Method for determining content of tris (2-chloroethyl) phosphate

A method of determination, phosphate ester technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of gas phase uncertainty, LC/DAD/MS, etc., and achieve the effect of convenient method, reliable method and reliable implementation

Inactive Publication Date: 2010-07-14
谱尼测试集团股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of this invention is to provide a kind of assay method to three (2-chloroethyl) phosphoric acid ester content by gas chromatography mass spectrometry, to overcome prior art gas phase can not qualitative, and LC / DAD / MS application is less insufficient

Method used

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  • Method for determining content of tris (2-chloroethyl) phosphate
  • Method for determining content of tris (2-chloroethyl) phosphate
  • Method for determining content of tris (2-chloroethyl) phosphate

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Experimental program
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Embodiment 1

[0056] The drawing of embodiment 1 standard curve

[0057] Accurately weigh three (2-chloroethyl) phosphate standard substance (purity 97.0% Bailingwei 12.89mg, acetone-methanol (volume ratio 1: 1) dissolves and settles to 25.0mL, concentration 500mg / L is used as stock solution, uses Acetone-methanol (volume ratio 1:1) was diluted 50 times to a concentration of 10 mg / L, and then diluted to 0.20, 0.50, 1.00, 2.00, 5.00 mg / L standard solutions.

[0058] Use gas chromatography-mass spectrometry to detect the above-mentioned standard liquid for use, take the quantitative ion (M / Z 249) chromatographic peak area as the ordinate, and draw the standard curve with the concentration of the standard liquid for abscissa. The linear equation of the standard curve is Y=463.34X+838.90, and the correlation coefficient is R2=0.9996.

Embodiment 2

[0059] The detection of three (2-chloroethyl) phosphate content in the embodiment 2PVC plastics

[0060] Preparation of sample test solution: Take 1.0 g of pulverized PVC plastic solid (accurately weighed to 0.0001 g), put it in an ultrasonic extractor, add 40 mL of acetone-methanol (volume ratio 1:3), and ultrasonicate for 60 min at 60°C; Take out and cool to room temperature, transfer the extraction solution into a 250 mL pear-shaped bottle and wash the container with acetone-methanol (volume ratio 1:3). Concentrate on a rotary evaporator to 1 mL of the test solution, pass it through a Waters Oasis HLB extraction column (specification: 500 mg / 6 ml), rinse with 15 mL of acetone-methanol (volume ratio 1:3), and collect the eluent. Rotary evaporate the solution Make the volume up to 1ml, dilute to 2mL with acetone-methanol (volume ratio 1:3), filter with a 0.45μm organic phase filter membrane, and use it as the sample test solution.

[0061] Repeat the preparation process of t...

Embodiment 3

[0065] The mensuration of three (2-chloroethyl) phosphoric acid ester content in the silicone rubber of embodiment 3 is because parameters such as used solvent, temperature and time have expanded the range of values ​​in specification and claims, therefore embodiment 3 and 4 The corresponding values ​​in have been adjusted to support the claimed range.

[0066] Prepare sample test solution: take 1.0 g of crushed neoprene solid sample (accurately weighed to 0.0001 g), place it in an ultrasonic extractor, add 60 mL of acetone-methanol (volume ratio 1:1), and reflux at 50 ° C; Take out and cool to room temperature, transfer the extraction solution into a 250 mL pear-shaped bottle and wash the container with acetone-methanol (volume ratio 1:3). Concentrate on a rotary evaporator to 1 mL of the test solution, pass it through a Waters Oasis HLB extraction column (specification: 500 mg / 6 ml), rinse with 10 mL of acetone-methanol (volume ratio 1:3), and collect the eluate. The volume...

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Abstract

The invention provides a method for determining the content of tris (2-chloroethyl) phosphate, which comprises the following steps: a sample to be tested is extracted with an organic solvent extractant, the obtained extract is purified via a Waters Oasis HLB extraction column after being concentrated, is concentrated to a definite volume after leacheate which is the organic solvent is collected, and finally is filtered to prepare a specimen test solution; and then the specimen test solution is detected with a gas chromatograph-mass spectrometer according to an external standard method. When the sample to be tested is a solid sample, the sample to be tested is pulverized firstly and then is extracted by ultrasound; and when the sample to be tested is liquid, the sample is extracted by ultrasound. The method for determining the content of the tris (2-chloroethyl) phosphate is rapid and effective, the error rate of is not more than 5 percent, and the detection limit is 0.05mg / kg. The invention provides a reliable and conveniently implementary method for detecting the content of tris (2-chloroethyl) phosphate in rubber, plastics, printing ink and paint products and can meet the needs in research and production.

Description

technical field [0001] The invention relates to a method for determining the content of tris (2-chloroethyl) phosphate, in particular to a method for determining the content of tris (2-chloroethyl) phosphate in rubber and plastic products, more specifically The invention relates to a method for determining the content of tris (2-chloroethyl) phosphate in rubber and plastics by means of a gas chromatography mass spectrometer. Background technique [0002] Tris (2-chloroethyl) phosphate, the English name is Tris (2-chloroethyl) phosphate. It is mainly used as a flame retardant for cellulose acetate, nitrocellulose, ethyl cellulose, polyurethane, polyvinyl acetate and phenolic resins. It can also be used as a plasticizer. Tris-(2-chloroethyl)phosphate {Tris-(2-chloroethyl)phosphate, TCEP} has been identified as a Group 3 carcinogen by the International Agency for Research on Cancer (IARC). ). As organophosphorus flame retardants are so widely used in daily life, tri-(2-chlo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/02
Inventor 宋薇
Owner 谱尼测试集团股份有限公司
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