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Digestion method of methyl silicone oil and method for measuring content of impurity nitrogen in methyl silicone oil

A technology of methyl silicone oil and nitrogen content, applied in the direction of measuring devices, preparation of test samples, color/spectral characteristic measurement, etc., to achieve simple and convenient operation, optimized digestion and detection methods, and good chemical stability

Pending Publication Date: 2022-03-18
湖北省兴发磷化工研究院有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Due to its high viscosity and good chemical stability, there is no effective digestion method for methyl silicone oil at present. This invention provides a new idea for the digestion of methyl silicone oil and the detection of impurities

Method used

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  • Digestion method of methyl silicone oil and method for measuring content of impurity nitrogen in methyl silicone oil
  • Digestion method of methyl silicone oil and method for measuring content of impurity nitrogen in methyl silicone oil
  • Digestion method of methyl silicone oil and method for measuring content of impurity nitrogen in methyl silicone oil

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Experimental program
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Effect test

Embodiment 1

[0040] Instrument models used: Multi N / C 3100TOC / TN Synchronous Analyzer (Jena, Germany); Mars7 Microwave Extractor (CEM Microwave Chemistry).

[0041] A kind of digestion method of methyl silicone oil and the mensuration of impurity nitrogen content in the methyl silicone oil based on this method, it comprises the following steps:

[0042] 1) Weigh about 1.0g of methyl silicone oil sample and place it in a microwave digestion tank. The solid-to-liquid ratio of methyl silicone oil to digestion solution is 1:15g / ml. In the digestion solution, 10mL of hydrofluoric acid and 5mL of concentrated sulfuric acid are mixed. Seal the digestion tank and place it in a microwave digestion apparatus for digestion. The mass fraction of hydrofluoric acid in the digestion solution is 40%, and the mass fraction of concentrated sulfuric acid is 98%.

[0043] 2) Set the heating program: heat preservation at 180°C for 10 minutes, heat preservation at 240°C for 20 minutes, and microwave power of 1...

Embodiment 2

[0053] Based on Example 1, the composition of the digestion solution was changed, and the others were the same as in Example 1 (10 mL of hydrofluoric acid and 5 mL of concentrated sulfuric acid). (The volume ratio of hydrofluoric acid and 5mL concentrated sulfuric acid is 2:1)

Embodiment 2-1

[0054] Example 2-1: 11.25mL hydrofluoric acid and 3.75mL concentrated sulfuric acid; (volume ratio of hydrofluoric acid and 5mL concentrated sulfuric acid 3:1)

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Abstract

The invention relates to a method for digesting methyl silicone oil and a method for measuring the content of impurity nitrogen in the methyl silicone oil, a digestion solution is composed of hydrofluoric acid and concentrated sulfuric acid, and the volume ratio of the hydrofluoric acid to the concentrated sulfuric acid is (2-3): 1. The microwave digestion instrument is used for digesting the methyl silicone oil, high-temperature and high-pressure digestion is performed under a sealed condition, and acid is removed at a low temperature, so that the loss of detected components is effectively avoided. And measuring the content of the impurity nitrogen in the methyl silicone oil sample by using a TOC / TN synchronous analyzer. According to the method, trace impurity nitrogen in the sample can be efficiently and rapidly determined, and the blank of methyl silicone oil in sample digestion and trace impurity detection is filled.

Description

technical field [0001] The invention relates to the field of chemical detection and analysis, in particular to a method for digestion of methyl silicone oil and a method for measuring the content of impurity nitrogen in methyl silicone oil. Background technique [0002] Methyl silicone oil is a colorless and transparent substance with excellent heat resistance, water resistance, chemical stability, and other excellent physical and chemical properties. It is widely used in many fields such as machinery manufacturing. [0003] The methyl silicone oil uses a nitrogen-containing catalyst in the synthesis. After the reaction is completed, the product contains a small amount of catalyst impurities that cannot be completely removed. The impurity removal effect of the methyl silicone oil is judged by detecting the impurity nitrogen content in the product. In order to improve the The quality of the product provides the basis. [0004] Due to its high viscosity and good chemical sta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/40G01N1/44G01N21/35
CPCG01N1/4044G01N1/44G01N21/35
Inventor 荣沙沙杜建侠卢会珍李红肖清燕余晓英
Owner 湖北省兴发磷化工研究院有限公司
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