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Method for measuring impurity content in methylhydrazine

A technology for rapid determination of impurity content, applied in the field of analytical chemistry, can solve problems such as inability to measure the impurity content of methyl hydrazine, and achieve the effects of overcoming long time, small relative error and accurate determination results.

Inactive Publication Date: 2012-07-25
XIAN HANGJIE CHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the technical problem that the existing methylhydrazine analysis method can only measure the content of methylhydrazine, but cannot measure the content of various impurities in methylhydrazine, the purpose of the present invention is to provide a rapid determination of methylhydrazine The method of impurity content in hydrazine provides timely and effective reference data for the industrial production of methylhydrazine

Method used

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  • Method for measuring impurity content in methylhydrazine
  • Method for measuring impurity content in methylhydrazine
  • Method for measuring impurity content in methylhydrazine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] ① Instrument: The gas chromatograph is equipped with a thermal conductivity detector, a split / splitless inlet, and a capillary column of 60m×0.32mm×5μm.

[0024] ②Test conditions: manual injection; injection volume 1 μL; oven temperature 60°C, rear inlet temperature 250°C, rear detector temperature 250°C; split ratio 25:1; column temperature 60°C for 9 Minutes, the temperature was programmed to rise to 150°C at 20°C / min, and the temperature was kept constant for 2 minutes; the flow rate of the chromatographic column was 3ml / min; the carrier gas was high-purity helium.

[0025] ③ Gas phase detection of methylhydrazine sample 1 was carried out by the area percentage method.

[0026] Chromatograms such as figure 1 As shown, the results are shown in Table 1, and each component and retention time are shown in Table 1.

[0027] Table 1

[0028]

Embodiment 2

[0030] Utilize the content of impurity in the rapid determination of methylhydrazine by gas chromatography, comprising the following steps:

[0031] ① Instrument: The gas chromatograph is equipped with a thermal conductivity detector; the inlet is a split / splitless inlet; the capillary column is 60 m long, with an inner diameter of 0.32 mm and a film thickness of 5 μm.

[0032] ②Test conditions: manual injection; injection volume 1 μL; column oven temperature 70°C, rear inlet temperature 250°C, rear detector temperature 270°C; split ratio 25:1; column temperature 70°C for 9 Minutes, the temperature was programmed to rise to 150°C at 20°C / min, and the temperature was kept constant for 2 minutes; the flow rate of the chromatographic column was 3ml / min; the carrier gas was high-purity helium.

[0033] ③Using the area percentage method to quantitatively analyze the impurities therein.

[0034] The chromatogram of the methylhydrazine sample separated by the chromatographic column ...

Embodiment 3

[0038] ① Instrument: The gas chromatograph is equipped with a thermal conductivity detector, a split / splitless inlet, and a capillary column of 60m×0.32mm×5μm.

[0039] ②Test conditions: manual injection; injection volume 1 μL; column oven temperature 80°C, rear inlet temperature 250°C, rear detector temperature 300°C; split ratio 25:1; column temperature 80°C for 9 Minutes, the temperature was programmed to rise to 160°C at 20°C / min, and the temperature was kept constant for 2 minutes; the flow rate of the chromatographic column was 5ml / min; the carrier gas was high-purity helium.

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Abstract

The invention relates to a method for measuring the impurity content in methylhydrazine. The method comprises the steps of introducing samples, gasifying, separating, detecting and calculating the content of the impurities and the like. The method solves the technical problems that in the existing analysis method, only the content of the methylhydrazine can be measured, and the various impurity contents in the methylhydrazine cannot be measured, according to the method, the impurity content in the methylhydrazine can be detected simply and rapidly, the measuring result is accurate, and the relative error is less than 5%, and the method is suitable for control analysis of the quality of the methylhydrazine in the industrial production.

Description

technical field [0001] The invention belongs to the field of analytical chemistry and provides a method for quickly measuring the impurity content in methylhydrazine. Background technique [0002] Methylhydrazine is an important intermediate in organic synthesis, widely used in medicine, pesticides, dyes, aerospace fuels and other fields. In the synthetic process of methylhydrazine, there are often unreacted raw materials hydrazine hydrate, methanol, by-product ammonia, p-dimethylhydrazine and trimethylhydrazine. The level of these impurities affects the methylhydrazine to a large extent The mass of hydrazine. Therefore, the quantitative analysis of various impurities in methylhydrazine will provide accurate analytical data for production, which will help to better adjust the control conditions, improve the production process, and further improve the quality of methylhydrazine . [0003] At present, the analytical method for the purity of methylhydrazine only stipulates t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 王卫国吉卉郭友闫小宁马翔田建军李承柱陈卫民白海龙罗斌姚中东李军平陈帅何宇苏雪春许东兴杨玲王龙龙许峰李军锋张慧刘丽
Owner XIAN HANGJIE CHEM TECH
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