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Method for identifying polyamide 6 or polyamide 66 in blended textiles

An identification method, polyamide technology, applied in the field of analysis and detection, can solve the problems of poor reproducibility of test results, low sensitivity, small sampling volume, etc., and achieve the effect of being beneficial to the experimental environment and human health, with less dosage and high efficiency

Inactive Publication Date: 2017-08-22
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Pyrolysis gas chromatography uses solid samples for analysis, and the sampling volume should be small (microgram level). For blended products, a small amount of sampling may not be representative of the sample, resulting in poor reproducibility of test results
These methods have the disadvantages of low sensitivity and poor reliability in the qualitative identification of low-content polyamide 6 or polyamide 66 components in blended products

Method used

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  • Method for identifying polyamide 6 or polyamide 66 in blended textiles
  • Method for identifying polyamide 6 or polyamide 66 in blended textiles
  • Method for identifying polyamide 6 or polyamide 66 in blended textiles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] 1. Sample reagent

[0053] Polyamide 6 standard (chip), polyamide 66 standard (fiber), anhydrous formic acid (analytical grade).

[0054] 2. Analysis and determination

[0055] Weigh 10 mg polyamide 6 standard product or polyamide 66 standard product, dissolve them in 10 mL of anhydrous formic acid, soak for 20 min, take 2 μL into the sample cup, heat at 150 ° C to remove formic acid, and perform pyrolysis chromatography-mass spectrometry analysis to obtain polyamide The standard pyrolysis chromatogram of 6, see attached figure 1 ; The standard pyrolysis chromatogram of polyamide 66, see appendix figure 2 .

[0056] figure 1 The chromatographic peak with a retention time of 10.33 min is the characteristic cracked substance of the polyamide 6 fiber component, that is, caprolactam, and the relative peak area content is about 89%.

[0057] figure 2 The chromatographic peak with a retention time of 3.28 min is the characteristic cracked substance of the polyamide 66...

Embodiment 2

[0059] 1. Sample reagent

[0060] Polyamide 6 fiber and wool fiber blended sample (mass ratio 21.7:78.3), anhydrous formic acid (analytical pure).

[0061] 2. Analysis and determination

[0062] Weigh 11.53 mg of polyamide 6 fiber and wool fiber blended sample, extract with 10 mL of anhydrous formic acid, soak for 20 minutes, take 2 μL into the sample cup, heat at 155 ° C to remove formic acid, and perform pyrolysis chromatography-mass spectrometry analysis. see attached image 3 . The characteristic cracking peak at the retention time of 10.33min is caprolactam, and the relative peak area content is about 76%.

[0063] As a comparison, weigh 0.09 mg polyamide 6 fiber and wool fiber blended sample and add it to the sample cup for pyrolysis chromatography-mass spectrometry analysis. The pyrolysis chromatogram obtained is shown in the attached Figure 4 . The characteristic cracking peak at retention time 10.33min is caprolactam, and the relative peak area content is about ...

Embodiment 3

[0065] 1. Sample reagent

[0066] Polyamide 66 fiber and cotton fiber blended sample (mass ratio 39.3:60.7), anhydrous formic acid (analytical grade), first grade pure water.

[0067] 2. Analysis and determination

[0068] Weigh 9.50 mg of polyamide 66 fiber and cotton fiber blended sample, extract with 10 mL of 80% formic acid solution, soak for 30 minutes, take 2 μL into the sample cup, heat at 160 ° C to remove formic acid, and perform pyrolysis chromatography-mass spectrometry analysis. See attached chromatogram Figure 5 . The characteristic cracking peak at the retention time of 3.33min is cyclopentanone, and the relative peak area content is about 93%.

[0069] As a comparison, weigh 0.11 mg of polyamide 66 fiber and cotton fiber blended sample and add it to the sample cup for pyrolysis chromatography-mass spectrometry analysis. The pyrolysis chromatogram obtained is shown in the attached Figure 6 . The characteristic cracking peak at the retention time of 3.30 mi...

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Abstract

The invention relates to a method for identifying polyamide 6 or polyamide 66 in blended textiles. The method comprises the following steps: (1) a polyamide 6 or polyamide 66 pure product is taken and a formic acid solution is added for dissolving, filtering is carried out, a solution is taken and placed in a sample cup, or a polyamide 6 or polyamide 66 pure product is directly taken and placed in a sample cup, a pyrolysis gas chromatography-mass spectrometry method is used for carrying out analysis, and a program and a mass spectrogram of a standard sample are obtained; (2) a blended textile sample to be measured is taken, a formic acid solution is added for carrying out immersion treatment, a polyamide component in the sample to be measured is dissolved, filtering is carried out, filtrate of the sample to be measured is placed in a sample cup, the pyrolysis gas chromatography-mass spectrometry method is used for carrying out analysis, and a program and a mass spectrogram of the sample to be measured are obtained; (3) compared with the standard sample, and according to characteristic pyrolysis substances and retention time of the sample to be measured as well as peak area and relative content thereof, identification and analysis of components are carried out. The method has the advantages of simple, sensitive and reliable operation, few reagent and sample amounts, and little influences on body health of test personnel and surrounding environment.

Description

technical field [0001] The invention relates to the field of analysis and detection, in particular to an identification method for polyamide 6 or polyamide 66 in blended products. Background technique [0002] Blended products of different composition account for a large part of the textile industry and trade. Rapid characterization of blend components and accurate quantitative analysis of blend ratios are very important to traders and consumers as well as textile workers. [0003] Because of its good elasticity, wear resistance, fatigue resistance and corrosion resistance, polyamide fiber is often used for blending with cotton, hemp, silk, wool, polyester, spandex, viscose and other fibers to make various blended products. At present, the polyamide used for spinning synthetic fibers in the market is mainly polyamide 6 or polyamide 66, accounting for more than 98% of the total amount of polyamide fibers. [0004] The national standard GB / T 2910.7 specifies the chemical dis...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/042
Inventor 陈海相林型跑谢甲增戴宏翔
Owner ZHEJIANG SCI-TECH UNIV
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