Method for determination of short-chain chlorinated paraffins in plastic, rubber and textile materials

A technology for short-chain chlorinated paraffins and textiles, applied in the field of analytical chemistry, to achieve the effect of removing impurity interference, high sensitivity and strong selectivity

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

[0006] The technical problem to be solved by this invention is to provide a method that can accurately measure short-chain chl

Method used

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  • Method for determination of short-chain chlorinated paraffins in plastic, rubber and textile materials
  • Method for determination of short-chain chlorinated paraffins in plastic, rubber and textile materials
  • Method for determination of short-chain chlorinated paraffins in plastic, rubber and textile materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] plastic sample

[0034] 1. Extraction of samples

[0035] After the plastic sample is cut into pieces, accurately weigh 1.0 into a 50mL sample bottle, accurately add 40mL of acetone:n-hexane (1:1) solution, sonicate in an ultrasonic instrument for 40min, filter into a concentration bottle, and concentrate to 3mL with a rotary evaporator , Prepare for purification.

[0036] 2. Purification of samples:

[0037] Add 4 mL of concentrated sulfuric acid to the concentrated sample solution, vortex and mix for 1 minute, separate with a centrifuge, and take the upper organic phase for analysis.

[0038] 3. Instrument measurement:

[0039] 3.1 Gas chromatography-electron capture detector test conditions:

[0040] Chromatographic column: HP-5MS capillary column, 30m×0.25mm×0.25μm

[0041] Carrier gas: nitrogen

[0042] Flow rate: 1.0mL / min

[0043] Injection volume: 1μL

[0044] Injection port temperature: 280°C

[0045] Programmed temperature rise: 100°C for 2 minutes, 2...

Embodiment 2

[0067] Addition experiment of known concentration of plastic, rubber, textile samples

[0068] Weigh 10 parts each of 1 g uniformly mixed plastic, rubber and leather samples, add a certain amount of SCCP standard solution (55.5% Cl), and analyze according to the pretreatment steps and ECD instrument conditions in the above-mentioned Example 1. According to the actual amount added and the measured results, the recovery rate and relative standard deviation of the samples were calculated. The calculation results are shown in Table 1 below:

[0069]

Embodiment 3

[0071] Qualitative Analysis of Rubber Samples on NCI Mass Spectrometer Detector

[0072] Take by weighing the rubber sample 1g that mixes homogeneously, carry out the processing of sample by the pretreatment step in embodiment 1, test by gas chromatography-NCI mass spectrometry detector test condition, gained chromatogram and mass spectrogram are shown in Figure 4-Figure 8 .

[0073] Depend on Figure 8 See, both SCCPs and MCCPs are present in this sample.

[0074] As can be seen from the above examples, the method of the present invention can effectively measure the content of short-chain chlorinated paraffins in plastics, rubber and textile materials.

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PUM

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Abstract

The invention belongs to the field of analytical chemistry, and specifically relates to a method for determining short-chain chlorinated paraffins in plastics, rubber, and textile materials. (2) purification by sulfonation with concentrated sulfuric acid; and (3) detection step (2) using gas chromatography-electron capture detector or gas chromatography-negative chemical ionization (NCI) mass spectrometry detector The content of short-chain chlorinated paraffins in the obtained purified samples. Beneficial effects of the present invention: Utilize concentrated sulfuric acid sulfonation purification method, can effectively remove interference, use gas chromatography-electron capture detector and NCI mass spectrometry detector to detect medium and short-chain chlorinated paraffins in plastics, rubber, textile materials, can realize Accurate quantification; according to the specific mass spectrum of short-chain chlorinated paraffins, the interference of medium and long-chain chlorinated paraffins can be effectively eliminated, making the qualitative more accurate, the selectivity stronger, and the sensitivity higher.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, in particular to a method for determining short-chain chlorinated paraffins in plastics, rubber and textile materials. Background technique [0002] Short-chain chlorinated paraffins (SCCPs) are a class of organic compounds with persistence, bioaccumulation, toxicity and long-distance migration, which are harmful to the environment and human health. Short-chain chlorinated paraffins are the most widely used in cables, and are also commonly used in the manufacture of water pipes, floors, films, artificial leather, plastic products and daily necessities. 65-70% short-chain chlorinated paraffins are mainly used as flame retardants, mixed with antimony trioxide and used in polyethylene, polystyrene, etc. In addition, short-chain chlorinated paraffins are also used as flame retardants for textiles, rubber and plastics, leather treatment agents, plasticizers for paints and other coatings, and metal...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/14
Inventor 王培花刘平年俞安敏冯颖陈志强
Owner SGS STANDARD TECHNICAL SERVICES SHANGHAI CO LTD
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