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Method for measuring content and migration volume of phosphorus-containing flame retardant in toys

A technology of migration and flame retardant, which is applied in the field of analysis and detection, can solve the problems of matrix interference, weak anti-interference ability, and easy blocking of chromatographic columns in GC-MS, and achieves high sensitivity, strong versatility and good reproducibility. Effect

Inactive Publication Date: 2019-04-23
GUANGDONG DONGGUAN QUALITY SUPERVISION TESTING CENT
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The detection methods of phosphorus-containing flame retardants in toys mainly include gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry. It is necessary to remove additives such as polymer compounds, pigments, and stabilizers in toys, otherwise it is easy to block the chromatographic column and contaminate the ion source
Moreover, ordinary purification columns are used, and the anti-interference ability is weak

Method used

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  • Method for measuring content and migration volume of phosphorus-containing flame retardant in toys
  • Method for measuring content and migration volume of phosphorus-containing flame retardant in toys
  • Method for measuring content and migration volume of phosphorus-containing flame retardant in toys

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Embodiment 1

[0038] Such as figure 1 As shown, the content and migration of phosphorus-containing flame retardants in plastic toys are determined. The phosphorus-containing flame retardants measured in this example are tris(2-chloroethyl) phosphate (TCEP), tris(2-chloropropyl phosphate) base) ester (TCPP) and tris(1,3-dichloro-2-propyl)phosphate (TDCP).

[0039] (1) Preparation before content determination:

[0040] a) Sample treatment: after crushing plastic toys, weigh 1.0g, accurate to 0.0001g, put it in a 50mL centrifuge tube, add 50mL of dichloromethane, ultrasonically extract for 40min, rotary evaporate to 1mL, and wait for purification.

[0041] b) Sample cleanup:

[0042] Activate the composite florisil column with 6mL of acetone and 6mL of dichloromethane respectively, add the sample concentrate, rinse with 5mL of dichloromethane, elute with 8mL of acetone, collect the eluate, and blow it with nitrogen at 40°C until it is nearly dry , dilute to 1mL with methanol, pass through a...

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Abstract

The invention discloses a method for measuring the content and migration volume of a phosphorus-containing flame retardant in toys. The method is characterized by comprising the following steps: (1) preparation before measuring of the content; (2) preparation before measuring of the migration volume; (3) preparation of a standard mixed solution; (4) analysis through a liquid chromatograph-mass spectrometer and the like. The content and migration volume of the phosphorus-containing flame retardant in the toys are measured, reproducibility is good, sensitivity is high, anti-jamming capability ishigh, operation is easy, and universality is high.

Description

technical field [0001] The invention relates to the field of analysis and detection, in particular to a method for measuring the content and migration of phosphorus-containing flame retardants in toys. Background technique [0002] Tris(2-chloroethyl)phosphate (TCEP), tris(2-chloropropyl)phosphate (TCPP) and tris(1 , 3-dichloro-2-propyl) ester (TDCP) content shall not exceed 5 mg / kg. TCEP belongs to Class 2 carcinogens and Class 1B reproductive toxic substances. Ingestion of TCEP can cause kidney, liver and brain toxicity, damage health and induce cancer. TCPP and TDCP are halogenated substitutes of TCEP, which have similar physicochemical properties and toxicological characteristics to TCEP. [0003] The detection methods of phosphorus-containing flame retardants in toys mainly include gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry. It is necessary to remove the polymer compounds, pigments, stabilizers and other additives in toys, otherw...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 钟少枢
Owner GUANGDONG DONGGUAN QUALITY SUPERVISION TESTING CENT