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Rapid detection method for content of phthalate

A phthalate ester and detection method technology, applied in the field of safety detection, can solve the problems of inability to truly simulate samples, errors, state and performance differences, etc., to avoid the use of sample pretreatment process and chemical reagents, and improve accuracy Accuracy and sensitivity, avoiding the effect of sample pretreatment process

Pending Publication Date: 2021-06-01
GUANGDONG TESTING INST OF PROD QUALITY SUPERVISION +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The traditional GC / MS (gas chromatography-mass spectrometry) method needs to use a large amount of chemical reagents, pollutes the environment, and the operation process is cumbersome; the existing PY-GC / MS (pyrolysis-gas chromatography / mass spectrometry) method detects o-benzene In the process of diformate content, the quantitative method of establishing a standard curve through liquid standard samples is mainly used. Since the state and performance of the liquid standard samples and the actual children’s samples are also quite different, it is impossible to truly simulate the samples. During the test process There will be a certain degree of error in the

Method used

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  • Rapid detection method for content of phthalate
  • Rapid detection method for content of phthalate
  • Rapid detection method for content of phthalate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] This embodiment provides a kind of rapid detection method of phthalate content, specifically as follows:

[0069] S1. Preparation of solid standard samples

[0070] Weigh 6 standard phthalates (dibutyl phthalate, phenyl butyl phthalate, dihexyl phthalate, dioctyl phthalate, phthalate Diisononyl formate and diisodecyl phthalate) were dissolved in tetrahydrofuran respectively to obtain a solution containing 6 kinds of phthalates; PVA was added to the phthalates solution, mixed After uniform drying, it is made into a plastic film to obtain a standard sample.

[0071] S2. Analysis of solid standard samples on the computer

[0072] Take the plastic film obtained in step S1, and test it on the machine, using the Shimadzu Py-Screener system;

[0073] The thermal cracking conditions are as follows: the initial temperature of the cracking furnace is 150°C, the temperature is raised to 320°C at 200°C / min, kept for 0.5min, and the interface temperature is 300°C.

[0074] The c...

Embodiment 2

[0087] This embodiment provides a kind of rapid detection method of phthalate content, specifically as follows:

[0088] S1. Preparation of solid standard samples

[0089] Weigh 6 standard phthalates (dibutyl phthalate, phenyl butyl phthalate, dihexyl phthalate, dioctyl phthalate, phthalate Diisononyl formate and diisodecyl phthalate) were dissolved in tetrahydrofuran respectively to obtain a solution containing 6 kinds of phthalates; PVA was added to the phthalates solution, mixed After drying evenly, make a plastic film to obtain a standard sample; in this standard sample, the weight content of phthalates is 1000mg / kg.

[0090] S2. Analysis of solid standard samples on the computer

[0091] Take the plastic film obtained in step S1, and test it on the machine, using the Shimadzu Py-Screener system;

[0092] The thermal cracking conditions are as follows: the initial temperature of the cracking furnace is 150°C, the temperature is raised to 320°C at 200°C / min, kept for 0.5...

Embodiment 3

[0099] This embodiment provides a kind of rapid detection method of phthalate content, specifically as follows:

[0100] S1. Preparation of solid standard samples

[0101] Weigh 6 standard phthalates (dibutyl phthalate, phenyl butyl phthalate, dihexyl phthalate, dioctyl phthalate, phthalate Diisononyl formate and diisodecyl phthalate) were dissolved in cyclohexanone respectively to obtain a solution containing 6 kinds of phthalates; in the phthalates solution, PU was added powder, mixed and dried to make a plastic film to obtain a standard sample; in this standard sample, the weight content of phthalates is 10mg / kg.

[0102] S2. Analysis of solid standard samples on the computer

[0103] Take the plastic film obtained in step S1, and test it on the machine, using the Shimadzu Py-Screener system;

[0104] The thermal cracking conditions are as follows: the initial temperature of the cracking furnace is 150°C, the temperature is raised to 320°C at 200°C / min, kept for 0.5min, ...

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Abstract

The invention provides a rapid detection method for content of phthalate. The method comprises the following steps: dissolving phthalate and plastic powder in a solvent, drying to form a film, and preparing a solid standard sample; weighing a to-be-tested sample, pretreating, and preparing a sample to be tested; and taking the solid standard sample and the to-be-tested sample, and carrying out thermal cracking-gas chromatography / mass spectrometry instrument determination. The solid standard sample is a plastic film; a sample injection mode adopted by the gas chromatography / mass spectrometry is split sample injection, and the split ratio is (45 to 55): 1; and the conditions of thermal cracking is as follows: the initial temperature of a cracking furnace is 140 to 160 DEG C, the temperature is raised to 310 to 330 DEG C at the rate of 190 to 210 DEG C / min, the temperature is kept for 0.3 to 0.8 min, and the interface temperature is 290 to 310 DEG C. The result of the detection method has the advantage of low detection limit, the recovery rate meets the test requirement, and the method is simple, convenient, rapid, green and environment-friendly.

Description

technical field [0001] The invention relates to the technical field of safety detection, in particular to a rapid detection method for phthalate content. Background technique [0002] As a key pollutant, phthalates are harmful to the human body in the form of interference with human endocrine, resulting in deformities of human limbs, endocrine disorders, reproductive system lesions, and increased incidence of breast cancer. Due to environmental and process pollution, or added to children's products as plasticizers, there is a risk of excessive content of phthalates in children's products such as textiles, shoe parts, toys, etc., and through the interaction with the human body when wearing or using Through friction and sweat extraction, it enters the human body and causes poisoning. In view of the serious harm of phthalates to the human body, especially children, national mandatory standards such as GB 31701 "Safety Technical Specifications for Infants and Children's Textile...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/32G01N30/72
CPCG01N30/02G01N30/06G01N30/30G01N30/32G01N30/72G01N2030/324
Inventor 胡勇杰韩健健殷桃胡辉赵晶
Owner GUANGDONG TESTING INST OF PROD QUALITY SUPERVISION
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