CN113433250A - Device and method for measuring water content in hexafluorobutadiene - Google Patents
Device and method for measuring water content in hexafluorobutadiene Download PDFInfo
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- CN113433250A CN113433250A CN202110921790.7A CN202110921790A CN113433250A CN 113433250 A CN113433250 A CN 113433250A CN 202110921790 A CN202110921790 A CN 202110921790A CN 113433250 A CN113433250 A CN 113433250A
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- 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
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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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- G01N30/64—Electrical detectors
- G01N30/68—Flame ionisation detectors
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Abstract
The invention provides a device for measuring the water content in hexafluorobutadiene, which comprises a gas chromatograph, wherein a sample injection valve, a chromatographic column and a hydrogen flame ionization detector are arranged in the gas chromatograph, the front end of a sample injection port of the gas chromatograph is connected with a filter, and the front end of the filter is connected with a water content converter. The invention also provides a method for determining the water content in the hexafluorobutadiene by using the gas chromatograph, which comprises the following steps: s1, connecting a pipeline; s2, establishing a standard curve; and S3, measuring the sample. Also provided is a device for measuring water content. The method can accurately detect the moisture in the hexafluorobutadiene, is simple to operate, establishes an analysis method of the moisture in the hexafluorobutadiene, and provides technical guarantee for the stable quality of the hexafluorobutadiene.
Description
Technical Field
The invention belongs to the technical field of detection of hexafluorobutadiene, and particularly relates to a device and a method for determining water content in hexafluorobutadiene.
Background
The hexafluorobutadiene is a dry etching gas with excellent etching performance and environmental protection, and is widely applied to the production process of large-scale integrated circuits and high-speed high-capacity memory chips. The moisture index in the hexafluorobutadiene brings serious influence on the optimization and promotion of integrated circuit and chip processes, so that the establishment of a reliable analysis technology for moisture in the hexafluorobutadiene is the key for ensuring the quality of the hexafluorobutadiene product.
At present, the current national standard has three methods for measuring trace moisture in gas: dew point, electrolytic and cavity ring down methods. Among them, the dew point method is simple to operate, but hexafluorobutadiene reacts with alumina to damage instruments, so that the dew point method cannot meet the requirements. For the electrolytic method and the cavity ring-down method, since hexachlorobutadiene has a boiling point of 6 ℃, it is easily liquefied to contaminate the hydrogen flame ionization detector, and thus the electrolytic method and the cavity ring-down method are not suitable.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method and a device for measuring the water content in hexafluorobutadiene, aiming at the defects of the prior art, wherein the method and the device are simple to operate, accurate in detection and high in academic research value, provide technical support for the quality improvement of the hexafluorobutadiene and meet the requirements of high-efficiency and rapid analysis in industrial production.
In order to solve the technical problems, the invention adopts the technical scheme that:
the utility model provides a device of method of survey hexafluorobutadiene water content which characterized in that, includes gas chromatograph, filter and moisture converter, be provided with injection valve, chromatographic column and hydrogen flame ionization detector in the gas chromatograph, the last introduction port that is provided with of gas chromatograph, the filter is passed through to the one end of introduction port and is connected moisture converter, and the introduction valve is connected to the other end of introduction port, moisture converter passes through the pressure reducer and connects the steel bottle that is equipped with hexafluorobutadiene standard gas and the sample that awaits measuring of hexafluorobutadiene, the chromatographic column is connected with injection valve and hydrogen flame ionization detector respectively.
Preferably, the water content converter is a stainless steel pipe with a length of 20-30 cm, the outer diameter of the middle part of the water content converter is 10mm, the outer diameters of the two end parts of the water content converter are 4mm, the lengths of the two end parts of the water content converter are both 3cm, the calcium carbide powder with a thickness of 0.08-0.25mm is filled in the middle part of the water content converter, and the glass fiber is filled in the two end parts of the water content converter.
Preferably, a plurality of filtering holes are uniformly distributed on the filter, and the pore diameter of each filtering hole is smaller than 0.5 μm. A method for determining the water content in hexafluorobutadiene by using a gas chromatograph is characterized by comprising the following steps:
s1, connecting pipeline: sequentially connecting a hexafluorobutadiene standard gas steel cylinder containing water with different concentrations and a hexafluorobutadiene sample steel cylinder to be detected to a sample inlet of a gas chromatograph through a pressure reducer, a moisture converter and a filter;
s2, establishing a standard curve: when a hexachlorobutadiene standard gas containing water with different concentrations and a hexachlorobutadiene sample to be detected pass through a water content converter, water and calcium carbide powder generate organic gas acetylene, then a gas chromatograph is used for testing the hexachlorobutadiene standard gas containing acetylene with different concentrations to obtain a chromatogram of the hexachlorobutadiene standard gas containing acetylene with different concentrations, finally, a standard curve of water content is established by taking the water concentration as a horizontal coordinate and the peak area of the chromatogram as a vertical coordinate, and the slope is calculated to be a correction coefficient;
s3, determining the water content of the sample to be tested of the hexafluorobutadiene: and testing the hexafluorobutadiene sample to be tested by using a gas chromatograph to obtain a chromatogram of the hexafluorobutadiene sample to be tested, and acquiring the peak area of the hexafluorobutadiene sample to be tested according to the chromatogram of the hexafluorobutadiene sample to be tested, wherein the water content of the hexafluorobutadiene sample to be tested is the correction coefficient multiplied by the peak area of the sample to be tested.
Preferably, three kinds of hexafluorobutadiene standard gases containing water at different concentrations are selected in S1, and the water concentrations of the three kinds of hexafluorobutadiene standard gases are 3ppm, 4ppm, and 5ppm, respectively.
Preferably, the chromatographic conditions employed by the gas chromatograph are: high-purity nitrogen with carrier gas flow of 35 mL/min; hydrogen with a combustion gas flow of 35 mL/min; the flow of combustion-supporting air is 400mL/min of air; a 3A molecular sieve chromatographic column with the chromatographic column temperature of 80 ℃; the hydrogen flame ionization detector temperature was 120 ℃.
Compared with the prior art, the invention has the following advantages:
1. the method can accurately detect the moisture in the hexafluorobutadiene, is simple to operate, establishes an analysis method of the moisture in the hexafluorobutadiene, and provides technical guarantee for the quality of the hexafluorobutadiene.
2. The moisture converter can effectively and quickly convert moisture in a sample to be detected into acetylene gas; the filter can effectively prevent particles from entering the chromatographic system, thereby reducing the blockage of the sample injection valve. The water content converter is filled with 0.08-0.25mm calcium carbide powder; the water converter is a stainless steel pipe with the length of about 25cm, the outer diameter of the middle part is 10mm, and the outer diameters of the two ends are 4mm and 3 cm; glass fiber is filled at two ends respectively to prevent the flowing leakage of the calcium carbide powder.
3. The gas chromatography is a chromatographic technique which uses gas as a mobile phase and separates and analyzes a mixture which is easy to volatilize but not decomposed by utilizing the difference of the distribution coefficients of components in a stationary phase and the mobile phase. In addition, water can react with the calcium carbide black solid to generate calcium hydrocarbonate white solid and acetylene gas, the reaction is rapid, and the conversion rate is high. Therefore, we can convert water into organic gas, and test the content of the organic gas by gas chromatography, thereby obtaining the water content. Based on the invention, a method for measuring the water content in the hexafluorobutadiene by using a gas chromatography method is designed.
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Drawings
FIG. 1 is a schematic view of the structure of the apparatus of the present invention.
Description of reference numerals:
1-gas chromatograph; 2-a sample injection valve; 3-chromatographic column;
4-hydrogen flame ionization detector; 5-a sample inlet; 6, a filter;
7-a moisture converter; 8-a pressure reducer; 9-steel cylinder.
Detailed Description
Example 1
As shown in figure 1, a device of water content in survey hexafluorobutadiene, including gas chromatograph 1, filter 6 and moisture converter 7, be provided with injection valve 2, chromatographic column 3 and hydrogen flame ionization detector 4 in the gas chromatograph 1, be provided with introduction port 5 on the gas chromatograph 1, filter 6 connection moisture converter 7 is passed through to introduction port 5's one end, and injection valve 2 is connected to introduction port 5's the other end, moisture converter 7 passes through pressure reducer 8 and connects the steel bottle 9 that is equipped with hexafluorobutadiene standard gas and the sample that awaits measuring of hexafluorobutadiene, chromatographic column 3 is connected with injection valve 2 and hydrogen flame ionization detector 4 respectively.
In this embodiment, the water content converter 7 is a stainless steel pipe with a length of 20 to 30cm, the outer diameter of the middle part of the water content converter 7 is 10mm, the outer diameters of the two end parts of the water content converter 7 are 4mm, the lengths of the two end parts of the water content converter 7 are both 3cm, the calcium carbide powder with a thickness of 0.08 to 0.25mm is filled in the middle part of the water content converter 7, and the glass fiber is filled in both end parts of the water content converter 7.
In this embodiment, a plurality of filtering holes are uniformly distributed on the filter 6, and the aperture of each filtering hole is smaller than 0.5 μm.
Example 2
The method for measuring the water content in hexafluorobutadiene using the apparatus for measuring the water content in hexafluorobutadiene disclosed in example 1, comprising the steps of:
s1, presetting and connecting pipelines: a hexafluorobutadiene standard gas steel cylinder 9 and a hexafluorobutadiene sample steel cylinder 9 with water concentrations of 3ppm, 4ppm and 5ppm are connected in parallel to a pressure reducer 8 through pipelines, the pressure reducer 8 is connected to an injection port 5 of a gas chromatograph 1 through a water converter 7 and a filter 6 in sequence, the gas chromatograph 1 is opened, and high-purity nitrogen with carrier gas flow of 35mL/min is arranged in the gas chromatograph; hydrogen with a combustion gas flow of 35 mL/min; the flow of combustion-supporting air is 400mL/min of air; a 3A molecular sieve chromatographic column with the chromatographic column temperature of 80 ℃; the temperature of the hydrogen flame ionization detector is 120 ℃;
s2, establishing a standard curve: and opening a steel cylinder valve of the standard gas, adjusting the pressure, continuously purging the pipeline for 10-30min through the standard gas to fully replace the pipeline, switching the sample injection valve 2 to inject the sample, and measuring and recording the peak area. Repeating the above operations to obtain chromatograms and peak areas of water concentrations of different standard gases, establishing a standard curve of water by taking the water concentration as a horizontal coordinate and the peak area as a vertical coordinate, and calculating the slope of the standard curve, namely the correction coefficient;
s3, determining the water content of the sample to be tested of the hexafluorobutadiene: opening a cylinder valve of a sample to be measured of the hexafluorobutadiene, adjusting the pressure, continuously flushing the pipeline for 10-30min by using gas to be measured to fully replace the pipeline, switching a sample injection valve 2 for sample injection, measuring and recording the peak area, and calculating the water content of the sample to be measured of the hexafluorobutadiene according to a calculation formula, wherein the water content of the sample to be measured of the hexafluorobutadiene is equal to a correction coefficient multiplied by the peak area of the sample to be measured. The water content of the hexafluorobutadiene gas is in the range of 2 to 5 ppm.
To reduce the calculation error, repeating the steps S1-S3 twice to obtain three sets of test data, which are summarized to obtain the results shown in the following Table 1:
| test No.) | Test No. two | Experiment three | |
| Correction factor | 0.0024 | 0.0023 | 0.0025 |
| Peak area of sample to be measured | 1235.7 | 1243.4 | 1202.1 |
| Water content (ppm) of sample to be tested | 2.97 | 2.86 | 3.01 |
TABLE 1
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (6)
1. The device for measuring the water content in the hexafluorobutadiene is characterized by comprising a gas chromatograph (1), a filter (6) and a water converter (7), a sample injection valve (2), a chromatographic column (3) and a hydrogen flame ionization detector (4) are arranged in the gas chromatograph (1), the gas chromatograph (1) is provided with a sample inlet (5), one end of the sample inlet (5) is connected with a moisture converter (7) through a filter (6), calcium carbide powder is filled in the moisture converter (7), the other end of the sample inlet (5) is connected with a sample injection valve (2), the water converter (7) is connected with a steel cylinder (9) filled with a hexafluorobutadiene standard gas and a hexafluorobutadiene sample to be tested through a pressure reducer (8), the chromatographic column (3) is respectively connected with the sample injection valve (2) and the hydrogen flame ionization detector (4).
2. The apparatus for determining the water content in hexafluorobutadiene as claimed in claim 1, wherein the water converter (7) is a stainless steel tube having a length of 20 to 30cm, the outer diameter of the middle portion of the water converter (7) is 10mm, the outer diameters of the two end portions of the water converter (7) are 4mm, the lengths of the two end portions of the water converter (7) are 3cm, the middle portion of the water converter (7) is filled with calcium carbide powder having a thickness of 0.08 to 0.25mm, and the two end portions of the water converter (7) are filled with glass fiber.
3. The device for measuring the water content in the hexafluorobutadiene as claimed in claim 1, wherein a plurality of filtering holes are uniformly distributed on the filter (6), and the pore diameter of the filtering holes is less than 0.5 μm.
4. A method for determining the water content of hexafluorobutadiene using the apparatus of claim 1, 2 or 3, comprising the steps of:
s1, connecting pipeline: a hexafluorobutadiene standard gas steel cylinder (9) containing water with different concentrations and a hexafluorobutadiene sample steel cylinder (9) to be detected are connected to a sample inlet (5) of a gas chromatograph (1) through a pressure reducer (8), a moisture converter (7) and a filter (6) in sequence;
s2, establishing a standard curve: when a hexachlorobutadiene standard gas containing water with different concentrations and a hexachlorobutadiene sample to be detected pass through a moisture converter (7), water and calcium carbide powder generate organic gas acetylene, a gas chromatograph (1) is used for testing the hexachlorobutadiene standard gas containing acetylene with different concentrations to obtain a chromatogram of the hexachlorobutadiene standard gas containing acetylene with different concentrations, finally, a standard curve of water content is established by taking the water concentration as a horizontal coordinate and the peak area of the chromatogram as a vertical coordinate, and the slope is calculated to be a correction coefficient;
s3, determining the water content of the sample to be tested of the hexafluorobutadiene: the method comprises the steps of testing a hexafluorobutadiene sample to be tested by using a gas chromatograph (1) to obtain a chromatogram of the hexafluorobutadiene sample to be tested, and obtaining the peak area of the hexafluorobutadiene sample to be tested by using the chromatogram of the hexafluorobutadiene sample to be tested, wherein the water content of the hexafluorobutadiene sample to be tested is equal to a correction coefficient multiplied by the peak area of the sample to be tested.
5. The method of claim 4, wherein three kinds of hexafluorobutadiene standard gases containing water at different concentrations are selected from S1, and the water concentrations of the three kinds of hexafluorobutadiene standard gases are 3ppm, 4ppm and 5ppm, respectively.
6. The method for determining the water content in hexafluorobutadiene as claimed in claim 4, wherein the chromatographic conditions of the test by gas chromatograph are as follows: high-purity nitrogen with carrier gas flow of 35 mL/min; hydrogen with a combustion gas flow of 35 mL/min; the flow of combustion-supporting air is 400mL/min of air; a 3A molecular sieve chromatographic column with the chromatographic column temperature of 80 ℃; the hydrogen flame ionization detector temperature was 120 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115266984A (en) * | 2022-07-29 | 2022-11-01 | 格力电器（芜湖）有限公司 | Method for detecting moisture of refrigerant in real time |
| WO2024103613A1 (en) * | 2022-11-16 | 2024-05-23 | 福建省杭氟电子材料有限公司 | Quality inspection system and method for electronic-grade hexafluorobutadiene |
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