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Detection method of phthalate plasticizer

A technology of ester plasticizer and phthalic acid, which is applied in the detection field, can solve the problems of quantitative measurement errors, low sensitivity of the measurement method, etc., and achieve the effect of improving accuracy

Inactive Publication Date: 2010-10-13
深圳出入境检验检疫局玩具检测技术中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] (2) Quantitative determination has errors
[0018] (3) The sensitivity of quantitative determination is low
Using such a low-abundance ion as a quantitative ion, the sensitivity of the determination method must be relatively low

Method used

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  • Detection method of phthalate plasticizer
  • Detection method of phthalate plasticizer
  • Detection method of phthalate plasticizer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Embodiment 1, a kind of detection method of phthalate plasticizer comprises the following steps:

[0062] 1. Weigh 0.0505g of PVC sample ground to powder, put it into a sealable glass vial, add 5ml THF and shake for 30 minutes to fully dissolve the sample. Then add 10ml of n-hexane to precipitate the polymer, let it stand for 5 minutes and filter the solution with 0.45 μm PTFE filter paper, take 0.1ml of the filtrate and add 1ml of 4.14ug / ml benzyl benzoate solution as an internal standard to prepare the solution to be tested.

[0063] 2. The solution to be tested is determined by gas chromatography and chemical ionization mass spectrometry: the specific steps are:

[0064] (1) Set the operation method steps of gas chromatography and chemical ionization mass spectrometry, and the following parameter conditions:

[0065] (1.1), the gas chromatography conditions are: chromatographic column: HP-5MS 30m×0.25mm×0.25um;

[0066] Carrier gas: helium;

[0067] Injection port...

Embodiment 2

[0082] Embodiment 2, a kind of detection method of phthalates plasticizer comprises the following steps:

[0083] 1. Weigh 0.0508g of PVC sample ground to powder into a sealable glass vial, add 5ml of THF and shake for 30 minutes to fully dissolve the sample. Then add 10ml of n-hexane to precipitate the polymer, let it stand for 20 minutes and filter the solution with 0.45 μm PTFE filter paper, take 0.1ml of the filtrate and add 1ml of 4.14ug / ml benzyl benzoate solution as an internal standard to prepare the solution to be tested.

[0084] 2. The solution to be tested is determined by gas chromatography and chemical ionization mass spectrometry: the specific steps are:

[0085] (1) Set the operation method steps of gas chromatography and chemical ionization mass spectrometry, and the following parameter conditions:

[0086] 1.1), the gas chromatography conditions are: chromatographic column: HP-5MS 30m×0.25mm×0.25um;

[0087] Carrier gas: helium;

[0088] Injection port tem...

Embodiment 3

[0103] Embodiment 3, a kind of detection method of phthalate plasticizer comprises the following steps:

[0104] 1. Weigh 0.0503g of PVC sample ground to powder into a sealable glass vial, add 5ml of THF and shake for 30 minutes to fully dissolve the sample. Then add 10ml of n-hexane to precipitate the polymer, let it stand for 8 minutes and filter the solution with 0.45 μm PTFE filter paper, take 0.1ml of the filtrate and add 1ml of 4.14ug / ml benzyl benzoate solution as an internal standard to prepare the solution to be tested.

[0105] 2. The solution to be tested is determined by gas chromatography and chemical ionization mass spectrometry: the specific steps are:

[0106] (1) Set the operation method steps of gas chromatography and chemical ionization mass spectrometry, and the following parameter conditions:

[0107] (1.1), the gas chromatography conditions are: chromatographic column: HP-5MS 30m×0.25mm×0.25um;

[0108] Carrier gas: helium;

[0109] Injection port temper...

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Abstract

The invention discloses a detection method of a phthalate plasticizer, comprising the following steps: 1. pretreatment: putting a sample to be detected into an organic solvent, and then dissolving and treating to obtain the solution to be detected in which the plasticizer is dissolved; and 2. content determination of the plasticizer: utilizing a gas chromatogram method and a chemical ionization mass spectrometry method to detect the type and the content of the plasticizer in the detected solution, wherein, the chemical ionization reagent used in the chemical ionization mass spectrometry method is composed of isobutane, methane or ammonia. The detection method of the phthalate plasticizer provided by the invention has high qualitative and quantitative accuracy and high quantitative detection sensitivity.

Description

technical field [0001] The invention relates to a detection method, in particular to a detection method of phthalate plasticizers. Background technique [0002] Because phthalates have good compatibility with plastics such as PVC, they are often used as general-purpose plasticizers, but such compounds have been proven to be harmful to the human reproductive system. The European Union has banned the use of six phthalate plasticizers in toys and children's products, including dibutyl phthalate (DBP, CAS: 84-74-2), phthalate Butylbenzyl dicarboxylate (BBP, CAS: 85-68-7), bis(2-ethylhexyl) phthalate (DEHP, CAS: 117-81-7), di-n-octyl phthalate ( DNOP, CAS: 117-84-0), diisononyl phthalate (DINP, CAS: 28553-12-0) and diisodecyl phthalate (DIDP, CAS: 26761-40-0) The Consumer Product Safety Promotion Act issued by the United States in 2008 also prohibits the use of the above six substances in toys, so the determination of these six phthalates is very important. [0003] The determ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N27/62G01N1/28
Inventor 李宣江丽媛卢瑜梁淑雯禹伟腾杨曦周昆郭宗宁
Owner 深圳出入境检验检疫局玩具检测技术中心
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