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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 liquid chromatography-mass spectrometry, low separation ability of liquid chromatography column, interference in testing process and the like, and achieves low cost. , The method is accurate and reliable, the effect is obvious

Inactive Publication Date: 2010-02-17
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 shredded (about 2mm×2mm) leather sample, mix with about 2g of anhydrous sodium sulfate, add to a 100mL conical flask with a stopper, accurately add 50mL of chromatographically pure acetonitrile; Ultrasonic (40 Hz) extraction was performed for 60 min at ~45°C, and then the extract in the Erlenmeyer flask was vacuum filtered through a 0.45 μm filter membrane, and the filtrate was cooled to room temperature.

[0025] (2) Chemical treatment of extract

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

[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 water, and cool ...

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 the shredded (about 2mm×2mm) synthetic leather sample, mix it with 1g~2g of anhydrous sodium sulfate, add it to a 100mL conical flask with a stopper, and accurately add 50mL of chromatographically pure acetonitrile; Ultrasonic (40 Hz) extraction was carried out at 40°C to 45°C for 60 minutes, and then the extract in the conical flask was vacuum filtered through a 0.45 μm filter membrane, and the filtrate was cooled to room temperature.

[0036] (2) Chemical treatment of extract

[0037] Accurately pipette 10 mL of the filtrate into a 50 mL flat-bottomed flask, then add 3 g of cleavage agent, and reflux at a temperature of 81°C to 85°C for 50 minutes.

[0038] (3) purification

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

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 chromatographically pure acetonitrile; Ultrasonic (40Hz) extraction was carried out for 60min at ℃~45℃. After the filtrate was cooled to room temperature, it was centrifuged at 4000r / min for 5min, and then the extract in the Erlenmeyer flask was vacuum filtered through a 0.45μm filter membrane.

[0047] (2) Chemical treatment of extract

[0048] Accurately pipette 10 mL of the filtrate into a 50 mL flat-bottomed flask, then add 3 g of cleavage agent, and reflux at a temperature of 81°C to 85°C for 50 minutes.

[0049] (3) purification

[0050] Take out the flask, carefully drop about 10 drops of distilled water into the flask, then add abou...

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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, in particular to a gas chromatography-mass spectrometry detection method for nonylphenol polyoxyethylene ether (abbreviated as NPEO), especially for nonylphenol polyoxyethylene ether in leather, synthetic leather, paper and textiles Concentration detection. 【Background technique】 [0002] Nonylphenol polyoxyethylene ether is a kind of non-ionic surfactant with excellent performance, which is widely used in the processing of textile, leather, paper and synthetic leather. Part of nonylphenol polyoxyethylene ether will remain in leather, textiles, etc. , paper and synthetic leather. Since nonylphenol, the final degradation product of nonylphenol polyoxyethylene ether, has strong physiological toxicity, it has been identified as a harmful substance in textiles, leather, paper and synthetic leather by the EU Directive 2003 / 53 / EC, and its residues Quantity is limited. Therefore, the detection...

Claims

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Application Information

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Patent Type & Authority Applications(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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