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Method for determining methyltrichlorosilane in dimethyl dichlorosilane

A technology of dimethyldichlorosilane and methyltrichlorosilane, which is applied in the field of production and detection of dimethyldichlorosilane, can solve the problems of downstream process inspection requirements, unsatisfactory sensitivity and accuracy, etc.

Inactive Publication Date: 2018-03-27
JIANGXI BLUESTAR XINGHUO SILICONE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Dimethyldichlorosilane is the basic product of organosilicon synthesis and the main raw material for downstream products of organosilicon. In the relevant national standards of dimethyldichlorosilane, the main content analysis is emphasized, while its trace impurity component, methyltrichlorosilane , is an integral part of the T chain link, and plays a vital role in the quality of downstream hydrolyzate, 107 rubber, raw rubber, hydroxyl silicone oil and other products; and under the current national standard method conditions related to dimethyldichlorosilane, Methyltrichlorosilane is quantified by the area normalization method of a thermal conductivity detector, and the sensitivity and accuracy cannot meet the inspection requirements of downstream processes

Method used

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  • Method for determining methyltrichlorosilane in dimethyl dichlorosilane
  • Method for determining methyltrichlorosilane in dimethyl dichlorosilane
  • Method for determining methyltrichlorosilane in dimethyl dichlorosilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Chromatograph: American Aglient, 7890A

[0016] (1) Determination of correction factor.

[0017] Chromatographic conditions: column temperature: initial temperature 40 °C, keep 6 min, first order rate 10 °C / min, end temperature 200 °C, keep 10 min; vaporization temperature: 200 °C; detection temperature: 300 °C; carrier gas flow rate (high-purity nitrogen ): 1.5 ml / min; hydrogen flow rate: 30 ml / min; air flow rate: 350 ml / min; split ratio: 100:1; injection volume: 0.4μl; capillary column: trifluoropropyl-methylpolysiloxane Alkane, 30m * 0.53mm * 1μm.

[0018] Dimethyldichlorosilane, n-octane and methyltrichlorosilane used in this example are chromatographically pure reagents.

[0019] Weigh 15ml of dimethyldichlorosilane in a headspace bottle, the weight is 12.5956g, and the content of 100ul is 99.6% CH 3 SiCl 3 , with a weight of 0.0939g, prepared CH 3 SiCl 3 The concentration is 7370ug / g mother liquor.

[0020] Accurately 10ml dimethyldichlorosilane, 10ul conte...

Embodiment 2

[0042] CH in dimethyldichlorosilane 3 SiCl 3 Determination of

[0043] Accurately measure 10ml dimethyldichlorosilane sample and 10ul internal standard octane, mix well, inject 0.2ul sample into chromatogram, use internal standard method for C 2 h 5 HSiCl 2 Quantify.

[0044] Chromatographic conditions: Chromatographic conditions: column temperature: initial temperature 40°C, hold for 6 minutes, first-order rate 10°C / min, end temperature 200°C, hold for 10 minutes; vaporization temperature: 200°C; detection temperature: 300°C; carrier gas flow ( High-purity nitrogen): 1.5ml / min; hydrogen flow rate: 30 ml / min; air flow rate: 350 ml / min; split ratio: 100:1; injection volume 0.4μl; capillary column: trifluoropropyl-methyl poly Silicone capillary column 30m*0.53mm*1μm.

[0045] The measured CH 3 SiCl 3 , octane area and the average correction factor RFi=12.4 obtained in embodiment 1, substitute following formula to calculate CH 3 SiCl 3 Content Wi, ug / g:

[0046]

[...

Embodiment 3

[0055] CH in dimethyldichlorosilane 3 SiCl 3 Determination of

[0056] Chromatographic conditions: Chromatographic conditions: column temperature: initial temperature 40°C, hold for 6 min, first order rate 10°C / min, end temperature 200°C, hold for 10 min; vaporization temperature: 100°C; detection temperature: 200°C; carrier gas flow ( High-purity nitrogen): 0.5ml / min; hydrogen flow rate: 20 ml / min; air flow rate: 100 ml / min; split ratio: 100:1; injection volume 0.1μl; capillary column: trifluoropropyl-methyl poly The siloxane capillary column is 30m*0.53mm*1μm, and the internal standard is C5, and the rest are the same as in Example 1.

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Abstract

The invention discloses a method for determining methyltrichlorosilane in dimethyl dichlorosilane. A hydrogen flame ionization detector is used for carrying out quantitative determination of content of methyltrichlorosilane in a sample, vaporization temperature is controlled at 100-230 DEG C, detection temperature is 200-300 DEG C, flow rate of carrier gas is 0.5-10ml / min, flow rate of hydrogen is20-40ml / min, air velocity is 100-500ml / min, and sample size is 0.1-0.6<mu>l; a capillary column employs a trifluoropropyl-polymethylhydrosiloxane capillary column, an internal standard substance C5-C12 is used. The method has the advantages of simple sample treatment, high sensitivity, high resolution, high accuracy and the like, and at same time, rapid feedback of data is carried out in order tosatisfy needs of production technology.

Description

technical field [0001] The invention relates to a detection technology for the production of dimethyldichlorosilane, in particular to a gas chromatography detection method for methyltrichlorosilane in dimethyldichlorosilane. Background technique [0002] Dimethyldichlorosilane is the basic product of organosilicon synthesis and the main raw material for downstream products of organosilicon. In the relevant national standards of dimethyldichlorosilane, the main content analysis is emphasized, while its trace impurity component, methyltrichlorosilane , is an integral part of the T chain link, and plays a vital role in the quality of downstream hydrolyzate, 107 rubber, raw rubber, hydroxyl silicone oil and other products; and under the current national standard method conditions related to dimethyldichlorosilane, Methyltrichlorosilane is quantified by the area normalization method of a thermal conductivity detector, and the sensitivity and accuracy cannot meet the inspection re...

Claims

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Application Information

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IPC IPC(8): G01N30/68
CPCG01N30/68
Inventor 吴红李莉
Owner JIANGXI BLUESTAR XINGHUO SILICONE CO LTD
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