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Method for using gas chromatography-mass spectrometry to detect content of phthalic anhydride in toy

A technology of phthalic anhydride and GC-MS, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of poor anti-interference ability and false positive, and achieve the effect of good solubility and high sensitivity

Active Publication Date: 2018-08-10
广东省中鼎检测技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the anti-interference ability of gas chromatography is relatively poor when qualitative. For toy materials with complex components, especially plastic samples with phthalates added as plasticizers, they will be affected by other phthalates during qualitative analysis. false positive

Method used

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  • Method for using gas chromatography-mass spectrometry to detect content of phthalic anhydride in toy
  • Method for using gas chromatography-mass spectrometry to detect content of phthalic anhydride in toy
  • Method for using gas chromatography-mass spectrometry to detect content of phthalic anhydride in toy

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] This embodiment provides a method for detecting the content of phthalic anhydride in toys by gas chromatography-mass spectrometry, comprising the following steps:

[0035] The first step is to take a sample from the toy: use stainless steel scissors to cut the toy sample into small rectangular pieces with a diagonal length not greater than 5mm.

[0036] In the second step, weigh 1.0 g of the shredded sample and place it in a 40 mL container (reaction tube in this example), then add 10 mL of toluene to the container, shake it so that the sample is completely submerged in toluene, and screw on the bottle cap , put the container in an ultrasonic cleaner for ultrasonic extraction for 60 minutes, the ultrasonic frequency is 50 kHz, and the ultrasonic temperature is 40° C. to obtain the extract;

[0037] The third step is to filter the extract obtained in the second step to obtain the test solution, specifically, filter 2 mL of the extract with a 0.45 μm polytetrafluoroethyle...

Embodiment 2

[0058] The difference from Example 1 lies in the first step to the third step:

[0059] The first step is to take a sample from the toy: use stainless steel scissors to cut the sample into small round pieces with a diameter of no more than 5mm.

[0060] In the second step, take 1.0 g of the shredded sample and place it in a 40 mL container (reaction tube in this embodiment), then add 8 mL of toluene to the container, shake it, so that the sample is completely submerged in toluene, and screw on the bottle cap , put the container in an ultrasonic cleaner for ultrasonic extraction for 120min, the ultrasonic frequency is 80kHz, and the ultrasonic temperature is 42°C to obtain the extract;

[0061] The third step is to filter the extract obtained in the second step to obtain the test solution, specifically, filter 2 mL of the extract with a 0.35 μm polytetrafluoroethylene filter membrane into the sample bottle;

[0062] The rest are the same as in Embodiment 1, and will not be rep...

Embodiment 3

[0066] The difference from Example 1 lies in the first step to the third step:

[0067] The first step is to take a sample from the toy: use stainless steel scissors to cut the sample into small oval pieces with a long axis of no more than 5mm.

[0068] In the second step, weigh 1.0 g of the shredded sample and place it in a 40 mL container (reaction tube in this embodiment), then add 12 mL of toluene to the container, shake it so that the sample is completely submerged in toluene, and screw on the bottle cap , put the container in an ultrasonic cleaner for ultrasonic extraction for 150 minutes, the ultrasonic frequency is 40kHz, and the ultrasonic temperature is 35°C to obtain the extract;

[0069] The third step is to filter the extract obtained in the second step to obtain the test solution, specifically, filter 2 mL of the extract with a 0.22 μm polytetrafluoroethylene filter membrane into the sample bottle;

[0070] The rest are the same as in Embodiment 1, and will not ...

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Abstract

The invention belongs to the technical field of a chemical detection method of consumer goods, and particularly relates to a method for using gas chromatography-mass spectrometry to detect the contentof phthalic anhydride in a toy. The method comprises the following the steps of sampling the toy to obtain a sample; weighing a certain amount of the sample to be put in a container, then adding methylbenzene into the container, sealing, and putting the container in a water bath ultrasonic instrument for ultrasonic extraction to obtain extraction liquor; filtering the extraction liquor to obtainto-be-tested liquor; using a gas chromatography-mass spectrometer (GC-MS) to analyze the to-be-tested liquor. Compared with the prior art, a proper extraction condition is selected, phthalic anhydridein the material of the toy can be efficiently extracted, and then the gas chromatography-mass spectrometer is utilized to analyze phthalic anhydride. The method is quick and simple and accurate in testing.

Description

technical field [0001] The invention belongs to the technical field of chemical detection methods for consumer products, and in particular relates to a method for detecting the content of phthalic anhydride in toys by gas chromatography-mass spectrometry. Background technique [0002] Phthalic anhydride, referred to as phthalic anhydride, is a cyclic anhydride formed by intramolecular dehydration of phthalic acid, and is an important raw material in chemical industry. Phthalic anhydride has a wide range of applications in plasticizer manufacturing, unsaturated resin synthesis, pigments and dyes, paints and coatings, food additives, medicine and pesticides. [0003] Phthalic anhydride is an acidic corrosive product. Repeated exposure can sensitize the skin, causing rashes, chronic eye irritation, chronic bronchitis, and asthma. In view of its harm to the human body, the "Washington State Children's Product Safety Act" published by Washington State of the United States listed...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 魏莹莹李静何晓莹
Owner 广东省中鼎检测技术有限公司
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