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A kind of gas chromatography test method of 4-ethoxyl-2,3-difluorophenol

A technology of difluorophenol and gas chromatography, which is applied in the field of chemical analysis, can solve the problems of material composition analysis, unstable analysis results, inability to accurately guide process production, etc., and achieve fast analysis speed, stable peak value, and cost-saving production Effect

Active Publication Date: 2017-01-04
BENGBU CHINA SYNCHEM TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] After a long period of production practice and analysis of chromatograms, it was found that it was difficult to analyze the material components clearly and accurately with the HP-5 chromatographic column, resulting in unstable analysis results and unable to accurately guide normal process production

Method used

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  • A kind of gas chromatography test method of 4-ethoxyl-2,3-difluorophenol
  • A kind of gas chromatography test method of 4-ethoxyl-2,3-difluorophenol
  • A kind of gas chromatography test method of 4-ethoxyl-2,3-difluorophenol

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Embodiment 1

[0038] Gas chromatography analysis of industrially produced 4-ethoxy-2,3-difluorophenol: Take industrially produced 4-ethoxy-2,3-difluorophenol samples. Refer to the operating conditions to set the gas chromatographic conditions. The oven temperature rise program: keep at 80°C for 0 min, raise the temperature to 140°C for 0 min at a rate of 5°C / min, then raise the temperature to 280°C for 5 min at a rate of 20°C / min; Inlet temperature: 280°C; detector temperature: 300°C; column flow: 1.0ml / min; chromatographic gas flow setting: hydrogen: 40ml / min, air: 400ml / min; split ratio: 50 / 1; Set the conditions of the gas chromatography. After the baseline is stable, use a 10 μL micro-sampler to inject samples from the injection port. The injection volume is 1 μL. Function, using the area normalization method to calculate the purity of 4-ethoxy-2,3-difluorophenol; parallel measurement 4 times, the difference between any two parallel measurement results shall not be greater than 0.1%, the...

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Abstract

Relating to the technical field of chemical analysis, the invention discloses a gas chromatography test method for 4-ethoxy-2, 3-difluorophenol. The method includes: firstly setting a column temperature program, a sample inlet temperature, a detector temperature, a chromatographic column flow and chromatogram gas flow, then conducting sample introduction, and finally utilizing the integrating function of Shimadzu GCSOLUTION chromatographic work station to calculate the purity of 4-ethoxy-2, 3-difluorophenol by area normalization method. According to the invention, the column temperature adopts programmed temperature raising and employs a two-step temperature raising program, the analysis speed is fast, the result is accurate, the production consumption is reduced, the cost of production is saved. By using the Agilent DB-1 capillary chromatographic column, the peak flowing out time and peak value of materials are stable, and the repeatability is good.

Description

[0001] Technical field: [0002] The invention relates to the technical field of chemical analysis, in particular to a gas chromatography test method for 4-ethoxy-2,3-difluorophenol. [0003] Background technique: [0004] 4-Ethoxy-2,3-difluorophenol is a commonly used chemical raw material, which is used as a liquid crystal intermediate to make negative liquid crystal materials for display screens such as televisions and mobile phones. Liquid crystal display technology is one of the main display methods in the field of flat panel display, and it has been widely used in various display terminals. Therefore, with the development of liquid crystal display technology, the requirements for research and development of new liquid crystal materials are becoming more and more urgent. The preparation method of 4-ethoxy-2,3-difluorophenol disclosed in China is: 4-ethoxy-2,3-difluoronitrobenzene, hydrogenation reduction reaction, diazotization reaction, low temperature Obtained by borat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 杨青赵士民汪洪湖陈毛毛
Owner BENGBU CHINA SYNCHEM TECH CO LTD
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