Method for detecting content of short-chain or medium-chain chlorinated paraffin in paint

A technology of chlorinated paraffin and determination method, which is applied in the direction of measuring device, material separation, analysis material, etc., and can solve the problems of instrument analysis interference and error

Active Publication Date: 2014-01-29
GUANGDONG TESTING INST OF PROD QUALITY SUPERVISION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The difficulty of the CPs analysis method is mainly manifested in the following: Some components of SCCP and MCCP have the same molecular weight and the same characteristic ions, and interfere with each other. When using low-resolution mass spectrometry, it is easy to cause errors
In addition, many chlorinated organic compounds (especially chlorinated aromatics, such as toxaphene, some PCB monomers, mirex, etc.) have the same characteristic ions as some components of CPs, which will interfere with instrument analysis
[0006] In the existing detection method, the same response factor is used for CPs with different chlorine contents, and the CPs detected by this method are not their real values, but only measured values, which need to be corrected

Method used

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  • Method for detecting content of short-chain or medium-chain chlorinated paraffin in paint
  • Method for detecting content of short-chain or medium-chain chlorinated paraffin in paint
  • Method for detecting content of short-chain or medium-chain chlorinated paraffin in paint

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Experimental program
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Effect test

Embodiment 1

[0037] The method for testing short-chain chlorinated paraffins in coatings is as follows:

[0038] (1) Select the paint and extract the short-chain chlorinated paraffin in the paint with the organic solvent dichloromethane. The mass-volume ratio of the paint mass to the organic solvent is 2g: 500mL. The extraction method is Soxhlet extraction, and the extract is concentrated. To obtain a concentrated solution, pass the concentrated solution through a glass chromatography column filled with 8g of florisil, 2g of neutral silica gel, 8g of acidic silica gel and 1g of anhydrous sodium sulfate from bottom to top, and then wash with about 1mL of n-hexane , repeated three times, rinsed with 50mL of n-hexane, and discarded; then rinsed with 60mL of dichloromethane, and collected the purified chlorinated paraffin fraction;

[0039](2) Using cyclohexane as a solvent, prepare a series of standard solutions of short-chain chlorinated paraffins with different chlorine contents. The chlori...

Embodiment 2

[0058] The method for testing medium-chain chlorinated paraffins in coatings is as follows:

[0059] (1) Select the paint, and use the organic solvent n-hexane to extract the medium-chain chlorinated paraffin in the paint. The mass-volume ratio of the paint mass to the organic solvent is 5g:500mL. The extraction method is Soxhlet extraction, and the extract is concentrated to obtain Concentrate, pass the concentrate through a glass chromatography column filled with 11g of florisil, 2g of neutral silica gel, 10g of acid silica gel and 1.5g of anhydrous sodium sulfate from bottom to top, and then wash with about 1mL of n-hexane , repeated three times, rinsed with 80mL of n-hexane, and discarded; then rinsed with 80mL of dichloromethane, and collected the purified chlorinated paraffin fraction;

[0060] (2) Using cyclohexane as a solvent, prepare a series of standard solutions of medium-chain chlorinated paraffins with different chlorine contents. Internal standard ε-HCH hexachl...

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Abstract

The invention discloses a method for detecting content of short-chain or medium-chain chlorinated paraffin in a paint. The method comprises the following steps: extracting the short-chain or medium-chain chlorinated paraffin in the paint, detecting with a gas chromatography-negative chemical ionization source mass spectrometry detector, using the internal standard method, performing linear association on a total response factor of a short-chain or medium-chain chlorinated paraffin standard sample on the NCI (negative chemical ionization) mass spectrometry detector with the chlorine content of a short-chain or medium-chain chlorinated paraffin standard solution, detecting the actually measured chlorine content of the sample by the gas chromatography-negative chemical ionization source mass spectrometry detector, corresponding the actually measured chlorine content with the a liner reaction expression of the total response factor and the chlorine content of the short-chain or medium-chain, to obtain the total response factor of the sample, and thus obtaining the content of the short-chain or medium-chain chlorinated paraffin in the paint. The analysis method disclosed by the invention is exact and fast, has small interfering, and can perform optimal separation and qualitative and quantitative detections on each component in the sample.

Description

technical field [0001] The invention belongs to the technical field of detection methods for chlorinated paraffins, in particular to a method for determining the content of short-chain or medium-chain chlorinated paraffins in coatings. Background technique [0002] Chlorinated paraffins (Chlorinated paraffin, CPs), the general chemical formula is C n h 2n+2-x Cl x , is a mixture of various halogenated alkanes. According to the different carbon chain lengths, CPs can be divided into short chains (C 10 -C 13 , SCCPs), medium chain (C 14 -C 17 , MCCPs) and long-chain chlorinated paraffins (C 18 -C 30 , LCCPs), schematic diagrams of short-chain and medium-chain chemical structures. [0003] Existing experience and model data fully show that short-chain chlorinated paraffins have strong persistence, bioaccumulation and toxicity, especially for aquatic organisms, and have the ability of long-range environmental migration. [0004] Chlorinated paraffin is a straight-chain...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 陈纪文陈满英梁德沛路风辉
Owner GUANGDONG TESTING INST OF PROD QUALITY SUPERVISION
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