Method for detecting total amount of perfluorooctane sulphonates (PFOS) in textile and leather

A perfluorooctanesulfonyl and detection method technology, applied in the field of detection and analysis, to achieve high extraction efficiency, realize analysis and detection, and achieve obvious effects

Inactive Publication Date: 2011-11-23
国家皮革质量监督检验中心(浙江)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The only way to reflect the total amount of PFOS is to detect the total amount of perfluorooctanesulfonyl that can be decomposed in PFOS, or a specific substance that can quantitatively characterize perfluorooctanesulfonyl, but there is currently no relevant technical report

Method used

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  • Method for detecting total amount of perfluorooctane sulphonates (PFOS) in textile and leather
  • Method for detecting total amount of perfluorooctane sulphonates (PFOS) in textile and leather
  • Method for detecting total amount of perfluorooctane sulphonates (PFOS) in textile and leather

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1: Determination of the total amount of perfluorooctanesulfonyl substances in leather

[0028] (1) Solvent extraction

[0029] Accurately weigh about 1g of sample particles that are cut into pieces (about 4mm×4mm), add them to a 100ml conical flask with a stopper, add 30mL of methanol, and extract in an ultrasonic bath (40Hz) for 30min after stoppering; filter out the extract, and use 60mL of methanol was extracted twice, each time for 10min; the extracts were combined, and about 2g of anhydrous magnesium sulfate was added for dehydration, and then the volume was adjusted to 100.0mL.

[0030] (2) Chemical treatment of extract

[0031] Pipette 10.0 mL of the sample solution into a 150 mL flat-bottomed flask, concentrate to dryness by rotation, add 5 mL of chromatographic grade tetrahydrofuran, and concentrate by rotation to dryness again; then add 5 mL of a solution containing a cleavage reagent to the bottle, and reflux at 90°C for 60 minutes; Remove the flask...

Embodiment 2

[0042] Example 2: Determination of the total amount of perfluorooctanesulfonyl substances in textiles

[0043] (1) Solvent extraction

[0044] Accurately weigh about 1g of sample particles that are cut into pieces (about 4mm×4mm), add them to a 100ml conical flask with a stopper, add 30mL of methanol, and extract in an ultrasonic bath (40Hz) for 30min after stoppering; filter out the extract, and use 60mL of methanol was extracted twice, each time for 10min; the extracts were combined, and about 2g of anhydrous magnesium sulfate was added for dehydration, and then the volume was adjusted to 100.0mL.

[0045] (2) Chemical treatment of extract

[0046] Pipette 10.0 mL of the sample solution into a 150 mL flat-bottomed flask, concentrate to dryness by rotation, add 5 mL of chromatographic grade tetrahydrofuran, and concentrate by rotation to dryness again; then add 5 mL of a solution containing a cleavage reagent to the bottle, and reflux at 90°C for 60 minutes; Remove the flask,...

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Abstract

The invention discloses a method for detecting total amount of perfluorooctane sulphonates (PFOS) in textile and leather, which sequentially comprises the following steps: solvent extraction of a sample, chemical treatment of extract liquid, purification and liquid chromatogram-mass spectroscopy. According to the invention, as PFOS in the sample are extracted by methanol with assist of ultrasonic wave, the extraction efficiency is high, the effect is obvious, and the operation is simple; a specific chemical cracking treatment is adopted so that the PFOS is decomposed into equivalent octanesulfonic acid and the measurement of perfluorooctane sulfonyl content in PFOS is realized; filler is adopted to purify the chromatographic column of silica gel, and interference of impurities in the extract liquid (oil, dye) on the liquid chromatogram-mass spectroscopy process is effectively reduced; and compared with the prior test technology, the method disclosed by the invention realizes analytical detection on the total amount of PFOS in the sample.

Description

【Technical field】 [0001] The invention belongs to the field of detection and analysis, in particular to a liquid chromatography-mass spectrometry detection method for perfluorooctanesulfonyl substances (abbreviated as PFOS), especially for the detection of the concentration of perfluorooctanesulfonyl substances in textiles and leather detection. 【Background technique】 [0002] Perfluorooctanesulfonyl substances (PFOS) are a large class of fluorine-containing compounds with perfluorooctanesulfonyl as the main body. The general molecular formula is (C 8 -F 17 -SO 2 -X). PFOS is widely used as a raw material in the industrial production process of textiles and leather because of its oleophobic and hydrophobic properties. However, because PFOS is recognized as highly bioaccumulative and systemic multi-organ toxicity, it is clearly listed as a restricted substance in textile and leather processing by EU Directive 2006 / 122 / EC. Therefore, the detection of the content of perflu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 马贺伟黄新霞
Owner 国家皮革质量监督检验中心(浙江)
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