Liquid nitrogen pulverization-gas chromatography method for detecting harmful substances of acrylonitrile, styrene and ethylbenzene in packaging materials

A technology of liquid nitrogen crushing and gas chromatography, which is applied in the fields of styrene, acrylonitrile and ethylbenzene in food packaging materials, can solve the problems of small proportion of harmful substances, low detection limit and limited solubility, and achieve Fast and accurate qualitative analysis, strong operability and low detection limit

Active Publication Date: 2019-03-01
江苏澄信检验检测认证股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the detection method of acrylonitrile in the national standard is mainly GB / T 5009.152-2003 "Styrene-acrylonitrile copolymer and rubber-modified acrylonitrile-butadiene-styrene resin for food packaging and residual acrylonitrile in its molded products "Determination of Monomer", the sample in the standard is dissolved in N, N-dimethylformamide, and the method of packed column-manual headspace is used for detection. In actual detection, this method has certain defects: (1) N , N-dimethylformamide is a high boiling point reagent, which is an ideal solvent in gas phase detection, but its dissolving ability in dissolving AS and ABS materials is limited, and some materials are often not completely dissolved after ultrasonic dissolution for 30 minutes, which affects Determination effect; (2) The standard stipulates to add 3mLN, N-dimethylformyl to dissolve the sample and perform headspace operation. Due to the large solvent content, the proportion of solvent after headspace heating is relatively large, and the proportion of harmful substances in the sample The specific gravity is small, resulting in a low detection limit of the method

Method used

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  • Liquid nitrogen pulverization-gas chromatography method for detecting harmful substances of acrylonitrile, styrene and ethylbenzene in packaging materials
  • Liquid nitrogen pulverization-gas chromatography method for detecting harmful substances of acrylonitrile, styrene and ethylbenzene in packaging materials
  • Liquid nitrogen pulverization-gas chromatography method for detecting harmful substances of acrylonitrile, styrene and ethylbenzene in packaging materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Cut the AS material into pieces of about 0.5cm×0.5cm, cool in liquid nitrogen for 10 minutes, and pulverize in a liquid nitrogen pulverizer. Weigh 0.5g of the pulverized sample into a 22mL headspace bottle, seal it quickly, press The above-mentioned chromatographic conditions were used for detection, and the retention time of each substance was used for qualitative determination and the standard curve for quantitative determination. The samples were tested 6 times in parallel. The analysis results are shown in Table 1. Through analysis, the relative standard deviation (RSD) of parallel samples is 2.07%-2.83%, and the repeatability is good.

[0028] Table 1. Contents of acrylonitrile, ethylbenzene and styrene in AS samples

[0029] Numbering

Embodiment 2

[0031] Cut the ABS material into fragments of about 0.5cm×0.5cm, cool in liquid nitrogen for 10 minutes, and crush in a liquid nitrogen pulverizer. Weigh 0.5g of the pulverized sample into a 22mL headspace bottle, seal it quickly, press The above-mentioned chromatographic conditions were used for detection, and the retention time of each substance was used for qualitative determination and the standard curve for quantitative determination. The samples were tested 6 times in parallel. The analysis results are shown in Table 2. Through analysis, the relative standard deviation (RSD) of parallel samples is 1.37%-3.33%, and the repeatability is good.

[0032] Table 2. Contents of acrylonitrile, ethylbenzene and styrene in ABS samples

[0033] Numbering

Embodiment 3

[0035] Cut the AS material whose content has been measured above into pieces of about 0.5cm×0.5cm, place it in liquid nitrogen to cool for 10 minutes, place it in a liquid nitrogen pulverizer, and pulverize it. After weighing the sample, add two levels of standards Solution, 6 parallel samples were made for each content level, and the recovery rate and standard deviation were calculated. The results are shown in Table 3. The standard addition recovery rate was between 92.63% and 106.06%, and the relative standard deviation was between 1.89% and 2.87%. The method is reliable.

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Abstract

The invention belongs to the field of packaging material analysis and detection, and in particular, relates to a method for detecting harmful substances of acrylonitrile, styrene and ethylbenzene in a packaging material by liquid nitrogen pulverization-gas chromatography. The method comprises the following steps: cutting a sample into small particles, cooling by liquid nitrogen, placing in a liquid nitrogen pulverization instrument, and pulverizing; and weighing a certain amount of crushed sample, placing in a headspace bottle, quickly sealing, setting the proper heating temperature and heating time, and carrying out gas chromatographic analysis of the harmful substances in the sample. According to the standard sample peak appearance time and appearance peak size, acrylonitrile, styrene and ethylbenzene in the packaging material are qualitatively and quantitatively analyzed; in the established method, the detection limit of acrylonitrile is 0.1 mg / kg, and the detection limits of styrene and ethylbenzene are both 0.2 mg / kg. The method is simple and convenient to operate, the result is stable and reliable, and the harmful substances in the sample can be qualitatively and quantitatively detected quickly. Compared with a conventional sample solvent-dissolution method, the method saves the sample pretreatment time, reduces the detection limits of the harmful substances, and has good promotion and application value.

Description

technical field [0001] The invention relates to a method for detecting harmful substances of acrylonitrile, styrene and ethylbenzene in food packaging materials, in particular to a liquid nitrogen pulverization-gas chromatography detection of acrylonitrile, styrene and ethylbenzene in plastic packaging materials AS and ABS method. Background technique [0002] Acrylonitrile-styrene copolymer (AS) and acrylonitrile-butadiene-styrene copolymer (ABS), as thermoplastic engineering plastics, have the characteristics of heat resistance, oil resistance, chemical corrosion resistance and high impact strength, and are widely used in food Containers, food processing machinery and equipment, such as food contact materials such as water cups, beverage cups, juicers, soybean milk makers, etc. [0003] The harmful monomers remaining in AS and ABS materials mainly include acrylonitrile, ethylbenzene and styrene. As early as the 1980s, the U.S. Consumer Product Safety Commission found tha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 汪仕韬邵卫卫薛娜娜冯秀梅胡建卫荣王敏周敏
Owner 江苏澄信检验检测认证股份有限公司
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