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Separation detection method of phenol compounds in textiles

A technology of phenolic compounds and detection methods, which is applied in the field of separation and detection of phenolic compounds in textiles, can solve the problems of time-consuming, inability to detect chlorophenol and o-phenylphenol at the same time, large amount of organic solvents, etc. Less dosage, overcoming time-consuming and polluting environment, good reproducible effect

Active Publication Date: 2017-05-10
GUANGZHOU FIBER PROD TESTING & RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These techniques have the disadvantages of not being able to detect various chlorophenols and o-phenylphenols at the same time, and they are time-consuming and use a large amount of organic solvents.

Method used

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  • Separation detection method of phenol compounds in textiles
  • Separation detection method of phenol compounds in textiles
  • Separation detection method of phenol compounds in textiles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 10g textile sample is joined in the extraction kettle (supercritical carbon dioxide extraction flow chart sees figure 1 ), add 500 μL acetic anhydride and 500 μL co-solvent-methanol, set the extraction temperature to 50 ° C, the pressure to 35 MPa, fill with 30 mL of supercritical CO 2 The textile samples were subjected to static extraction with supercritical carbon dioxide for 10 minutes; then dynamic extraction for 15 minutes at the same temperature and 2 The flow rate is 2.0mL / min; the discharge valve is opened, and the extracted target substance is dissolved in 15mL of n-hexane in a cooled separation collector, and 3mL of potassium carbonate solution with a mass fraction of 1% is added to the extract, shaken for 1min, and n-hexane The alkane phase was dehydrated with 1 g of anhydrous sodium sulfate to obtain the sample solution to be tested; the sample solution to be tested was analyzed qualitatively and quantitatively by gas chromatography-mass spectrometry (GC-MS)...

Embodiment 2

[0042] Add 10g of textile samples into the extraction kettle, add 500μL of acetic anhydride and 500μL of co-solvent-dichloromethane, set the extraction temperature to 50°C, the pressure to 40MPa, and fill with 30mL of supercritical CO 2 The textile samples were subjected to static extraction with supercritical carbon dioxide for 5 minutes; then dynamic extraction at the same temperature and pressure for 20 minutes, supercritical CO 2 The flow rate is 1.2mL / min; open the discharge valve, and the extracted target substance is dissolved in 15mL of toluene in a cooled separation collector, and 3mL of potassium carbonate solution with a mass fraction of 1% is added to the extract, shaken for 1min, and the toluene phase After dehydration with 1g of anhydrous sodium sulfate, the sample solution to be tested was obtained; the sample solution to be tested was analyzed qualitatively and quantitatively by GC-MS or GC-FID. The test conditions of GC-MS and GC-FID are the same as in Example...

Embodiment 3

[0044] Add 10g of textile samples into the extraction kettle, add 500 μL of acetic anhydride and 500 μL of co-solvent-acetone, set the extraction temperature to 70°C, the pressure to 30MPa, and the flow rate of supercritical carbon dioxide to 8.0mL / min, the textile samples are subjected to super Dynamic extraction with critical carbon dioxide for 30 min; add 15 mL of ethyl acetate to the collection device, open the discharge valve, collect the precipitate, add 3 mL of potassium carbonate solution with a mass fraction of 1% to the extract solution, shake for 1 min, and ethyl acetate phase 1g of anhydrous sodium sulfate was dehydrated to obtain the sample solution to be tested; the sample solution to be tested was analyzed qualitatively and quantitatively by GC-MS or GC-FID. The test conditions of GC-MS and GC-FID are the same as in Example 1.

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Abstract

The invention relates to a separation detection method of phenol compounds in textiles. The separation detection method includes following steps: taking and adding a to-be-detected textile sample into an extraction kettle, adding a derivatization reagent or adding a derivatization reagent and a cosolvent, performing supercritical carbon dioxide extraction at temperature of 40-90 DEG C and pressure of 15-45MPa on the to-be-detected textile sample, and collecting to obtain an extract; using an organic solvent to dissolve the extract to obtain an extract solution, adding a potassium carbonate solution, shaking, and using a drying agent to dry an organic phase to obtain a to-be-detected sample solution; detecting the phenol compounds in the to-be-detected sample solution. The separation detection method is low in solvent consumption during pretreatment and environment-friendly, has the advantages of quickness, high repeatability and simple operation, can detect various chlorine-containing phenol and o-phenylphenol at the same time and is high in recycling rate of the phenol compounds.

Description

technical field [0001] The invention relates to the fields of textiles and analysis and detection, in particular to a separation and detection method for phenolic compounds in textiles. Background technique [0002] The phenolic compounds that may be contained in textiles mainly include chlorinated phenolic compounds (pentachlorophenol (PCP), tetrachlorophenol (TeCP), trichlorophenol (TrCP), dichlorophenol (DCP), monochlorophenol (MCP) ) and o-phenylphenol (OPP), etc., these compounds are commonly used as fungicides and preservatives. These compounds all have certain biological toxicity effects, which can affect the environment and human health. Therefore, their residues in textiles and leather have attracted much attention. With the continuous deepening of research on toxicity and toxicology, relevant laws, regulations and standards have strict restrictions on its residue limits in textiles. Germany's limit requirements for TeCP and PCP: 0.05mg / kg for products in direct c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 莫月香罗峻廖芸胡剑灿杨昊明杨欣卉黎仲明
Owner GUANGZHOU FIBER PROD TESTING & RES INST
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