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Detection method for bis(2-ethylhexyl)amine in leather and textiles

A detection method and textile technology, applied in the field of chemical analysis, can solve problems such as product obstruction, achieve high sensitivity and accuracy, and have good application prospects

Active Publication Date: 2017-04-26
广电计量检测(西安)有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the detection method of diisooctylamine in the product has not been reported, which has formed a certain obstacle to the entry of related products in my country into the EU market.

Method used

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  • Detection method for bis(2-ethylhexyl)amine in leather and textiles
  • Detection method for bis(2-ethylhexyl)amine in leather and textiles
  • Detection method for bis(2-ethylhexyl)amine in leather and textiles

Examples

Experimental program
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Effect test

Embodiment 1

[0051] Cut the leather or textile sample to a size of 2mm×2mm×2mm, weigh 1g±0.1g (accurate to 0.1mg) into a 60ml glass reaction bottle, add 10ml of methanol, conduct ultrasonic extraction at 60°C for 60min±5min, repeat the extraction once , combined the two extracts and mixed evenly, concentrated to about 2ml with a rotary evaporator, slowly blown with nitrogen to near dryness, fixed the volume to 1ml with methanol, filtered through a 0.45μm microporous membrane, and then performed gas chromatography-mass spectrometry Use detection.

[0052] Gas chromatography conditions: Chromatographic column: DB-624, length 30m, film thickness 1.4μm, inner diameter 0.25mm; heating program: initial temperature is 120°C, keep for 1min, rise to 250°C at a rate of 20°C / min, keep for 3.5min ; Inlet temperature: 250°C; Injection mode: splitless; Injection volume: 1 μL; Carrier gas: Helium, purity ≥ 99.999%; Flow rate: 1.5ml / min; External standard method for quantification. Mass spectrometry cond...

Embodiment 2

[0054] The detection method is basically the same as in Example 1, the difference is only in the heating program: the initial temperature is 100°C, kept for 1min, raised to 250°C at a rate of 30°C / min, kept for 7min, the chromatographic results are as follows image 3 As shown, it can be seen that diisooctylamine can be separated, but compared with Example 1, the response value is lower, the peak time is earlier, and the analysis time is longer.

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Abstract

The invention discloses a detection method for bis((2-ethylhexyl)amine in leather and textiles. The detection method comprises the following steps: treating a sample, namely taking a sample to be detected, adding the sample to be detected into an organic solvent, and extracting to obtain extract liquor; and carrying out gas chromatography-mass spectrometry detection. The detection method disclosed by the invention is simple, convenient and rapid, methanol is preferably taken as an extraction agent, after extraction with methanol, bis((2-ethylhexyl)amine is subjected to chromatographic analysis once within 11min under the optimized detection condition, and a good separation effect can be obtained. The method has good linearity when the concentration range of bis((2-ethylhexyl)amine is of 0.1-10mg / L, the linearly dependent coefficient reaches 0.9998, the detection limit reaches 0.1mg / L, the repeatability relative standard deviation is less than 3%, and the sample adding standard recovery rate is 95%-110%, so that the detection method has good application prospect.

Description

technical field [0001] The invention relates to the field of chemical analysis, in particular to a method for detecting diisooctylamine in leather and textiles. Background technique [0002] Diisooctylamine is mainly used as an intermediate of surfactant, used in leather textiles, and can also be used for ore floating washing, extraction agent of rare metals, emulsifier, etc. Studies have shown that diisooctylamine is toxic to fish, irritating to eyes and skin, has potential persistence, bioaccumulation and toxicity, and seriously endangers human health. On March 17, 2015, ECHA, the European Chemicals Agency, officially released the 2015-2017 EU Community Rolling Action Plan (CoRAP) substance list, which contains a total of 134 substances, and diethylamine is included in it. It can be seen that the hazards of diisooctylamine have attracted great attention from the society. Therefore, it is very necessary to establish an appropriate detection method to detect the content of ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/72
CPCG01N30/02G01N30/06G01N30/30G01N30/72G01N2030/062
Inventor 王华严洪连李支薇任祥祥
Owner 广电计量检测(西安)有限公司
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