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A gas chromatography test method for 4-ethoxy-2,3-difluorobenzene

A gas chromatography and inspection method technology, applied in the field of gas chromatography inspection of 4-ethoxy-2,3-difluorobenzene, can solve the problem of inability to accurately guide process production, difficult substance component analysis, and unstable analysis results and other problems, to achieve the effect of stable peak value, fast analysis speed and stable peak time.

Active Publication Date: 2016-10-26
BENGBU CHINA SYNCHEM TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] After a long period of production practice and analysis of chromatograms, it is found that it is difficult to analyze the material components clearly and accurately with the DB-1 chromatographic column, resulting in unstable analysis results and unable to accurately guide normal process production

Method used

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  • A gas chromatography test method for 4-ethoxy-2,3-difluorobenzene
  • A gas chromatography test method for 4-ethoxy-2,3-difluorobenzene
  • A gas chromatography test method for 4-ethoxy-2,3-difluorobenzene

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Embodiment 1

[0031] Gas chromatographic analysis of industrially produced 4-ethoxy-2,3-difluorobenzene: Take industrially produced 4-ethoxy-2,3-difluorobenzene samples. Refer to the operating conditions to set the conditions of the gas chromatography. The oven temperature rise program: keep at 100°C for 1 minute, raise the temperature to 150°C for 1 minute at a rate of 10°C / min, then raise the temperature to 280°C for 5 minutes at a rate of 20°C / min; Inlet temperature: 250°C; detector temperature: 280°C; column flow rate: 1.0ml / min; chromatographic gas flow setting: hydrogen: 30ml / min, air: 300ml / min; carrier gas flow: 25ml / min; Ratio: 50 / 1; set the conditions of gas chromatography, after the baseline is stable, use a 10 μL micro-sampler to inject samples from the injection port, the injection volume is 0.2 μL, and after completing all the steps of the temperature program, use the workstation The purity of 4-ethoxy-2,3-difluorobenzene is calculated using the area normalization method of th...

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Abstract

The invention discloses a gas chromatography examination method of 4-ethoxy-2,3-difluorobenzene, and relates to the technical field of chemical analysis. The method comprises the following steps: setting the heating program of a column oven, the temperature of an injection port, the temperature of a detector, the flow of a chromatographic column and the gas flow of a chromatograph, introducing a sample, and calculating the purity of 4-ethoxy-2,3-difluorobenzene through an area normalization technique by using the integration function of an Agilent ChemStation chromatographic workstation. The temperature of the column oven adopts temperature programming, and two step temperature programming is adopted, so the analysis speed is fast, the analysis result is accurate, the production consumption is reduced, and the production cost is saved; and when an Agilent HP-5 capillary chromatographic column is used, the peak appearance time and the peak value of a material are stable, and the repeatability is good.

Description

Technical field: [0001] The invention relates to the technical field of chemical analysis, in particular to a gas chromatography test method for 4-ethoxy-2,3-difluorobenzene. Background technique: [0002] 4-Ethoxy-2,3-difluorobenzene 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-difluorobenzene disclosed in China is: 4-ethoxy-2,3-difluoronitrobenzene, hydrogenation reduction reaction, diazotization reaction, concentration and obtained by distillation. ...

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