Analytical investigating method of tetrafluoro-propionic methyle ester methoxide

A technology for the determination of methyl methoxytetrafluoropropionate, which is applied in the field of analysis and determination of methyl methoxytetrafluoropropionate, can solve the problems of unsuitability for routine analysis of enterprises and expensive instruments, and achieve high practicality The effect of simple value and method

Inactive Publication Date: 2007-07-18
SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, it is difficult to quantitatively analyze it with infrared analysis and nuclear magnetic resonance, an

Method used

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  • Analytical investigating method of tetrafluoro-propionic methyle ester methoxide
  • Analytical investigating method of tetrafluoro-propionic methyle ester methoxide
  • Analytical investigating method of tetrafluoro-propionic methyle ester methoxide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: the analytical determination method of methyl methoxytetrafluoropropionate

[0018] 1.1 Instrument

[0019] American PE 500 chromatograph

[0020] 1.2 Chromatographic conditions

[0021] Detector: FID (Flame Ionization Detector)

[0022] Column: DB-200

[0023] Column length: ￠0.25*30m

[0024] Column temperature: 150°C

[0025] Injector: 180°C

[0026] Detector: 300°C

[0027] 1.3 Sample analysis

[0028] Quickly sample 1uL for chromatographic analysis, and obtain the content of methyl methoxytetrafluoropropionate according to the following formula.

[0029]

[0030] In the formula: A is the peak area of ​​methyl methoxy tetrafluoropropionate

[0031] ΣA is the total area of ​​each peak.

[0032] For example, in Figure 1, the peak area of ​​methyl methoxy tetrafluoropropionate is 5479771, the peak area of ​​methoxy octafluoropentanone is 27937, and the content of methyl methoxy tetrafluoropropionate is:

[0033]

[0034] The following is ...

Embodiment 2

[0043] Embodiment 2: the selection of chromatographic conditions

[0044] The capillary columns of DB-1, DB-200 and DB-624 with a liquid film of 0.32um and the well-aged packings coated with DNP, SE-52 and squalane on the Chromosob P.AW-DMCS support were respectively The column was installed on a PE500 chromatograph, and the separation test was carried out at different temperatures (column temperature). The results are shown in Table 2 and Table 3. The DB-1, DB-200 and DB-624 are chromatographic column types (capillary column), and DNP and SE-52 are dinonyl phthalate fixative and 5% phenyl elastomer fixative respectively.

[0045] Table 2 Resolution of capillary column at different temperatures

[0046] NOTE: Resolution indicates how well the components are separated from each other in the column. Adjacent two chromatographic peaks can be completely separated when the resolution is greater than 1.5. Only when the resolution is good can the measurement results have suffici...

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Abstract

The invention discloses methoxy-tetrafluoro-methyl propionate analyzing and measuring method. It includes the following steps: processing gas-chromatography analysis for the methoxy-tetrafluoro-methyl propionate; using area normalization to directly measure its content; chromatographic analysis temperature is 150 degree centigrade; chromatographic column type is DB-200; liquid membrane is 0.32um; detector is flame ionization. The invention has reliable result, simple operation, can be used to guide methoxy-tetrafluoro-methyl propionate study and production.

Description

technical field [0001] The invention relates to a method for analyzing and measuring methyl methoxytetrafluoropropionate. Background technique [0002] Methyl methoxytetrafluoropropionate is an important fluorine-containing synthetic intermediate. It is formed by the reaction of tetrafluoroethylene, dimethyl carbonate and sodium methoxide. During the reaction, methoxytetrafluoropropionic acid will be produced Methoxy octafluoropentanone with a boiling point very close to the methyl ester. Methoxy octafluoropentanone will seriously affect the quality of subsequent products, so high-purity methyl methoxy tetrafluoropropionate is required in production. However, it is difficult to quantitatively analyze it with infrared analysis and nuclear magnetic resonance, and the price of the instrument is relatively expensive, which is not suitable for routine analysis in enterprises. Contents of the invention [0003] Aiming at the deficiencies in the prior art, the invention provide...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/68G01N30/60
Inventor 董光辉张永明王梁房瑾
Owner SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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