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2,2',4,4'-tetrabromodiphenyl ether solution standard substance in methanol and preparation method thereof

A technology of tetrabromodiphenyl ether and standard substance, which is applied in the field of measurement and can solve problems such as the inability to achieve uniform values

Pending Publication Date: 2021-06-25
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 2,2 ', 4,4'-tetrabromodiphenyl ether solution standard substance and preparation method thereof in methanol, to solve the problem of 2,2',4,4'-tetrabromodiphenyl ether in the prior art The problem that brominated diphenyl ethers cannot achieve a uniform value

Method used

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  • 2,2',4,4'-tetrabromodiphenyl ether solution standard substance in methanol and preparation method thereof
  • 2,2',4,4'-tetrabromodiphenyl ether solution standard substance in methanol and preparation method thereof
  • 2,2',4,4'-tetrabromodiphenyl ether solution standard substance in methanol and preparation method thereof

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[0045] The present invention will be described in further detail below in conjunction with the accompanying drawings. Among them, the purity sample 2,2′,4,4′-tetrabromodiphenyl ether used in this example comes from Ultra, CAS5436-43-1, the purity (HPLC, 235nm) is 98.18%, and 4 bottles of samples are purchased , 2.5g / bottle, after grinding evenly, preserve in desiccator; Methanol is bought from commercial channel, is the chromatographic pure level reagent that Merck company (Germany) produces, does not introduce impurity after purity test; Experimental water is ultrapure water.

[0046] Standard material preparation equipment: 250mL grade A volumetric flask; electronic balance (CPA225D, d=0.1mg) (Sartorius, Germany), all passed the test; packaging container: 2mL brown ampoule bottle and sealing equipment.

[0047] The instruments used are as follows: gas chromatograph (7890B, Agilent Technologies), equipped with FID detector; liquid chromatograph (e2695, Waters), equipped with...

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Abstract

The invention discloses a preparation method of a 2,2',4,4'-tetrabromodiphenyl ether solution purity standard substance in methanol. The method comprises the following steps: carrying out qualitative analysis on 2,2',4,4'-tetrabromodiphenyl ether; preparing a 2,2',4,4'-tetrabromodiphenyl ether solution in 2.0 mg / mL methanol as purity sample; carrying out primary homogeneity detection on the purity sample by adopting a liquid chromatography method; preparing a 2,2',4,4'-tetrabromodiphenyl ether solution in methanol from the 2,2',4,4'-tetrabromodiphenyl ether subjected to primary homogeneity detection and accurate valuation as a standard sample; and carrying out uniformity test, stability test, valuing and uncertainty analysis on the standard sample according to metrology requirements, wherein if the uniformity, stability and uncertainty all meet requirements, definite value is accurate and stable, and metrology characteristics are met, the substance is purity standard substance. According to the invention, the 2,2',4,4'-tetrabromodiphenyl ether solution purity standard substance in methanol is mainly used as a standard of quantity transfer, meets the requirements of current research and detection, and is used for related research of brominated flame retardants.

Description

technical field [0001] The invention belongs to the technical field of measurement and relates to organic standard substances, in particular to a standard substance of 2,2',4,4'-tetrabromodiphenyl ether solution in methanol and a preparation method thereof. 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] 2,2′,4,4′-Tetrabromodiphenyl ether is a kind of polybrominated diphenyl ether, the existing detection generally adopts gas chromatography, liquid chromatography, liquid chromatography-mass spectrometry, gas chromatography-mass spectrometry Com...

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Application Information

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IPC IPC(8): G01N30/02G01N30/04G01N24/08
CPCG01N24/08G01N30/02G01N30/04G01N2030/047
Inventor 崔厚祥陈玲黄彦捷吴武杰王世超
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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