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Method for detecting dibromoneopentyl glycol in textiles

A dibromoneopentyl glycol and detection method technology, which is applied in the field of detection of dibromoneopentyl glycol in textiles, can solve cumbersome and time-consuming problems, difficulty in realizing dibromoneopentyl glycol qualitative and quantitative analysis, poor accuracy, etc. problem, to achieve the effect of short separation time, high accuracy and accurate results

Active Publication Date: 2018-06-26
广电计量检测(成都)有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Li Shan et al. used hydrogen ion flame-gas chromatography to analyze the brominated products of pentaerythritol. This method is not only cumbersome and time-consuming, but also has poor accuracy. Qualitative and quantitative analysis of bromoneopentyl glycol content, the existing technology is difficult to achieve qualitative and quantitative analysis of dibromoneopentyl glycol in textiles

Method used

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  • Method for detecting dibromoneopentyl glycol in textiles
  • Method for detecting dibromoneopentyl glycol in textiles
  • Method for detecting dibromoneopentyl glycol in textiles

Examples

Experimental program
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Effect test

Embodiment 1

[0049] In the present embodiment, the detection method of dibromoneopentyl glycol in textiles comprises the following steps:

[0050] Sample pretreatment: Take the textile sample to be tested, cut it into 2mm×2mm size, accurately weigh 1.0g, put it into a 60mL sample bottle, add 10mL of acetone accurately, put it in an ultrasonic generator after sealing it with a stopper, ultrasonically extract for 45min, and extract The solution was filtered with a 0.45 μm PTFE microporous membrane, and the filtrate was taken to obtain the solution to be tested.

[0051] Gas chromatography-mass spectrometry detection: the filtrate is subjected to gas chromatography-mass spectrometry detection, and the external standard method is used for quantification.

[0052] In this example, the gas chromatography conditions are as follows: chromatographic column: DB-624 capillary chromatographic column: 30m×250μm×1.40μm; heating program: initial temperature of 150°C, keep for 1min, then rise to 250°C, h...

Embodiment 2

[0067] The precision and recovery of the detection method

[0068] Add 0.5mg / L, 5mg / L, 20mg / L 3 levels of concentration to the negative sample respectively and add the standard recovery measurement, according to the gas chromatography-mass spectrometry detection method described in Example 1, repeat the measurement for each addition level 7 times , the results are shown in Table 3.

[0069] The standard recovery and precision (n=7) of table 3 dibromoneopentyl glycol

[0070] Add scalar

[0071] As can be seen from Table 3, under 3 kinds of standard addition levels, its standard addition recovery rate is 99.4%~100.7%, and relative standard deviation (RSD) is 1.9%~3.6%, shows that detection method recovery rate of the present invention is good, High precision. Comparative example 1

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Abstract

The invention discloses a method for detecting dibromoneopentyl glycol in textiles. The method comprises pre-treatment on a sample: taking a sample to be tested, adding acetone into the sample, carrying out ultrasonic extraction and collecting the extract to obtain a solution to be tested, and gas chromatography-mass spectrometry detection: carrying out gas chromatography-mass spectrometry detection on the filtrate and carrying out quantification through an external standard method, wherein the gas chromatography conditions comprise a DB-624 capillary column as a chromatographic column, a programmed heating mode, a sample inlet temperature of 230-260 DEG C and a splitless sample introducing mode and the mass spectrometry conditions comprise electron bombardment ionization, an ion source temperature of 200-230 DEG C, a gas chromatography-mass spectrometry interface temperature of 230-280 DEG C and a full scanning mode and a selected ion scanning mode as collection modes. The method hasa fast detection rate, a detection limit of 0.045 mg / L, an adding standard recovery rate of 99.4%-100.7% and relative standard deviation of less than or equal to 3.6%.

Description

technical field [0001] The invention relates to the field of analysis and determination of flame retardants, and more specifically, the invention relates to a method for detecting dibromoneopentyl glycol in textiles. Background technique [0002] Dibromoneopentyl glycol is a reactive flame retardant with excellent performance. It is suitable for unsaturated polyester resins, thermoplastic resins and polyurethane resins, and can also be used in rigid polyurethane foams. When it is added to polymers, the prepared polymers have excellent flame retardancy, light stability and chemical resistance. properties, and the dosage is small, and has no effect on the mechanical properties of the base resin, especially its mixture with antimony trioxide is especially suitable for flame-retardant fibers. This mixture and high polymer can form good fluidity and spinnability The melt of the obtained flame retardant fiber has good mechanical properties. Therefore, dibromoneopentyl glycol is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/72G01N30/02
CPCG01N30/02G01N30/7206
Inventor 李支薇王华严洪连任祥祥
Owner 广电计量检测(成都)有限公司
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