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Detection method of purity of antimony pentafluoride products

A detection method for antimony pentafluoride, which is applied in the direction of material analysis through observation of the influence of chemical indicators, analysis through chemical reaction of materials, thermal excitation analysis, etc., and can solve the problem that there is no enterprise standard, industry standard or Other standards, antimony pentafluoride has not established a unified standard, purity and valence analysis has not been reported, etc., to achieve the effect of easy operation and high measurement accuracy

Active Publication Date: 2012-06-20
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

[0003] At present, there is no literature report on the determination of the purity of antimony pentafluoride, only reports on the determination of impurity antimony in alloys, such as photometric determination of antimony content, ion chromatography, atomic fluorescence, atomic absorption spectrometry and atomic emission spectrometry, etc. However, they are all reports on the determination of low-content antimony, and there are no reports on the determination of the purity of antimony fluoride and the analysis of the valence state of antimony.
[0004] So far, there is no uniform standard for the purity analysis of antimony pentafluoride at home and abroad, and there are no corresponding enterprise standards, industry standards or other standards

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Sample preparation

[0042] Take a sample from the product bottle to a sampling bottle made of polytetrafluoroethylene, and weigh the antimony pentafluoride sample by differential gravimetric method. The sample weight is 5.2124g.

[0043] At 8°C, the sample was solidified into a solid.

[0044] Put 150ml of deionized water in a beaker made of polytetrafluoroethylene, put 5.2124g of solid antimony pentafluoride sample into deionized water in an ice water bath to make it completely hydrolyzed, and dilute to 250ml.

[0045] Trivalent antimony quantification

[0046] Take 25ml of antimony pentafluoride hydrolysis solution and titrate with 0.01008mol / L potassium permanganate standard solution. When the sample solution is light pink and does not change color within 30 seconds, record the volume of potassium permanganate standard solution to be 1.23 ml, the calculated trivalent antimony content is 0.0377g.

[0047] Antimony total content detection

[0048] Prepare a series of antimony st...

Embodiment 2

[0051] Sample preparation

[0052] Take a sample from the product bottle to a sampling bottle made of polytetrafluoroethylene, and weigh the antimony pentafluoride sample by differential gravimetric method. The weight of the sample is 10.0615 g.

[0053] At 0°C, the sample was solidified into a solid.

[0054] Put 300ml of deionized water in a beaker made of polytetrafluoroethylene, put the weighed solid antimony pentafluoride sample into deionized water in an ice water bath, make it hydrolyze completely, and dilute to 500ml .

[0055] Trivalent antimony quantification

[0056] Take 50ml of antimony pentafluoride hydrolysis solution and titrate with 0.01008mol / L potassium permanganate standard solution. When the sample solution is light pink and does not change color within 30 seconds, record the volume of the standard solution to 2.15ml, and calculate The trivalent antimony content is 0.0660g.

[0057] Antimony total content detection

[0058] Prepare a series of antimony standard solu...

Embodiment 3

[0061] Sample preparation

[0062] Take a sample from the product bottle to a sampling bottle made of polytetrafluoroethylene, and weigh the antimony pentafluoride sample by differential gravimetric method. The weight of the sample is 14.1089 g.

[0063] At -10°C, the sample is solidified into a solid.

[0064] Put 500ml of deionized water in a beaker made of polytetrafluoroethylene, put the weighed solid antimony pentafluoride sample into deionized water in an ice water bath, make it completely hydrolyzed, and dilute to 1000ml .

[0065] Trivalent antimony quantification

[0066] Take 100ml of antimony pentafluoride hydrolysis solution and titrate it with 0.01008mol / L potassium permanganate standard solution. When the sample solution is light pink and does not change color within 30 seconds, record the volume of the standard solution used as 2.89ml, calculated The trivalent antimony content is 0.0887g.

[0067] Antimony total content detection

[0068] Prepare a series of antimony stan...

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Abstract

The invention discloses a detection method of purity of antimony pentafluoride products. The detection method comprises the following steps of: (i) preparing a sample, including sampling, solidifying and hydrolyzing; (ii) quantifying trivalent antimony, namely utilizing an oxidation-reduction titration method to measure the trivalent antimony; (iii) detecting total content of antimony, namely using an inductively coupled plasma emission spectrometer, selecting 206.836nm as an analytical line used for measuring, and detecting the content of total antimony elements in hydrolysate; (iv) calculating the content of pentavalent antimony, namely subtracting the content of the trivalent antimony from the total content of the antimony elements to obtain the content of the pentavalent antimony; andthrough calculating, obtaining the purity of the antimony pentafluoride products. The detection method is simple and convenient and feasible and is convenient for operation, the measurement accuracy is high, and the method is particularly suitable for detecting the purity of the antimony pentafluoride products prepared by fluoride and simple substance antimony as raw materials.

Description

Technical field [0001] The invention belongs to a method for detecting the purity of antimony pentafluoride products, and specifically relates to a method for detecting the purity of antimony pentafluoride products prepared by using fluorine gas and elemental antimony as raw materials. Background technique [0002] Antimony pentafluoride (SbF 5 ) Is a high-energy fluorinating agent. It is the main component of the catalyst in perfluoroalkyl iodide (PFAIS). It is the main product to replace chloroalkane refrigeration. It is the catalyst for the production of refrigeration difluoromethane. It is the production of new explosives and jets. The catalyst of fuel is the catalyst of certain drugs (such as fluoromethyl quinoline, etc.), the additive of anti-cancer drugs, and the intermediate of special membranes, plastics, lubricants, medical anesthetics, blood substitutes, etc. It is an improvement Catalyst for the production of gasoline-quality isobutylation. [0003] At present, there a...

Claims

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Application Information

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IPC IPC(8): G01N21/79G01N21/71
Inventor 张桂芬邓建平钱琳王萍丽贺邓仝庆李于教
Owner RES INST OF PHYSICAL & CHEM ENG OF NUCLEAR IND
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