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Method for measuring short chain chlorinated paraffin in high polymer material

A technology of short-chain chlorinated paraffins and polymer materials, which is applied in the direction of analysis materials, material separation, and measuring devices. It can solve the problems of interference with short-chain chlorinated paraffins analysis and incomplete separation, so as to avoid interference and improve extraction rate. Effect

Inactive Publication Date: 2015-04-22
通标标准技术服务(天津)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are many analytical methods for short-chain chlorinated paraffins, such as high-resolution gas chromatography and high / low-resolution mass spectrometry, comprehensive two-dimensional gas chromatography-fast scanning quadrupole mass spectrometry, high performance liquid chromatography-chlorine enhanced atmospheric pressure chemistry Ionization ion trap mass spectrometry, but because the short-chain chlorinated paraffins in the polymer materials only account for a small part, and the main components of the polymer materials are polyethylene, polyvinyl chloride and other additives such as stabilizers, lubricants, etc. due to pre-treatment separation Incomplete, it will interfere with the analysis of short-chain chlorinated paraffins in the later detection process

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  • Method for measuring short chain chlorinated paraffin in high polymer material

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Embodiment 1

[0022] The invention provides a method for measuring short-chain chlorinated paraffins in polymer materials, comprising:

[0023] Step 1. Dedusting the plastic to be tested, soaking the plastic to be tested in clean water for 20 minutes, and brushing off the dust and dirt on the surface of the plastic to be tested.

[0024] Step 2: Cut the plastic to be tested after dust removal into an area of ​​0.2cm 2 Weigh 2g of small pieces and place them in a round bottom flask, heat to 150°C to be in a molten state; pour the molten plastic to be tested into the first reaction container, add 20mL of cyclohexanone, and put the first reaction The container was placed on a shaker and vibrated for 10 min, and the first extract was passed through the filter paper equipped with anhydrous sodium sulfate, then extracted once with 10 mL of cyclohexanone and filtered into the second reaction container; in the second reaction container Add 10mL of ethyl acetate and pentyl acetate mixed solution wi...

Embodiment 2

[0030] The invention provides a method for measuring short-chain chlorinated paraffins in polymer materials, comprising:

[0031] Step 1. Dedusting the rubber to be tested, soaking the rubber to be tested in clear water for 40 minutes, and brushing off the dust and dirt on the surface of the rubber to be tested.

[0032] Step 2: Cut the rubber to be tested after dust removal into an area of ​​0.5cm 2Weigh 3g of small pieces and place them in a round bottom flask, and heat them to 180°C to be in a molten state; pour the molten rubber to be tested into the first reaction container, add 30mL of cyclohexanone, and put the first reaction The container was placed on a shaker to vibrate for 15min, and after the first extract was passed through the filter paper equipped with anhydrous sodium sulfate, it was extracted once with 15mL of cyclohexanone and filtered into the second reaction vessel; in the second reaction vessel Add 15mL of a mixture of ethyl acetate and amyl acetate with ...

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Abstract

The present invention relates to the field of measurement of short chain chlorinated paraffin and particularly relates to a method for measuring short chain chlorinated paraffin in a high polymer material. The method comprises the following steps: dedusting the high polymer material; shearing the dedusted high polymer material into pieces, putting the pieces in a round-bottom flask, and heating the pieces to a molten state; pouring the molten high polymer material into a first reaction container, adding cyclohexanone in twice, oscillating and filtering; adding mixed liquor of ethyl acetate and amyl acetate into a second reactor, oscillating and filtering; adding mixed liquor of acetone / normal hexane / dichloromethane with a volume ratio of 1:2:1, and oscillating and concentrating the mixed liquor in an ultrasonic oscillator; spraying the concentrated solution onto a chromatographic column, leaching and receiving eluant; feeding the eluant into a chromatographic column from the sample feed opening of a metastable atom bombardment high-resolution mass spectrometer to realize mass spectrometric detection. According to the invention, the main components and the added components in the high polymer material are fully separated to improve the detection efficiency and accuracy of the short chain chlorinated paraffin.

Description

technical field [0001] The invention relates to the field of determination of short-chain chlorinated paraffins, in particular to a method for determining short-chain chlorinated paraffins in polymer materials. Background technique [0002] Chlorinated paraffin is a polychlorinated long-chain normal alkanes, the chain length can vary from C10 to C30, and the chlorine content is between 30wt% and 70wt%. According to the different chain lengths, chlorinated paraffins can be divided into short-chain (C10-C13), medium-chain (C14-C17) and long-chain (C18-C30) chlorinated paraffins. Short-chain chlorinated paraffins, also known as short-chain chlorinated normal alkanes, are also called chlorinated alkanes, chlorinated alkanes, and chlorinated paraffins. Short-chain chlorinated paraffins are n-paraffins with a carbon chain length of 10 to 13 carbon atoms. The degree of chlorination is about 16% to 78% by weight, and its molecular formula is CxH(2x-y+2)Cly, wherein, x=10-13, y=1-1...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 刘潇
Owner 通标标准技术服务(天津)有限公司
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