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4-bromodiphenyl ether purity valuing method

A technology for brominated diphenyl ether and purity, which is applied in the field of 4-brominated diphenyl ether purity determination, and can solve the problems that the detection method cannot meet the determination requirements and the like

Active 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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Problems solved by technology

[0005] The purpose of the present invention is to provide a method for determining the purity of 4-bromodiphenyl ether, so as to solve the problem that the detection methods in the prior art cannot meet the requirements for determining the value

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Embodiment Construction

[0036] The present invention will be described in further detail below in conjunction with the accompanying drawings.

[0037] The method for determining the purity of 4-bromodiphenyl ether comprises:

[0038] (1) Calibrate the differential scanning calorimeter with Ga and In national standard material thermal analysis standard material, and then verify it with phenyl salicylate;

[0039] (2) Select 4-bromodiphenyl ether with a purity greater than 99% as a purity sample, randomly select 11 parts of accurately weighed 4-bromodiphenyl ether samples, and test each sample twice as follows: 4-bromodiphenyl ether Phenyl ether is placed in a differential scanning calorimeter, cooled to solidification, and then heated up after stabilization, at a heating rate of 0.5K / min to 40°C, and the purity result is calculated according to the melting peak area;

[0040] (3) Carry out normal distribution test and outlier test to the purity result, to correct the purity result, get the average va...

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Abstract

The invention discloses a 4-bromodiphenyl ether purity valuing method. The method comprises the following steps of: accurately weighing 4-bromodiphenyl ether, placing the 4-bromodiphenyl ether in a differential scanning calorimeter, cooling the 4-bromodiphenyl ether until the 4-bromodiphenyl ether is solidified and stabilized, then heating the 4-bromodiphenyl ether, heating the 4-bromodiphenyl ether to 40 DEG C at a heating rate of 0.5-1.0 K / min, and calculating the purity of the 4-bromodiphenyl ether according to a melting peak area; randomly selecting at least ten parts of 4-bromodiphenyl ether samples, testing each part of sample for at least two times according to the method, and calculating purity results; and performing normal distribution test and abnormal value test on the purity results to correct the purity results, and taking the average value of the corrected purity results, namely a purity constant value. The 4-brominated diphenyl ether purity valuing method provided by the invention provides a method basis for research on standard substances of brominated flame retardants such as the 4-brominated diphenyl ether, and ensures the traceability of measurement.

Description

technical field [0001] The invention belongs to the technical field of measurement, and relates to a method for determining the purity of organic matter, in particular to a method for determining the purity of 4-bromodiphenyl ether. Background technique [0002] Polybrominated diphenyl ethers are a class of brominated flame retardants (PBDEs), which are widely used in various industrial and daily products due to their excellent flame retardancy. However, studies in recent years have shown that PBDEs are a class of persistent organic pollutants (Persistent Organic Pollutants, POPs) that are ubiquitous in the global environment and have been included in the Stockholm Convention. [0003] Due to the different substitution positions and numbers of bromine, polybrominated diphenyl ethers are a series of compounds, 4-bromodiphenyl ether is one of them, and the molecular formula is C 12 h 9 OBr, CAS101-55-3, melting point 18°C, boiling point 305°C. 4-Bromodiphenyl ether has a lo...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N5/00G01N30/02G01N30/72
CPCG01N5/00G01N30/02G01N30/72
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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