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Testing method for purity of germanium tetrafluoride product

A technology of germanium tetrafluoride and product purity, which is applied in the direction of material analysis by observing the influence of chemical indicators, and analysis by making materials undergo chemical reactions, and can solve the problem of no enterprise standards, industry standards or other standards, four Germanium fluoride has not established a unified standard, etc., to achieve the effect of easy operation and high measurement accuracy

Active Publication Date: 2016-02-03
RES INST OF PHYSICAL & CHEM ENG OF NUCLEAR IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] So far, the purity analysis of germanium tetrafluoride at home and abroad has not established a unified standard, and there are no corresponding enterprise standards, industry standards or other standards

Method used

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  • Testing method for purity of germanium tetrafluoride product
  • Testing method for purity of germanium tetrafluoride product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (i) Sample preparation

[0034] a. 0.6853g germanium tetrafluoride is taken out from the sample bottle by a sampling device;

[0035] b. Quantitatively absorb the sample with 20mL of 1g / ml sodium hydroxide absorption solution;

[0036] c. Transfer the solution into a beaker, add a sulfuric acid solution with a volume ratio of sulfuric acid to water of 1:1 to neutralize until the solution is slightly acidic;

[0037] d. Transfer the solution obtained in step c to a volumetric flask, and dilute to 100mL with water to obtain the sample solution;

[0038] (ii) Purity analysis of germanium tetrafluoride product

[0039] Utilize potassium iodate volumetric method to carry out titration analysis to germanium tetrafluoride sample solution, get step (i) gained sample solution 5mL in Erlenmeyer flask, add 10mL water, 3mL massfraction is the hydrochloric acid of 37%, 10mL massfraction is 85% phosphoric acid, 3g sodium hypophosphite, seal the conical flask with a cover funnel, t...

Embodiment 2

[0041] (i) Sample preparation

[0042] a. 4.2102g germanium tetrafluoride is taken out from the sample bottle by a sampling device;

[0043] b. Quantitatively absorb the sample with 40mL of 1g / ml sodium hydroxide absorption solution;

[0044] c. Transfer the solution into a beaker, add a sulfuric acid solution with a volume ratio of sulfuric acid to water of 1:1 to neutralize until the solution is slightly acidic;

[0045] d. Transfer the solution obtained in step c to a volumetric flask, and dilute to 500mL with water to obtain the sample solution;

[0046] (ii) Purity analysis of germanium tetrafluoride product

[0047] Utilize potassium iodate volumetric method to carry out titration analysis to germanium tetrafluoride sample solution, get step (i) gained sample solution 50mL in Erlenmeyer flask, add 10mL water, 6mL massfraction is the hydrochloric acid of 37%, 20mL massfraction is 85% phosphoric acid, 4g sodium hypophosphite, seal the conical flask with a cover funnel, ...

Embodiment 3

[0049] (i) Sample preparation

[0050] a. 7.8014g germanium tetrafluoride is taken out from the sample bottle by a sampling device;

[0051] b. Quantitatively absorb the sample with 40mL of 1g / ml sodium hydroxide absorption solution;

[0052]c. Transfer the solution into a beaker, add a sulfuric acid solution with a volume ratio of sulfuric acid to water of 1:1 to neutralize until the solution is slightly acidic;

[0053] d. Transfer the solution obtained in step c to a volumetric flask, and dilute to 500mL with water to obtain the sample solution;

[0054] (ii) Purity analysis of germanium tetrafluoride product

[0055] Utilize potassium iodate volumetric method to carry out titration analysis to germanium tetrafluoride sample solution, get step (i) gained sample solution 50mL in conical flask, add 10mL water, 10mL mass fraction are 37% hydrochloric acid, 40mL mass fraction is 85% phosphoric acid, 6g sodium hypophosphite, use a cover funnel to seal the conical flask, then ...

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Abstract

The invention discloses a method for detecting the purity of a germanium tetrafluoride product and belongs to the field of halides of germanium. The detection method comprises performing titrimetric analysis on a germanium tetrafluoride product test sample by a potassium iodate volumetric method, and comprises the following specific steps of: absorbing germanium tetrafluoride from the sample by using an alkali absorption liquid and performing acidizing treatment on the solution after absorption by using sulfuric acid. Under an acidic condition, tetravalent germanium is reduced to bivalent germanium by using a reducing agent (potassium iodate); starch is used as an indicator; the standard solution of potassium iodate is used for titration; finally, the purity of the germanium tetrafluoride product is obtained through formula calculation. The method provided by the invention is simple and easy to implement, convenient to operate, high in measurement accuracy, and especially suitable for analysis of the germanium tetrafluoride product which is prepared through direct reaction of fluorine and germanium and has the purity of more than 95%.

Description

technical field [0001] The invention belongs to the field of germanium halides, in particular to a method for detecting the purity of germanium tetrafluoride products. Background technique [0002] Germanium tetrafluoride is an important semiconductor raw material for metal germanium chemical vapor deposition, and is an isotope additive for double beta decay test experiments. [0003] Germanium tetrafluoride products have the following special chemical properties: Germanium tetrafluoride is a colorless gas at normal temperature and pressure, is extremely sensitive to air, and emits smoke when it meets air. Soluble in water, the mixture with hydrogen fluoride can corrode low carbon steel, aluminum, etc. Germanium tetrafluoride is a poisonous gas, which has a strong irritation and corrosion effect on the respiratory tract, eyes and skin. [0004] Due to the special chemical properties of germanium tetrafluoride, the sampling, sample preparation and analysis of germanium tetr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/79
Inventor 贾玲玲崔学文邓建平肖初李长富钱琳
Owner RES INST OF PHYSICAL & CHEM ENG OF NUCLEAR IND
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