CN111579669B - Method for analyzing and measuring hexafluoroacetone content - Google Patents
Method for analyzing and measuring hexafluoroacetone content Download PDFInfo
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- CN111579669B CN111579669B CN202010453325.0A CN202010453325A CN111579669B CN 111579669 B CN111579669 B CN 111579669B CN 202010453325 A CN202010453325 A CN 202010453325A CN 111579669 B CN111579669 B CN 111579669B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/52—Physical parameters
- G01N30/54—Temperature
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/68—Flame ionisation detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
Abstract
The invention discloses an analytical determination method for hexafluoroacetone content. Performing gas chromatography analysis on hexafluoroacetone, and directly and quantitatively determining the content of the hexafluoroacetone by an area normalization method, wherein the chromatographic conditions during detection are as follows: the chromatographic column is a nonpolar column; temperature of the column: 40-200 ℃; sample inlet temperature: 60-140 ℃; detector temperature: 250-300 ℃; carrier gas: high-purity nitrogen; flow rate of carrier gas: 0.8-1.5mL/min; the split ratio is as follows: 30-100 parts of; operating time: 20min, pre-column pressure: 13Psi; sample introduction amount: 0.1-1.0mL. The detector is a hydrogen flame detector. The chromatographic analysis method for directly and quantitatively determining the purity in the production of the hexafluoroacetone has the advantages of reliable result, simple operation and lower test price, is suitable for enterprises to carry out conventional analysis, has higher practical value, and can be used for guiding the research of the hexafluoroacetone and the detection of the production process.
Description
Technical Field
The invention relates to an analytical determination method for hexafluoroacetone content, belonging to the field of chemical analysis.
Background
Hexafluoroacetone is an important industrial fluorine-containing compound, is prepared by isomerizing hexafluoropropylene oxide, and is an important intermediate for synthesizing organic fluorine compounds. It has been widely used in high-tech fields such as medicine, pesticide, textile, aerospace, microelectronics, synthetic materials and the like, for example, as a monomer for preparing synthetic resin, synthetic rubber and the like, or as an intermediate of a crosslinking agent such as bisphenol AF and the like. Impurities with a boiling point very close to that of hexafluoroacetone are generated in the production process, and the presence of the impurities affects the quality of downstream products, so that high-purity hexafluoroacetone is required in the production. Therefore, the method has great significance for the research on the preparation of the hexafluoroacetone.
The method for synthesizing hexafluoroacetone, which is researched more and has the most industrialized prospect, takes hexafluoropropylene oxide as a raw material, but the boiling points of the two substances are very close (hexafluoropropylene oxide is-27.0 ℃, and hexafluoroacetone is-27.4 ℃), so that great technical problems are brought to later-stage separation. Therefore, the research on the gas chromatography analysis method of the mixed gas of the hexafluoroacetone and the hexafluoropropylene oxide has positive significance for evaluating the advantages and disadvantages of different solid catalysts and controlling the synthesis conditions. However, it is difficult to perform quantitative analysis by infrared analysis and nuclear magnetic resonance, and the price of the instrument is expensive, so that it is not suitable for mass production for routine analysis. Through repeated tests, a rapid and accurate analysis method for hexafluoropropylene oxide and hexafluoroacetone is screened out.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an analytical determination method of hexafluoroacetone content. The gas chromatography analysis measuring method for directly and quantitatively measuring the content of the hexafluoroacetone has reliable result and simple operation, and can be used for guiding research and production process detection of the hexafluoroacetone.
The technical scheme of the invention is as follows:
a method for analyzing and measuring the content of hexafluoroacetone is characterized in that the hexafluoroacetone is analyzed by gas chromatography, the content of the hexafluoroacetone is directly and quantitatively measured by an area normalization method, and the chromatographic conditions during detection are as follows: the chromatographic column is a nonpolar column; temperature of the column: 40-200 ℃; sample inlet temperature: 60-140 ℃; temperature of the detector: 250-300 ℃; carrier gas: high-purity nitrogen; carrier gas flow rate: 0.8-1.5mL/min; the split ratio is as follows: 30-100 parts of; operating time: 20min, pre-column pressure: 13Psi; sample introduction amount: 0.1-1.0mL.
According to the invention, it is preferred that:
the detector is preferably a hydrogen flame detector.
The chromatographic column is HP-INNOWAx, has a length of 30m, an inner diameter of 0.32mm, and a liquid membrane thickness of 0.25um.
The amount of the hexafluoroacetone sample was 0.8mL.
The temperature of the chromatographic column is programmed temperature rise, the initial temperature is 80 ℃, the temperature is kept for 1-2min, and the temperature is raised to 180 ℃ at the speed of 20 ℃/min and then kept for 5min.
The inlet temperature is preferably 100 ℃ and the detector temperature is preferably 300 ℃.
The split ratio is preferably 50:1.
the chromatograph for gas chromatographic analysis is 7890B chromatograph produced by Agilent USA.
The gas chromatography quantitative analysis adopts an area normalization method, and the content formula of hexafluoroacetone is as follows: hexafluoroacetone (%) = a/Σ a,
in the formula: a is the peak area of hexafluoroacetone, and Σ A is the total area of the respective peaks.
The invention has the advantages that:
the chromatographic analysis measuring method for directly and quantitatively measuring the purity in the production of the hexafluoroacetone selects and utilizes gas chromatography to detect according to the product characteristics, selects the strong polarity chromatographic column bonded with the polyethylene glycol stationary phase and utilizes the characteristic of the highest temperature upper limit of the polyethylene glycol stationary phase, has simple operation, lower test price and reliable result, is suitable for enterprises to carry out conventional analysis, has higher practical value and can be used for guiding the research and the production process detection of the hexafluoroacetone.
Drawings
FIG. 1 is a chromatogram of hexafluoroacetone in example 1, with time on the abscissa and peak on the ordinate. Wherein 1.377min is hexafluoropropylene oxide, 2.904min is hexafluoroacetone (peak top).
Detailed Description
The present invention is further illustrated by, but not limited to, the following examples. The examples are not specifically described in the prior art.
Example 1:
the method of the invention is adopted to measure the content of hexafluoroacetone in two samples: wherein, the 'I' is hexafluoroacetone with the purity of more than 98.0 percent produced by Shandong China Shenzhou New Material Co. "II" is hexafluoroacetone produced by the future hydrogen energy materials Limited in east of Shandong.
1.1 Instrument
7890B chromatograph manufactured by Agilent USA.
1.2 chromatographic conditions
A detector: a hydrogen flame detector;
a chromatographic column: HP-INNOwax; column length: inner diameter of 30 m: 0.32mm, liquid film thickness: 0.25um;
column temperature: and (3) temperature programming, wherein the initial temperature is 80 ℃, the temperature is kept for 1-2min, then the temperature is increased by 20 ℃ per minute, and the temperature is kept for 5min after being increased to 180 ℃.
Sample inlet temperature: 100 ℃;
detector temperature: 300 ℃;
carrier gas: high-purity nitrogen;
flow rate of carrier gas: 1.2mL/min;
the split ratio is as follows: 50;
operating time: 20min
Pressing the column in front: 13Psi;
sample introduction amount: 0.8mL;
1.3 sample analysis
Because the sample is very volatile, the attention action is rapid when the sample is injected. 0.8mL of the sample was sampled quickly and subjected to chromatography, and the hexafluoroacetone content was determined by the following formula.
Hexafluoroacetone (%) = a/Σ a, in which: a is the peak area of hexafluoroacetone, and Σ A is the total area of the respective peaks.
As shown in fig. 1, the peak area of hexafluoroacetone is 14187, and the peak area of other carbonyl fluorides and hexafluoropropylene oxide is 240, so that the content of hexafluoroacetone is: the peak area of hexafluoroacetone/(peak area of hexafluoroacetone + peak area of carbonyl fluoride and hexafluoropropylene oxide) = 14187/(14187 + 240) =98.333%.
The following is a comparison of results obtained by the method of this example for nine consecutive determinations of each of the two samples. As is clear from the results of the analysis of the samples in Table 1, the method can provide relatively stable analysis results.
TABLE 1 comparison of results of nine consecutive determinations of samples
Note: the "measured value" is the result of analysis by the analysis method of the present invention.
The "average value" is the average result of the analysis results of nine consecutive injections.
The "relative average deviation" is a percentage of the average of the absolute values of the absolute deviations of the respective measurements in the average of the respective measurements. It is used to express the reliability of the analysis result, and can represent the mutual closeness of the values obtained by the same sample in a plurality of measurements.
Example 2: selection experiment of chromatographic conditions
The capillary chromatographic columns, which had been aged and had a liquid film thickness of 0.25um, of HP-5, CP-PLOTQ, HP-INNOwax, respectively, were mounted on an Agilent 7890B chromatograph, and the results of the resolution tests were carried out at different column temperatures, as shown in Table 2. The HP-5, CP-PLOTQ, HP-INNOwax are of the type of chromatographic column.
TABLE 2 degree of separation of liquid film thickness 0.25um at different temperatures for chromatography columns
Note: the separation degree can indicate the condition that all components are separated from each other in the chromatographic column, when the separation degree is more than 1.5, two adjacent chromatographic peaks can be completely separated, the separation degree is good, and the measurement result can have good enough parallelism and accuracy.
"- - - -" means that the peak could not be separated.
In summary, it can be seen that HP-INNOwax was chosen with a liquid film of 0.25um, with the best degree of separation at an initial column temperature of 80 ℃.
Claims (6)
1. The method for analyzing and measuring the content of the hexafluoroacetone is characterized in that the hexafluoroacetone is subjected to gas chromatography, the content of the hexafluoroacetone is directly and quantitatively measured by an area normalization method, and the chromatographic conditions during detection are as follows: temperature of the column: 40-200 ℃; the temperature of the chromatographic column is programmed temperature rise, the initial temperature is 80 ℃, the temperature is kept for 1-2min, and the temperature is raised to 180 ℃ at the speed of 20 ℃/min and then kept for 5min; sample inlet temperature: 60-140 ℃; temperature of the detector: 250-300 ℃; carrier gas: high-purity nitrogen; flow rate of carrier gas: 0.8-1.5mL/min; the split ratio is as follows: 30-100 parts of; operating time: 20min, pre-column pressure: 13Psi; sample introduction amount: 0.1-1.0mL;
the chromatographic column type be HP-INNOWAx, chromatographic column length is 30m, the internal diameter is 0.32mm, liquid film thickness is 0.25um, the detector is the hydrogen flame detector.
2. The method for the analytical measurement of hexafluoroacetone content as claimed in claim 1, wherein the amount of the hexafluoroacetone sample is 0.8mL.
3. The method for analyzing and measuring hexafluoroacetone content as claimed in claim 1, wherein the injection port temperature is 100 ℃ and the detector temperature is 300 ℃.
4. The method for the analytical determination of the hexafluoroacetone content as claimed in claim 1, wherein the split ratio is 50:1.
5. the method according to claim 1, wherein the chromatograph for gas chromatography is 7890B, agilent.
6. The method for analyzing and measuring hexafluoroacetone content as claimed in claim 1, wherein said gas chromatography quantitative analysis is area normalization, and the hexafluoroacetone content formula is: hexafluoroacetone (%) = a/Σ a, in which: a is the peak area of hexafluoroacetone, and Σ A is the total area of the respective peaks.
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