The invention discloses a determination method for impurity arsenic in trichlorosilane. The determination method comprises the following steps: metering 15ml of a trichlorosilane sample in a closed treatment device protected under insert gas; putting the trichlorosilane sample into a platinum crucible and heating at a low temperature of 30 DEG C until the sample is dried; adding 0.1mL-0.3mL of electron-grade hydrogen peroxide and adding 1mL of electron-grade hydrofluoric acid; raising the temperature to 150 DEG C and evaporating the sample to be dried; leaching the impurity arsenic out by using 3mL of 1v% nitric acid; determining the content of the arsenic in a trichlorosilane sample solution; and after volatilizing all base bodies of the trichlorosilane sample at the low temperature of 30 DEG C in the pre-treatment process of the trichlorosilane sample, adding the electron-grade hydrogen peroxide. A phenomenon that the hydrogen peroxide is directly added into the sample, the reaction is severe and a large quantity of hydrolysates are generated can be prevented; meanwhile, trivalent arsenic is converted into a pentavalent arsenic compound which is not easy to volatilize and the determined result shows that the recycling rate of the arsenic is increased.
Description
Technical field
The present invention relates to chemical field, be specifically related to a kind of assay method of arsenic.
Background technology
Trichlorosilane for silicon epitaxy (TCS) is the novel silicon source gas of used in electronic industry, is to be widely used in the critical materials of producing polysilicon and semiconductor devices.The content of the metallic impurity elements in trichlorosilane, can affect resistivity and the conductivity model of silicon chip, so very high to the purity requirement of trichlorosilane, in Accurate Determining trichlorosilane, the content of impurity element is extremely important.Conventionally in trichlorosilane, main impurity element has boron, phosphorus, arsenic and aluminium etc.
Arsenic mainly exists with arsenic trichloride form in trichlorosilane, because its boiling point is lower, in trichlorosilane sample pretreatment process, can cause the recovery of arsenic on the low side because of volatilization, the content of arsenic element in cannot Accurate Determining trichlorosilane, is therefore necessary to seek the method for arsenic content in Accurate Determining trichlorosilane.
Summary of the invention
Goal of the invention: the object of the invention is to for the deficiencies in the prior art, provide a kind of and arsenic is converted into stable compound so that the measurement result assay method of arsenic impurities in trichlorosilane accurately.
Technical scheme: the assay method that the invention provides arsenic impurities in a kind of trichlorosilane, in the closed processes device of inert gas shielding, measure 15ml trichlorosilane sample, be placed in platinum crucible, 30 ℃ of low-temperature heats, to sample evaporate to dryness, add 0.1 ~ 0.3mL electronic grade hydrogen peroxide, then add 1mL electronic-stage hydrofluoric acid, be warming up to 150 ℃, treat that sample evaporation, to dry, leaches arsenic impurities with the nitric acid that 3mL volume fraction is 1%, measure the content of arsenic in trichlorosilane sample solution; Arsenic element main existence form in trichlorosilane is arsenic trichloride, its boiling point is 130 ℃, while not adding hydrogen peroxide, the arsenious recovery is on the low side, lower than 30%, after adding 0.3mL hydrogen peroxide, arsenic is oxidized to not volatile pentavalent arsenic compound from trivalent arsenic, and the recovery is 99%, therefore the content of this method energy Accurate Determining trichlorosilane arsenic in sample.
Further, use is equipped with the icp ms of crash response pool technology to measure the content of arsenic in trichlorosilane, measurement range is 0.01ng/g～10ng/g, inductivity coupled plasma mass spectrometry crash response pool technology can effectively be eliminated the interference that ArCl diatomics is measured arsenic element, has greatly improved the accuracy that arsenic is analyzed.
Beneficial effect: in trichlorosilane sample pretreatment process, under 30 ℃ of low temperature, after the volatilization of trichlorosilane sample matrices is eliminated, add again electronic grade hydrogen peroxide, in the time of can preventing from directly hydrogen peroxide being added to sample, produce the generation of vigorous reaction and a large amount of hydrolysates, again trivalent arsenic is changed into not volatile pentavalent arsenic compound, in measurement result, the recovery of arsenic improves simultaneously; In addition, determined that adding the method for hydrogen peroxide to compare adds other oxygenants, can play good oxidation, analytic process has not been produced to interference, again the platinum crucible using has not been produced to corrosion.
Embodiment
Below technical solution of the present invention is elaborated, but protection scope of the present invention is not limited to described embodiment.
embodiment:
Embodiment 1: in the closed processes device of inert gas shielding; the trivalent arsenic standard solution of 30ng/g is added in platinum crucible; add again 15mL trichlorosilane sample; after 30 ℃ of low temperature evaporates to dryness; add 0.1mL electronic grade hydrogen peroxide that trivalent arsenic is wherein oxidized to not volatile pentavalent arsenic; add 1mL electronic-stage hydrofluoric acid; be heated to 150 ℃; make the silicon dioxide hydrolysate producing in reagent adding procedure be converted into volatile silicon tetrafluoride; after volatilization eliminates; arsenic impurities enrichment of element is in crucible bottom, the HNO that is then 1% by 3mL volume fraction
3solution leaches arsenic element, and solution is used icp ms to measure, and recording trivalent arsenic content in the standard solution adding is 22.5ng/g, thereby show that the recovery that trivalent arsenic is measured is 75%.
Comparative example as the present embodiment; in the closed processes device of inert gas shielding; the trivalent arsenic standard solution of 30ng/g is added in platinum crucible; add again after 30 ℃ of low temperature evaporates to dryness of 15mL trichlorosilane sample; do not add electronic grade hydrogen peroxide; only add 1mL electronic-stage hydrofluoric acid, 150 ℃ of evaporates to dryness, use 3mL1%HNO
3solution leaches arsenic element, and solution is measured by icp ms, and recording trivalent arsenic content is 9ng/g, and the recovery of arsenic is only 30%, and reason is because trivalent arsenic is unstable, volatile, causes arsenic measured quantity seriously less than normal.
Embodiment 2: change the addition of electronic grade hydrogen peroxide in embodiment 1 into 0.2mL, other conditions are identical, and the recovery that calculates trivalent arsenic mensuration becomes 86%.
Embodiment 3: change the addition of electronic grade hydrogen peroxide in embodiment 1 into 0.3mL, other conditions are identical, and the recovery that calculates trivalent arsenic mensuration becomes 99%.
As mentioned above, although represented and explained the present invention with reference to specific preferred embodiment, it shall not be construed as the restriction to the present invention self.Not departing under the spirit and scope of the present invention prerequisite of claims definition, can make in the form and details various variations to it.
Claims (2)
1. the assay method of arsenic impurities in a trichlorosilane; it is characterized in that: in the closed processes device of inert gas shielding, measure 15ml trichlorosilane sample; be placed in platinum crucible; 30 ℃ of low-temperature heats, to sample evaporate to dryness, add 0.1 ~ 0.3mL electronic grade hydrogen peroxide, then add 1mL electronic-stage hydrofluoric acid; be warming up to 150 ℃; treat that sample evaporation, to dry, leaches arsenic impurities with the nitric acid that 3mL volume fraction is 1%, measure the content of arsenic in trichlorosilane sample solution.
2. the assay method of arsenic impurities in trichlorosilane according to claim 1, is characterized in that: the content that uses arsenic in the icp ms mensuration trichlorosilane that is equipped with crash response pool technology.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310720900.9A CN103645241A (en) | 2013-12-24 | 2013-12-24 | Determination method for impurity arsenic in trichlorosilane |
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| CN201310720900.9A CN103645241A (en) | 2013-12-24 | 2013-12-24 | Determination method for impurity arsenic in trichlorosilane |
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| CN103645241A true CN103645241A (en) | 2014-03-19 |
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| CN201310720900.9A Pending CN103645241A (en) | 2013-12-24 | 2013-12-24 | Determination method for impurity arsenic in trichlorosilane |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107643281A (en) * | 2017-09-29 | 2018-01-30 | 通标标准技术服务有限公司 | Industrial silicon dirt content test method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1403372A (en) * | 2002-10-23 | 2003-03-19 | 同济大学 | Method of producing polysilicon with mixed source of trichloro-hydrosilicon and silicon tetrachloride |
-
2013
- 2013-12-24 CN CN201310720900.9A patent/CN103645241A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1403372A (en) * | 2002-10-23 | 2003-03-19 | 同济大学 | Method of producing polysilicon with mixed source of trichloro-hydrosilicon and silicon tetrachloride |
Non-Patent Citations (3)
| Title |
|---|
| 何健: "三价砷的检测", 《当代化工》 * |
| 国标: "《中华人民共和国国家标准》", 31 December 2012, 中国国家标准化管理委员会 * |
| 张志等: "氧化-混凝工艺处理碱性含砷废水的试验研究", 《工业水处理》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107643281A (en) * | 2017-09-29 | 2018-01-30 | 通标标准技术服务有限公司 | Industrial silicon dirt content test method |
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Application publication date: 20140319 |
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