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A kind of application method of vacuum sampling device for gas chromatograph
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A technology for a gas chromatograph and a sampling device, which is applied in the field of vacuum sampling devices for gas chromatographs, can solve problems such as interference analysis results, overloaded detector response, error in analysis results, etc. High and reduce the effect of analysis error
Inactive Publication Date: 2018-04-20
INST OF NUCLEAR PHYSICS & CHEM CHINA ACADEMY OF
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[0003] The sampling method of commercialized valve sampling system for gas samples is easy to operate and has good quantitative repeatability, but it is not suitable for sample injection analysis of normal pressure and negative pressure samples, and it is difficult to avoid the contamination of gas samples by ambient air, which will affect the analysis results. Interference, especially for the quantitative analysis of trace oxygen and nitrogen components in gas samples, the oxygen and nitrogen impurities in the air will seriously interfere with the analysis results
If the sampling method of the traditional purging method is used to remove the air in the sampling line, it will consume a lot of time and sample gas, and it is difficult to remove the impurities in the air.
In addition, the sampling method of the traditional valve sampling method cannot adjust the injection pressure. When measuring high-concentration sample components or low-concentration sample components, due to the overload or low response of the detector, it will cause large errors in the analysis results.
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Embodiment 1
[0043] The first application method of a vacuum sampling device for a gas chromatograph is used to measure the purity of a sample gas. Take a helium sample gas tank, install it on the position of the sample container 2, and measure the volume concentration of each impurity component in the helium sample according to the following steps.
[0044] 1a. Open the pressure sensor valve 11 and the vacuum gauge valve 14, and obtain the air pressure value, vacuum degree and temperature value from the pressure display instrument 9, vacuum display instrument 16 and temperature display instrument 7, and the temperature value is 19.9°C;
[0045] 1b. Close calibration gas valve 5, vacuum valve 17 and vent valve 13;
[0046] 1c. Start the vacuum pump 18, open the vacuum valve 17 and the sample gas valve 6 in turn, and start vacuuming;
[0047] 1d. When the reading of the vacuum display instrument 16 is lower than 5Pa, close the vacuum valve 17, open the switch of the sample container 2 until ...
Embodiment 2
[0052] The second application method of a vacuum sampling device for a gas chromatograph is used for measuring standard gases. Take a standard gas cylinder whose balance gas is He and whose components are 5ppmH2, 6.1ppmO2, and 7.5ppmN2, install it on the position of standard gas cylinder 1, and measure the peak area of each component chromatographic peak in the standard gas according to the following steps .
[0053] 2a. Open the pressure sensor valve 11 and the vacuum gauge valve 14, and obtain the air pressure value, vacuum degree and temperature value from the pressure display instrument 9, vacuum display instrument 16 and temperature display instrument 7, and the temperature value is 19.9°C;
[0054] 2b. Close the sample gas valve 6 and the vacuum valve 17, open the switch of the standard gas cylinder 1, the standard gas valve 5 and the vent valve 13, adjust the pressure reducing valve 3, and use the standard gas to purge for 3-5 minutes;
[0055] 2c. Close the calibrat...
Embodiment 3
[0061] The embodiment of this embodiment is basically the same as that of Embodiment 2, the main difference is that, considering the interference of oxygen and nitrogen in the atmosphere during the measurement process, the oxygen and nitrogen content in high-purity helium with a purity higher than 99.999% was measured. Take a high-purity helium cylinder with a purity higher than 99.999%, install it on the position of the standard gas cylinder 1, measure and analyze the oxygen and nitrogen content, and obtain the background oxygen and nitrogen volume concentration in the measurement step as O2: 0.06ppm, N2 : 0.25ppm.
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Abstract
The invention discloses an application method of a vacuum sample injection device for a gas chromatograph. A standard gas cylinder and a sample container in the vacuum sample injection device used in the application method are respectively connected with a gas inlet of the gas chromatograph through a gas pipe; a vacuum pump is connected with a gas outlet of the gas chromatograph through a gas pipe; a pressure sensor for measuring the gas pressure valve in the gas pipe and a vacuum meter for measuring the vacuum degree in the gas pipe are mounted on the gas pipe; and a temperature sensor for measuring the ambient temperature value is further mounted. The vacuum sample injection device improves the traditional valve sample injection manner of the gas chromatograph, and prevents ambient air from polluting the sample gas to be measured; a sample injection method developed on the basis of the vacuum sample injection device effectively improves the quantitative analysis precision of the components (especially oxygen and oxygen components in trace amount) in the sample gas; and the application method avoids overloaded response or over-low response of a gas chromatograph detector, widens the response linear range of the gas chromatograph detector and reduces the analysis error.
Description
technical field [0001] The invention belongs to the technical field of gas chromatograph analyzers, and in particular relates to an application method of a vacuum sampling device for a gas chromatograph. Background technique [0002] Gas chromatography is widely used in petroleum, chemical industry, biochemistry, medicine and health, food industry, environmental protection, etc., and can perform qualitative and quantitative analysis of gases. In gas chromatography, sampling is one of the main sources of quantitative analysis errors. The principle, structure, materials used, temperature of sample injection, sample volume, speed of sample injection, tools used for sample injection, etc. will affect the quantitative and qualitative repeatability and accuracy of gas chromatographic analysis. direct impact. [0003] The sampling method of commercialized valve sampling system for gas samples is easy to operate and has good quantitative repeatability, but it is not suitable for s...
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Application Information
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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/16
CPCG01N30/16
Inventor 薛志彦兰晓华刘聪刘显坤唐彬张百甫王梓游庆明
Owner INST OF NUCLEAR PHYSICS & CHEM CHINA ACADEMY OF
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