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4, 4 '-dibromodiphenyl ether purity standard substance and preparation method thereof

A technology of dibromodiphenyl ether and standard substance, which is applied in the field of measurement and can solve the problems that the detection method cannot meet the requirements of the fixed value

Inactive Publication Date: 2021-06-22
广东省计量科学研究院(华南国家计量测试中心)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The object of the present invention is to provide a kind of 4,4'-dibromodiphenyl ether purity standard substance and its preparation method, to solve the problem that the detection method existing in the prior art can't satisfy the fixed value requirement

Method used

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  • 4, 4 '-dibromodiphenyl ether purity standard substance and preparation method thereof
  • 4, 4 '-dibromodiphenyl ether purity standard substance and preparation method thereof

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Embodiment Construction

[0040] The present invention will be described in further detail below in conjunction with the accompanying drawings. Among them, the purity sample 4,4'-dibromodiphenyl ether used in this example comes from SIGMA-ALDRICH, CAS2050-47-7, the nominal purity (GC) is 99.2%, and 5 bottles of samples are purchased, 100g / Bottles were ground evenly and stored in a desiccator; during the experiment, methanol and acetonitrile were chromatographic grade reagents (Merck), and the experimental water was ultrapure water.

[0041] Equipment for standard substance preparation: 250mL grade A volumetric flask; electronic balance (CPA225D, d=0.1mg) (Sartorius, Germany), all passed the test; packaging container: 5mL brown sample bottle.

[0042]The instruments used are as follows: gas chromatograph (7890B, Agilent Technologies), equipped with FID detector; liquid chromatograph (e2695, Waters), equipped with diode array detector (2998, Waters), C18 chromatographic column (250mm×4.6mm, i.d. ,5 μm)...

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Abstract

The invention discloses a preparation method of a 4, 4 '-dibromodiphenyl ether purity standard substance. The preparation method comprises the following steps of: respectively carrying out qualitative analysis on 4, 4'-dibromodiphenyl ether by gas chromatography-mass spectrometry and nuclear magnetic resonance; determining raw material substances through qualitative analysis, carrying out primary uniformity detection on the 4, 4 '-dibromodiphenyl ether by adopting a liquid chromatography method, and screening out a sample with uniform purity as a the 4, 4'-dibromodiphenyl ether purity standard substance candidate; performing homogeneity test, stability test and constant value and uncertainty analysis on the 4, 4 '-dibromodiphenyl ether purity standard substance candidate according to metrology requirements, and under the conditions that the homogeneity, the stability and the uncertainty of thesubstance candidate all meet the requirements, the constant value of the substance candidate is accurate and stable, and the substance candidate accords with metrology characteristics,taking the substance candidate as the 4, 4'-dibromodiphenyl ether purity standard substance. The 4, 4 '-dibromodiphenyl ether purity standard substance developed by the method of the invention 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 an organic standard substance, in particular to a 4,4'-dibromodiphenyl ether purity standard substance and a preparation method thereof. Background technique [0002] In the prior art, methods such as gas chromatography, liquid chromatography, and gas chromatography-mass spectrometry are generally used for the detection and detection of PBDEs. However, the sensitivities of various methods are inconsistent, resulting in large differences in drug analysis results. Therefore, unified The standard substance realizes the unification of quantity and value. As a kind of polybrominated diphenyl ether, 4,4′-dibromodiphenyl ether has a great reality in the development of its purity standard, the traceability of the value, and the comparability and uniformity of the test results. Significance, therefore, it is very necessary to provide a kind of 4,4'-dibromodiphenyl ether purity standard ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/04G01N24/08
CPCG01N24/08G01N30/02G01N30/04G01N2030/047
Inventor 陈玲许俊斌罗思婷廖泽荣
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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