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4-Bromodiphenyl ether purity standard substance determination method

A brominated diphenyl ether and standard substance technology, applied in the field of measurement, can solve the problem that the detection method cannot meet the requirements of the fixed value

Active Publication Date: 2021-11-16
广东省计量科学研究院(华南国家计量测试中心)
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Problems solved by technology

[0004] The object of the present invention is to provide a kind of 4-bromodiphenyl ether purity standard substance determination method, to solve the problem that the detection method existing in the prior art can not satisfy the determination requirement

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  • 4-Bromodiphenyl ether purity standard substance determination method
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  • 4-Bromodiphenyl ether purity standard substance determination method

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Embodiment Construction

[0047] The present invention will be described in further detail below in conjunction with the accompanying drawings.

[0048] The 4-bromodiphenyl ether purity standard substance determination method comprises the steps:

[0049] (1) Accurately weigh 50.2 mg of 4-bromodiphenyl ether, and dilute to 25 mL with methanol to obtain a methanol solution of 4-bromodiphenyl ether with a concentration of 2.0 mg / mL. Diphenyl ether purity standard substance organic purity fixed value;

[0050] (2) Utilize gas chromatography to determine the organic purity of 4-bromodiphenyl ether purity standard substance;

[0051] (3) adopt Karl Fischer moisture meter to test 4-bromodiphenyl ether purity material moisture;

[0052] (4) test the inorganic elements contained in the 4-bromodiphenyl ether purity standard substance by ICP / MS;

[0053] (5) Solvent residue analysis was performed on the pure raw materials used for the preparation of the 4-bromodiphenyl ether purity standard substance by GC-MS...

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Abstract

The invention discloses a method for determining the value of a 4-bromodiphenyl ether purity standard substance, which comprises the following steps: using high performance liquid chromatography to determine the organic purity of the 4-bromodiphenyl ether purity standard substance; using gas chromatography to determine the value of the 4-bromodiphenyl ether The organic purity value of brominated diphenyl ether purity standard substance is determined; the moisture content of 4-bromodiphenyl ether purity standard substance is tested by Karl Fischer moisture analyzer, and the inorganic elements contained in the 4-bromodiphenyl ether purity standard substance are tested by ICP / MS , using GC-MS to carry out solvent residue analysis to the 4-bromodiphenyl ether purity standard substance; the 4-bromodiphenyl ether purity standard substance is determined by the formula. The method for determining the value of 4-bromodiphenyl ether purity standard substance provided by the present invention uses high performance liquid chromatography and gas chromatography to determine the organic impurities, determines the moisture content with the Karl Fischer moisture analyzer, and determines the content of the inorganic impurities by ICP / MS, and performs solvent extraction. Residue analysis, using the mass balance method to determine the purity of 4-bromodiphenyl ether, the standard substance determination method, has traceability.

Description

technical field [0001] The invention belongs to the technical field of measurement, and relates to a method for determining the value of standard substances of standard purity of organic substances, in particular to a method for determining the value of standard substances of purity of 4-bromodiphenyl ether. Background technique [0002] Polybrominated diphenyl ethers are recognized as global organic pollutants, and their use is restricted or banned worldwide. The development of polybrominated diphenyl ether standard products, determination of their purity and the content of impurities contained in them are useful for the detection of polybrominated diphenyl ethers. Phenyl ether compounds are of great significance to ensure production safety and people's livelihood and health. [0003] In the prior art, gas chromatography-mass spectrometry is generally used for the detection and detection of polybrominated diphenyl ethers. For example, HJ 909-2017 discloses the determination...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/72G01N30/74
CPCG01N30/02G01N30/72G01N30/74
Inventor 陈玲周瑾艳阮瑞雯花秀兵王世超
Owner 广东省计量科学研究院(华南国家计量测试中心)
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