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Gas chromatography detection method for benzotrichloride

A technology of trichlorotoluene and gas chromatography, which is applied in the field of analysis, can solve problems such as easy hydrolysis, difficulty in analysis, and smoke generation, and achieve the effects of fast analysis speed, low analysis cost, and good repeatability

Inactive Publication Date: 2016-04-06
SHANDONG KAISHENG NEW MATERIALS
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  • Application Information

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Problems solved by technology

[0002] Trichlorotoluene is a colorless transparent liquid with a special pungent smell, mainly produced by free radical chlorination substitution reaction of toluene and chlorine gas under light or a free radical initiator, fumes in the air, is unstable, and is easily hydrolyzed
[0004] Trichlorotoluene will produce a lot of by-product impurities such as monochlorine substitution, dichlorination substitution and benzene ring substitution in the production process, and the impurities have similar boiling points and little difference in polarity, which brings great difficulty to its analysis
At present, there is no unified inspection standard for the detection of chloromethylbenzene

Method used

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  • Gas chromatography detection method for benzotrichloride
  • Gas chromatography detection method for benzotrichloride
  • Gas chromatography detection method for benzotrichloride

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Embodiment 1

[0034] 1. Reagents and instruments

[0035] Reagents: trichlorotoluene and carbon tetrachloride (chromatographic grade) produced in industry.

[0036] Instruments: Agilent7820A gas chromatograph (with autosampler), Agilent OpenLAB workstation, AgilentDB-5 capillary column with a specification of 30m×0.32mm×0.25μm; hydrogen flame ionization detector.

[0037] 2. Detection steps

[0038] The gas chromatography detection method of described trichlorotoluene, comprises the steps:

[0039] (1) The trichlorotoluene sample of industrial production is miscible with carbon tetrachloride according to the volume ratio of 1:1;

[0040] (2) Set the working conditions of the gas chromatograph:

[0041] Chromatographic column: AgilentDB-5 capillary column;

[0042] Oven temperature: 150~240℃;

[0043] Injection port temperature: 280°C;

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Abstract

The invention belongs to the technical of analysis, and particularly relates to a gas chromatography detection method for benzotrichloride. The detection method comprises the steps that 1, a sample to be detected is dissolved with a solvent; 2, working conditions of a gas chromatograph are set, wherein an Agilent DB-5 capillary column is adopted as a chromatographic column, the column box temperature is 150-240 DEG C, the sample inlet temperature is 280 DEG C, the temperature of a detector is 300 DEG C, the flow rate of carrier gas of the chromatographic column is 1 mL / min, the air flow speed is 300 mL / min, the hydrogen flow speed is 30 mL / min, and the split ratio is 100:1; 3, an automatic sampler is used for sampling, and a chromatogram starts to be detected and recorded; 4, an area normalization method is used for calculating out the content of benzotrichloride. The gas chromatography detection method has the advantages of being high in analysis speed, accurate in result, low in analysis cost, capable of effectively and rapidly guiding production arrangement, and capable of accurately measuring the content of a benzotrichloride product.

Description

technical field [0001] The invention belongs to the technical field of analysis, and in particular relates to a gas chromatography detection method of trichlorotoluene. Background technique [0002] Trichlorotoluene is a colorless transparent liquid with a special pungent smell, mainly produced by free radical chlorination substitution reaction of toluene and chlorine gas under light or a free radical initiator, fumes in the air, is unstable, and is easily hydrolyzed . Trichlorotoluene has a melting point of -5°C and a boiling point of 220.8°C. [0003] Trichlorotoluene is mainly used as the basic raw material of dyes, pharmaceutical intermediates and ultraviolet absorbers UV-9 and UV-531. It is an important intermediate in organic synthesis and can be used to manufacture benzoic acid, benzoyl chloride, triphenyl Methyl methane dyes, anthraquinone dyes and quinoline dyes, etc. [0004] Trichlorotoluene will produce many by-product impurities such as monochlorine substitut...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/025
Inventor 宋立伟薛居强毕义霞张泰铭李文娟张聪聪
Owner SHANDONG KAISHENG NEW MATERIALS
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