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Method for determining purity and impurity content of 1,3,3,3-tetrafluoropropene product by gas chromatography

A technology of gas chromatography and tetrafluoropropene, which is applied in the field of analysis and determination of fluorine-containing olefin products and their impurities, and can solve problems such as difficult separation

Active Publication Date: 2019-11-12
ZHEJIANG RES INST OF CHEM IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the research and production of 1,3,3,3-tetrafluoropropene (HFO-1234ze(Z)), the product purity and main impurities of 1,3,3,3-tetrafluoropropene (HFO-1234ze(Z)) The content is an important factor affecting product quality. According to different processes, there may be nearly 20 kinds of impurities with similar properties, which are not easy to separate

Method used

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  • Method for determining purity and impurity content of 1,3,3,3-tetrafluoropropene product by gas chromatography
  • Method for determining purity and impurity content of 1,3,3,3-tetrafluoropropene product by gas chromatography
  • Method for determining purity and impurity content of 1,3,3,3-tetrafluoropropene product by gas chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] A 7890A gas chromatograph and FID detector from Agilent were used.

[0042]Test sample preparation: Inject 2.05g of HFO-1234ze(Z) sample into a 1L vacuum-treated air bag, inject 0.4ml methane, 5ml R116, 0.2ml R115, 0.2ml R1216, 0.2ml R143a, 0.2ml with a sealed syringe R1234yf, 0.2ml R114, 0.2ml R114a, 0.2ml 3,3,3-trifluoropropyne, 1.0ml R1112, 0.2ml R245cb, 0.2mlR1234ze(E), 0.5ml R1233xf, 0.2ml R124, 0.5ml R1233zd(Z ), 0.2ml R133a, 0.2ml R245fa, 0.2ml R245eb, the operating environment of the above gases and the background gas should be consistent.

[0043] Select the chromatographic conditions as follows:

[0044]

[0045] The prepared sample to be tested is carried by the carrier gas through the selected chromatographic column, and the components are separated by different partition coefficients between the mobile phase (carrier gas) and the stationary phase in the chromatographic column. Enter the detector; different substances have different characteristics, and...

Embodiment 2

[0050] A 7890A gas chromatograph and FID detector from Agilent were used.

[0051] Test sample preparation: Inject HFO-1234ze(Z) into a 1L vacuum-treated air bag as background gas, inject methane and appropriate amount of impurities into a sealed syringe including: R115, R1216, R143a, R1234yf, R114, R114a, 3, 3,3-Trifluoropropyne, R1112, R245cb, R1234ze(E), R1233xf, R124, R1233zd(Z), R133a. The operating environment of the above-mentioned gases and the background gas shall be consistent. Select the same chromatographic conditions as in Example 1 to analyze, and the chromatogram is detailed in the attached description image 3 .

[0052] The content of each impurity is calculated as follows. First use (2) (3) correction formula to correct the R1234ze(E) and R1234ze(Z) peak areas, and then use (1) area normalization method to calculate, the results are as follows:

[0053]

[0054]

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Abstract

The invention discloses a method for determining impurities in a 1,3,3,3-tetrafluoropropene product by gas chromatography. Chromatographic conditions include an Al2O3 capillary column [(10-200)mx(200-600)[mu]mx(0.2-20)[mu]m)] and the like. The method provided by the invention can be used for qualitatively and quantitatively analyzing the purity and impurity content of the 1,3,3,3-tetrafluoropropene product.

Description

technical field [0001] The invention relates to a method for analyzing and measuring fluorine-containing olefin products and impurities thereof, in particular to a method for measuring the purity of 1,3,3,3-tetrafluoropropene products and the content of impurities thereof by gas chromatography. Background technique [0002] Ozone layer depletion and global warming are two major global environmental issues facing the international community. The research, development and production of a new generation of ODS substitutes with zero ODP and low GWP has become a hot spot of common concern. The ODP value of fluorinated olefins (HFOs) is zero, and the GWP value is also extremely low. When directly emitted, CO 2 The emission reduction rate is greater than 99%, and it has good environmental performance. It is the most important variety for the development of a new generation of ODS substitutes. [0003] As a representative of fluoroolefins (HFOs) products, 1,3,3,3-tetrafluoropropene...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 史婉君张建君潘晋亨徐娇鬲春丽
Owner ZHEJIANG RES INST OF CHEM IND CO LTD
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