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Method for analyzing and determining content of hexafluoroacetone
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A technology of hexafluoroacetone and its determination method, which is applied in the field of chemical analysis, can solve the problems of being unsuitable for large-scale production and expensive instruments, and achieve the effects of low test price, reliable results and high practical value
Active Publication Date: 2020-08-25
SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD
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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 large-scale production
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Embodiment 1
[0021] The method of the present invention is used to determine the content of hexafluoroacetone in two samples: wherein, "No. 1" is hexafluoroacetone with a purity greater than 98.0% produced by Shandong Huaxia Shenzhou New Material Co., Ltd. "No. II" is hexafluoroacetone produced by Shandong Dongyue Future HydrogenEnergy Materials Co., Ltd.
[0022] 1.1 Instrument
[0023] Agilent 7890B chromatograph produced in the United States.
[0026] Chromatographic column: HP-INNOwax; column length: 0.32mm*0.25μm*30m, liquid film thickness is 0.25um;
[0027] Column temperature: program temperature rise, the initial temperature is 80°C, keep for 1-2min, then increase by 20°C per minute, after rising to 180°C, keep for 5min.
[0046] Embodiment 2: the selection experiment of chromatographic conditions
[0047] The HP-5, CP-PLOTQ, and HP-INNOwax aging capillary columns with a liquid film thickness of 0.25um were installed on the Agilent 7890B chromatograph, and the separation test was carried out at different column temperatures. See Table 2. The HP-5, CP-PLOTQ, and HP-INNOwax are chromatographic column types.
[0048] Table 2 The resolution of the chromatographic column with a liquid film thickness of 0.25um at different temperatures
[0049]
[0050] Note: The resolution can indicate the separation of each component in the chromatographic column. When the resolution is greater than 1.5, the adjacent two chromatographic peaks can be completely separated. If the resolution is good, the measurement results can have sufficient parallelism and accuracy.
[0051] "----" means that the peak cannot be separated.
[0052] In summary, it can be seen that the HP-INNOwax with a liquid film of 0.25um is ...
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Abstract
The invention discloses a method for analyzing and determining the content of hexafluoroacetone. Hexafluoroacetone is subjected to gas chromatographic analysis, the content of hexafluoroacetone is directly and quantitatively determined by an area normalization method, and chromatographic conditions during detection are as follows: a chromatographic column is a non-polar column; the temperature ofa chromatographic column is 40-200 DEG C; the temperature of a sample inlet is 60-140 DEG C; the temperature of a detector is 250 to 300 DEG C; the carrier gas is high-purity nitrogen; the flow rate of carrier gas is 0.8 mL / min to 1.5 mL / min; the split ratio is (30-100): 1; the operation time is 20 min, and the pre-column pressure is 13 Psi; and the sample size is 0.1 to 1.0 mL. And the detector is a hydrogenflamedetector. The chromatographic analysis method for directly and quantitatively determining the purity of hexafluoroacetone in production has the advantages of reliable result, simpleoperation and low test price, is suitable for routine analysis of enterprises, has high practical value, and can be used for guiding the research and production process detection of hexafluoroacetone.
Description
technical field [0001] The invention relates to an analysis and determination method for the content of hexafluoroacetone, which belongs to the field of chemical analysis. Background technique [0002] Hexafluoroacetone is an important industrial fluorine-containing compound, which is formed by isomerization of hexafluoropropyleneoxide and is an important intermediate for the synthesis of organic fluorine compounds. It has been widely used in high-tech fields such as medicine, pesticide, textile, aerospace, microelectronics and synthetic materials. body. In the production process, impurities that are very close to the boiling point of hexafluoroacetone will be generated. Due to the existence of these impurities, the quality of downstream products will be affected, so high-purity hexafluoroacetone is required in production. Therefore, the research on the preparation of hexafluoroacetone also has great significance. [0003] At present, the method of synthesizing hexafluor...
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IPC IPC(8): G01N30/02G01N30/54G01N30/68G01N30/86
CPCG01N30/02G01N30/54G01N30/68G01N30/8675
Inventor 魏刚史翔张永超王一帆崔永文冯威张永明
Owner SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD
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