Gas chromatography detection method for trace N,N-dimethyl formamide in synthesized leather

A technology of dimethylformamide and gas chromatography is applied in the field of detection of trace N,N-dimethylformamide in wet-process synthetic leather products, which can solve the problems of complicated operation, long time consumption and the like, and achieves good separation effect, Simple operation and cost saving effect

Inactive Publication Date: 2014-08-06
HEFEI UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In the prior art method, Ma Hewei extracted the N,N-dimethylformamide in the sample with distilled water, and the N,N-dimethylformamide in the extract was back-extracted with chloroform and then detected by GC-MS. This method is complicated to operate and takes a long time

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  • Gas chromatography detection method for trace N,N-dimethyl formamide in synthesized leather
  • Gas chromatography detection method for trace N,N-dimethyl formamide in synthesized leather
  • Gas chromatography detection method for trace N,N-dimethyl formamide in synthesized leather

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Embodiment 1

[0029] The specific operation steps of gas chromatographic detection of trace amounts of N,N-dimethylformamide in polyurethane synthetic leather are as follows:

[0030] (1) Preparation of N,N-dimethylformamide solution: add about 10mL of methanol in advance into a 25mL volumetric flask, then add 113.0mg of N,N-dimethylformamide, then add methanol to the scale line, and prepare a concentration of 4. 520mg / mL N,N-dimethylformamide solution;

[0031] (2) Prepare the internal standard solution: add about 10mL of methanol in advance into a 25mL volumetric flask, then add 1.000g of n-butanol, then add methanol to the mark, and prepare an internal standard solution of n-butanol with a concentration of 40mg / mL;

[0032] (3) Sample pretreatment: Weigh about 1g of the polyurethane synthetic leather to be tested (about 2mm×2mm) after being cut into pieces, add it to a 45mL screw cap sample bottle, and add 0.1mL of n-butanol internal standard solution with a concentration of 40mg / mL , a...

Embodiment 2

[0038] (1) Preparation of N,N-dimethylformamide solution: add about 10mL of methanol in advance into a 25mL volumetric flask, then add 362.0mg of N,N-dimethylformamide, then add methanol to the scale line, and prepare a concentration of 14.48mg / mL N,N-dimethylformamide solution;

[0039] (2) Prepare the internal standard solution: add about 10mL of methanol in advance into a 25mL volumetric flask, then add 1.000g of n-butanol, then add methanol to the mark, and prepare an internal standard solution of n-butanol with a concentration of 40mg / mL;

[0040] (3) Sample pretreatment: Weigh about 1g of the polyurethane synthetic leather to be tested (about 2mm×2mm) after being cut into pieces, add it to a 45mL screw cap sample bottle, and add 0.1mL of n-butanol internal standard solution with a concentration of 40mg / mL , accurately add 20mL of analytical pure methanol, and tighten the bottle cap to obtain the treatment A;

[0041] (4) Sample pretreatment for adding standard samples: ...

Embodiment 3

[0046] (1) Prepare N,N-dimethylformamide solution: add about 10mL of methanol in advance to a 25mL volumetric flask, then add 232.4mg of N,N-dimethylformamide, then add methanol to the scale line, and prepare a concentration of 9. 296mg / mL N,N-dimethylformamide solution;

[0047] (2) Prepare the internal standard solution: add about 10mL of methanol in advance into a 25mL volumetric flask, then add 1.000g of n-butanol, then add methanol to the mark, and prepare an internal standard solution of n-butanol with a concentration of 40mg / mL;

[0048] (3) Sample pretreatment: Weigh about 1g of the polyurethane synthetic leather to be tested (about 2mm×2mm) after being cut into pieces, add it to a 45mL screw cap sample bottle, and add 0.1mL of n-butanol internal standard solution with a concentration of 40mg / mL , accurately add 20mL of analytical pure methanol, and tighten the bottle cap to obtain the treatment A;

[0049] (4) Sample pretreatment for adding standard samples: Weigh ab...

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Abstract

The invention belongs to the product quality detection range, and mainly relates to a quick detection method for N,N-dimethyl formamide with trace content in polyurethane synthesized leather. The residual trace N,N-dimethyl formamide in the polyurethane synthesized leather is extracted through ultrasonic auxiliary enhanced methyl alcohol extraction; a gas chromatography analysis method is adopted to execute qualification, and an internal standard method is adopted to execute quantification, so that the content of the N,N-dimethyl formamide in an extracting solution is measured; the accuracy of the method is checked through a standard adding method. The method disclosed by the invention can be used for detecting micro or trace N,N-dimethyl formamide residues in a synthesized leather product. Compared with the conventional method, the method disclosed by the invention is low in cost and high in accuracy.

Description

technical field [0001] The invention belongs to the scope of quality detection of polyurethane synthetic leather, and in particular relates to a detection method for trace amounts of N,N-dimethylformamide in wet-process synthetic leather products. Background technique [0002] N,N-dimethylformamide is mainly used as an organic solvent in organic synthesis, dyes, pharmaceuticals, resins, leather and other industrial production. In the production of wet-process polyurethane synthetic leather, N,N-dimethylformamide is The washing and curing agent of polyurethane resin can enter the human body through the intact skin and digestive tract to damage the central nervous system and important organs. N,N-Dimethylformamide has been determined by the People's Republic of China Light Industry Standard QB / T4342-2012 "Safety Requirements for Polyurethane Synthetic Leather for Clothing" as the main raw materials such as base fabric and polyurethane resin, which can be coated by wet or dry m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 崔鹏徐怡清窦焰
Owner HEFEI UNIV OF TECH
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