Method for Determination of Tris(2-Chloroethyl) Phosphate Content

A method of determination, phosphate technology, applied in the field of analytical chemistry, can solve the problems of easy decomposition, not very suitable for the detection of tris (2-chloroethyl) phosphate, difficult to volatilize, etc., achieve high sensitivity, convenient and fast sample pretreatment , strong selective effect

Inactive Publication Date: 2011-12-21
SGS STANDARD TECHNICAL SERVICES SHANGHAI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the commonly used method for the determination of tris (2-chloroethyl) phosphate is mainly gas chromatography-mass spectrometry, and tris (2-chloroethyl) phosphate has a boiling

Method used

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  • Method for Determination of Tris(2-Chloroethyl) Phosphate Content
  • Method for Determination of Tris(2-Chloroethyl) Phosphate Content
  • Method for Determination of Tris(2-Chloroethyl) Phosphate Content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 was carried out as follows.

[0026] 1. Sample Preparation

[0027] Get the blank plastic material that does not contain three (2-chloroethyl) phosphates, mix it with different amounts of three (2-chloroethyl) phosphates, prepare the content of three (2-chloroethyl) phosphates 4mg / kg, 20mg / kg, 80mg / kg, 200mg / kg samples.

[0028] 2. Organic solvent extraction and filtration

[0029] After the sample is cut into pieces, accurately weigh 1.0g into a 50mL sample bottle, accurately add 20mL of acetonitrile, sonicate in an ultrasonic water bath (45°C) for 60min, filter through a 0.22μm filter membrane, and take an appropriate amount into a sample bottle for analysis on the machine .

[0030] 3. Instrument measurement:

[0031] The measurement conditions are as follows:

[0032] Chromatographic column: Agilent Plus C18, 2.1×100mm×3.5μm

[0033] Mobile Phase: A: Acetonitrile

[0034] B: 0.01mol / L ammonium acetate buffer solution

[0035] Mobile phase gradient:...

Embodiment 2

[0054] Carry out with reference to embodiment 1, difference is that sample is variegated decorative cloth, and sample weight is 0.5g, and used organic solvent is acetonitrile, and add-on is 10mL, and the content of three (2-chloroethyl) phosphates in sample is 20mg / kg, 80mg / kg, 200mg / kg. The test results are shown in Table 2.

[0055] The recovery rate of standard addition of table 2 sample

[0056]

Embodiment 3

[0058] Carried out with reference to Example 1, the difference is that the sample is leather, the sample weight is 0.5g, the organic solvent used is acetonitrile, and the addition is 10mL, and the content of tris (2-chloroethyl) phosphate in the sample is 20mg / kg , 80mg / kg, 200mg / kg. The test results are shown in Table 3.

[0059] The recovery rate of standard addition of table 3 sample

[0060]

[0061] As can be seen from the above examples, the method of the present invention can accurately and effectively measure the content of tris (2-chloroethyl) phosphate in plastic products, textiles and leather products.

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Abstract

The invention belongs to the field of analytical chemistry, and in particular relates to a method for determining the content of tris (2-chloroethyl) phosphate, which is characterized in that it comprises the following steps in sequence: (1) extracting with an organic solvent; (2) extracting from step (1) The obtained extraction solution is filtered; (3) the filtered extraction solution is determined by a high performance liquid chromatography-mass spectrometer detector. The invention has the beneficial effects of detecting tris(2-chloroethyl)phosphate with a high-performance liquid chromatography-mass spectrometer, strong anti-interference ability, convenient and fast sample pretreatment, accurate qualitative and quantitative, and avoiding the target The decomposition of compounds has stronger selectivity and higher sensitivity.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, in particular to a method for determining the content of tris (2-chloroethyl) phosphate. Background technique [0002] Tris(2-chloroethyl)phosphate (TCEP) is an additive flame retardant widely used in acetate, nitrocellulose, ethylcellulose, polyvinyl chloride, polyurethane, polyvinyl acetate and phenolic resins etc. It can also be used as metal extractant, lubricating oil and gasoline additive, and polyimide processing modifier. [0003] Canada ruled in 2009 that tris(2-chloroethyl)-phosphate is a carcinogen, may pose a threat to human life or health, and may cause male infertility. Health Canada believes that children under the age of three are exposed to three ( 2-Chloroethyl) phosphate, which pose the highest risk of adverse health effects. Therefore, in September 2010, Health Canada proposed to add products that are wholly or partly made of polyurethane latex containing tris(2-chloroet...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/14
Inventor 王培花刘平年蔡细香林家豪冯颖
Owner SGS STANDARD TECHNICAL SERVICES SHANGHAI CO LTD
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