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Gas phase chromatograph-mass spectrum detection method for nonylphenol polyoxyethylene ether in leather, synthetic leather, paper and textile

A technology of nonylphenol polyoxyethylene ether and gas chromatography, which is applied in the field of detection and analysis, can solve the problems of high price of liquid chromatography-mass spectrometry, weak separation ability of liquid chromatography column, and interference in the test process, and achieve low cost , the method is accurate and reliable, and the effect is obvious

Inactive Publication Date: 2012-06-27
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

However, the price of liquid chromatography-mass spectrometry is expensive, and the test cost is high, so it is difficult to popularize; at the same time, textiles, leather, paper and synthetic leather contain more fillers (such as oils, dyes, resins), due to the conventional liquid chromatography The separation ability of the chromatographic column is not strong, which leads to serious interference in the test process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: Gas chromatography-mass spectrometry detection of nonylphenol polyoxyethylene ether content in leather

[0023] (1) Solvent extraction

[0024] Accurately weigh 2g of leather sample cut (about 2mm×2mm), mix with about 2g of anhydrous sodium sulfate, add it to a 100mL conical flask with stopper, and accurately add 50mL of chromatographic pure acetonitrile; after stoppering, the temperature is 40℃ Perform ultrasonic (40 Hz) extraction at ~45°C for 60 minutes, then pass the extract in the Erlenmeyer flask through a 0.45 μm filter membrane for vacuum filtration, and cool the filtrate to room temperature.

[0025] (2) Chemical treatment of extract

[0026] Accurately pipet 10 mL of the filtrate, add it to a 50 mL flat-bottomed flask, and then add 3 g of lysing agent, and reflux for 50 min at a temperature of 81°C to 85°C.

[0027] (3) Purification

[0028] Take out the flask, first carefully add 5-10 drops of distilled water to the flask, then add about 5mL of distilled wat...

Embodiment 2

[0033] Example 2: Gas chromatography-mass spectrometry detection of nonylphenol polyoxyethylene ether content in synthetic leather

[0034] (1) Solvent extraction

[0035] Accurately weigh 1g of synthetic leather sample cut (approximately 2mm×2mm), mix with 1g~2g of anhydrous sodium sulfate, add it to a 100mL conical flask with stopper, and accurately add 50mL of chromatographic pure acetonitrile; after stoppering, at temperature Perform ultrasonic (40 Hz) extraction for 60 minutes at 40°C to 45°C, then pass the extract in the Erlenmeyer flask through a 0.45 μm filter membrane for vacuum filtration, and cool the filtrate to room temperature.

[0036] (2) Chemical treatment of extract

[0037] Use a pipette to accurately transfer 10 mL of the filtrate, add it to a 50 mL flat-bottomed flask, and then add 3 g of lysing agent, and reflux for 50 min at a temperature of 81°C to 85°C.

[0038] (3) Purification

[0039] Take out the flask, first carefully add about 10 drops of distilled water i...

Embodiment 3

[0044] Example 3: Gas chromatography-mass spectrometry detection of nonylphenol polyoxyethylene ether content in paper

[0045] (1) Solvent extraction

[0046] Accurately weigh 1.0g of crushed paper scraps (or fibers), mix with 1g~2g of anhydrous sodium sulfate, add to a 100mL conical flask with a stopper, and then accurately add 50mL of chromatographic pure acetonitrile; after stoppering, at a temperature of 40 Perform ultrasonic (40Hz) extraction at ℃~45℃ for 60min. After the filtrate is cooled to room temperature, it is centrifuged at 4000r / min for 5min, and then the extract in the Erlenmeyer flask is vacuum filtered through a 0.45μm filter membrane.

[0047] (2) Chemical treatment of extract

[0048] Use a pipette to accurately transfer 10 mL of the filtrate, add it to a 50 mL flat-bottomed flask, and then add 3 g of lysing agent, and reflux for 50 min at a temperature of 81°C to 85°C.

[0049] (3) Purification

[0050] Take out the flask, carefully add about 10 drops of distilled w...

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Abstract

The invention discloses a gas phase chromatograph-mass spectrum detection method for nonylphenol polyoxyethylene ether in leather, synthetic leather, paper and textile, relating to the field of detecting and analyzing. The method comprises the following steps: extracting a solvent, chemically processing extractive liquid, purifying a solid phase extractive column, detecting through the chromatograph-mass spectrum and obtaining the concentration value of the nonylphenol polyoxyethylene ether through comparing with a standard curve. The invention has easy operation, environment protection, goodreproducibility and precise stability; the content of the nonylphenol polyoxyethylene ether in the leather, the synthetic leather, the paper and the textile can be rapidly analyzed without using an expensive liquid phase hromatograph-mass spectrometer. Compared with the prior test technology, the invention does not adopt the expensive liquid phase hromatograph-mass spectrometer in the process of detecting the nonylphenol polyoxyethylene ether so that the method is precise and reliable with low cost.

Description

【Technical Field】 [0001] The invention belongs to the field of detection and analysis, and particularly relates to a gas chromatography-mass spectrometry detection method for nonylphenol polyoxyethylene ether (NPEO in English), especially for nonylphenol polyoxyethylene ether in leather, synthetic leather, paper and textiles Concentration detection. 【Background technique】 [0002] Polyoxyethylene nonylphenol ether is a class of non-ionic surfactants with excellent performance. It is widely used in the processing of textiles, leather, paper and synthetic leather. Part of the polyoxyethylene nonylphenol ether will remain in leather and textiles. , Paper and synthetic leather. As the final degradation product of nonylphenol polyoxyethylene ether, nonylphenol, has strong physiological toxicity, it has been identified as a harmful substance in textiles, leather, paper and synthetic leather by EU Directive 2003 / 53 / EC, and its residues The amount is limited. Therefore, the detection ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72B01D11/02
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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