A kind of analysis method of bromine content in industrial liquid chlorine
An analysis method and technology of bromine content, applied in the field of analytical chemistry, can solve the problems of high price, complicated operation, high maintenance cost and operation cost, and achieve the effects of high accuracy, simple operation and low harm
Active Publication Date: 2019-01-11
DALIAN BIO CHEM
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Problems solved by technology
[0004] In the existing literature reports, the bromine content in liquid chlorine can be determined by the inductively coupled plasma spectrophotometry ICP-AES method, but this method requires professional analytical instruments, which are expensive, have high maintenance and operating costs, and are complicated to operate; Therefore, how to choose a simple, fast, accurate, and low-cost determination technology for bromine content in liquid chlorine has become a technical problem in analysis and detection.
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[0018] The present invention will be further explained below in conjunction with specific examples.
[0019] ●Instruments and reagents
[0020] Instrument: Agilent 1260 high performance liquid chromatography (with VWD detector, automatic sampler, chemical workstation).
[0021] Reagents: methanol (chromatographic grade), distilled water, carbon tetrachloride (analytical grade), 2,6-dimethylphenol (analytical grade).
[0022] ●Column: ZORBAX XDB-C18, 150mm×4.6mm×5μm.
[0023] ●Detection wavelength: 275nm.
[0024] The analysis protocol steps are as follows:
[0025] 1) Sample chemical derivatization treatment:
[0026] Add about 60 milliliters of 10% concentration of 2,6-dimethylphenol carbon tetrachloride solution to the 250ml iodine measuring bottle in advance, cover and seal, and set aside;
[0027] Use a liquid chlorine sampler to collect a liquid chlorine sample at the liquid phase port of an industrial liquid chlorine steel cylinder, then add 2-3g of liquid chlorine ...
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The invention discloses a high performance liquid chromatography analysis method for determining the bromine content in industrial liquid chlorine. The method comprises the following steps: according to the characteristic that liquid chlorine and bromine can quickly and quantitatively perform aromatic ring electrophilic halogenating reaction with 2,6-dimethyl phenol, carrying out chemical derivation treatment on a liquid chlorine sample, carrying out quantitative detection on chloro(bromo) dimethyl phenol in the derivation treatment sample by using high performance liquid chromatography, and determining the bromine content in the industrial liquid chlorine according to the chlorine / bromine relative proportion obtained on the basis of the content of the chloro(bromo) dimethyl phenol. The analysis method can quickly and accurately determine the bromine content in industrial liquid chlorine, thereby providing a reliable analysis method for quality control on the liquid chlorine product.
Description
technical field [0001] The invention relates to a method for measuring bromine content in industrial liquid chlorine by using a derivatization method, belonging to the field of analytical chemistry. Background technique [0002] Industrial liquid chlorine is widely used in papermaking, textiles, pesticides, organic synthesis, metal smelting, chemical raw materials and other industries. With the application of liquid chlorine products in emerging fields more and more widely, some customers, especially some foreign high-end customers, found that bromine in liquid chlorine would affect the quality of their products, and proposed to limit the bromine content in liquid chlorine Require. [0003] At present, the national standard GB5138-2006 stipulates that the detection items of industrial liquid chlorine only include routine detection items such as purity, moisture, and nitrogen trichloride, and there are no detection requirements and methods for bromine content. [0004] In t...
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IPC IPC(8): G01N30/02G01N30/06G01N30/74G01N30/88
CPCG01N30/02G01N30/06G01N30/74G01N30/88G01N2030/067
Inventor 张晓娜顾振鹏李明王金凤王勇
Owner DALIAN BIO CHEM