CN213275507U - Trace dynamic standard gas preparation device for calibrating nitrogen oxide analyzer - Google Patents

Trace dynamic standard gas preparation device for calibrating nitrogen oxide analyzer Download PDF

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Publication number
CN213275507U
CN213275507U CN202022195221.2U CN202022195221U CN213275507U CN 213275507 U CN213275507 U CN 213275507U CN 202022195221 U CN202022195221 U CN 202022195221U CN 213275507 U CN213275507 U CN 213275507U
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gas
nitrogen
tee joint
path
gas path
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CN202022195221.2U
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夏春
李剑
程丽萍
贺媛媛
刘学刚
薛岩明
刘巍
陈全森
吕利
汪圣甲
刘培源
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Qingdao Institute Of Measurement Technology
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Qingdao Institute Of Measurement Technology
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Abstract

The utility model relates to the technical field of environmental monitoring equipment, and discloses a trace dynamic standard gas preparation device for calibrating a nitrogen oxide analyzer, which comprises a gas dilution device; the zero gas source nitrogen steel cylinder and the NO standard gas steel cylinder are respectively communicated with a gas diluting device; the method is characterized in that: the gas diluting device comprises a first gas circuit, a second gas circuit and a third gas circuit, and the communicating pipelines of the gas diluting device are anti-adsorption EP material pipelines. The trace dynamic standard gas preparation device has reasonable uncertainty of prepared standard gas, uniform mixing and stable quantity value, can trace the national standard, can provide calibration for a nitrogen oxide analyzer by a chemiluminescence method in the (5-10) ppb order of magnitude, ensures the accuracy of instrument measurement and has stronger practicability.

Description

Trace dynamic standard gas preparation device for calibrating nitrogen oxide analyzer
Technical Field
The utility model relates to an environmental monitoring equipment technical field specifically is a nitrogen oxide analysis appearance calibration is with gaseous preparation facilities of trace dynamic standard.
Background
The content of nitrogen, oxygen, argon and carbon dioxide in the atmosphere is 99.997 percent of that of dry air, the content of other gases is only 0.003 percent, and the contents of the gases are very small and are mostly trace gases. Such as nitrogen oxides, hydrocarbons, sulfides and chlorides. Nitrogen oxides are one of main pollutants of air pollution, are seriously harmful to human health, and are closely concerned by various social circles in recent years in monitoring, treating and other works of nitrogen oxides in the air. The chemiluminescence method detection technology is based on the fact that NO can perform chemiluminescence reaction with O3, the luminous intensity is in direct proportion to the concentration of NO, and the nitrogen oxide analyzer is based on the chemiluminescence method detection technology to detect the content of nitrogen oxide. In the long-term operation of the nitrogen oxide analyzer, along with the increase of the working time of the analyzer, the sensitivity of the analyzer has a trend of decreasing, so that the data of the nitrogen oxide analyzer is distorted, calibration is needed, and the working stability of the analyzer is improved. When the nitrogen oxide analyzer is used normally, the effective service life of the sensor is 24-36 months. During the useful life, calibration and detection should be frequent to ensure accurate and effective gas monitoring.
When the nitrogen oxide analyzer is calibrated, dynamic standard gas is used, the dynamic standard gas is measured by a relative comparison method, a zero gas and a gas with standard concentration are firstly used for calibrating the analyzer, a standard curve is obtained and stored in the analyzer, and when the nitrogen oxide analyzer is measured, the electric signal generated by the concentration of the gas to be measured is compared with the electric signal with standard concentration by the analyzer, and an accurate gas concentration value is obtained through calculation. The preparation of dynamic standard gases is particularly important at low concentrations, especially at the 10ppb level. Frequent calibration of a nox analyzer is an indispensable task to ensure that the measurement of the instrument is accurate.
The gas preparation device is used for accurately mixing and blending various gases with high concentration through a mass flow controller to provide accurate standard gases for different purposes.
SUMMERY OF THE UTILITY MODEL
To prior art's not enough, the utility model provides a nitrogen oxide analysis appearance is trace dynamic standard gas preparation facilities for calibration can prepare the dynamic standard gas below the 10ppb level, and gas mixing is even, and the calibration concentration value is stable.
The utility model provides a following technical scheme:
a trace dynamic standard gas preparation device for calibrating a nitrogen oxide analyzer comprises a gas dilution device; the zero gas source nitrogen steel cylinder and the NO standard gas steel cylinder are respectively communicated with a gas diluting device; the gas diluting device comprises a first gas circuit, a second gas circuit and a third gas circuit, and the communicating pipelines of the gas diluting device are anti-adsorption pipelines;
one end of the first gas path is communicated with an NO standard gas steel cylinder, and the other end of the first gas path is connected with a tee joint I; the gas circuit is provided with a gas flowmeter I which is electrically connected with a flow display instrument I; a pressure reducing valve I is arranged between the NO standard gas steel cylinder and the gas flowmeter I;
one end of the second gas path is communicated with a zero gas source nitrogen steel cylinder, and the other end of the second gas path is connected with a tee joint I; the gas path is provided with a gas flowmeter II which is electrically connected with a flow display instrument II; a nitrogen purification device is arranged between the zero gas source nitrogen steel cylinder and the gas flowmeter II; a pressure reducing valve II is arranged between the zero gas source nitrogen steel cylinder and the nitrogen purifying device;
one end of the third gas path is connected with a tee joint I, the other end of the third gas path is communicated with a nitrogen oxide analyzer, a tee joint IV is arranged on the gas path, and one port of the third gas path is communicated with the atmosphere.
Preferably, the gas dilution device further comprises a fourth gas path; one end of the second gas path is communicated with the second gas path through a tee joint II, and the tee joint II is arranged between the gas flowmeter II and the nitrogen purification device on the second gas path; the other end of the third gas path is communicated with a third gas path through a tee joint III, and the tee joint III is arranged between the tee joint I and the tee joint IV on the third gas path; and a gas flowmeter III is arranged on the fourth gas path and is electrically connected with a flow display instrument III.
Preferably, the nitrogen purification device is formed by connecting a nitrogen purifier I and a nitrogen purifier II in series in a gas path.
Preferably, the nitrogen purifier I is a 7N purifier, and the nitrogen purifier II is a 9N purifier.
Optimally, the adsorption-preventing pipelines are all stainless steel EP material pipelines.
Preferably, the tee joint I, the tee joint II, the tee joint III and the tee joint IV are all stainless steel tee joints.
The utility model discloses a nitrogen oxide analysis appearance calibration is with trace dynamic standard gas preparation facilities, at first solved matrix gas's purity problem. 99.9999% nitrogen is used as substrate gas, a nitrogen purification device is arranged on a low-pressure pipeline, and NO in outlet gas2,H2O,02,CO,CO2,H2The NMHC aliquot was less than 1 ppb. And secondly, the gas pipeline is an all-welded EP material pipeline, is sealed by all metal and has no clamping sleeve and interface, so that gas adsorption is reduced to the maximum extent. The device can fully and uniformly mix the mixed trace gas, further dilute the mixed trace gas, obtain the dynamic standard gas with the minimum concentration of 1ppb, has reasonable uncertainty for preparing the standard gas, uniform mixing and stable quantity value, and can be used for preparing the dynamic standard gas with the minimum concentration of 1ppbTracing to the national standard, the method can provide calibration for the nitrogen oxide analyzer by the chemiluminescence method in the (5-10) ppb order, ensure the accuracy of the measurement of the analyzer and have stronger practicability.
Drawings
Fig. 1 is a schematic view of a gas path structure in embodiment 1 of the present invention.
Fig. 2 is a schematic view of a gas path structure in embodiment 2 of the present invention.
In the figure: 1. A NO standard gas cylinder; 2. a zero gas source nitrogen cylinder; 3. a pressure reducing valve I; 4. a pressure reducing valve II; 5. a nitrogen purification device; 6. a nitrogen oxide analyzer; 7. an anti-adsorption pipeline; 11. A gas flowmeter I; 12. a gas flow meter II; 13. a gas flow meter III; 21. a flow display instrument I; 22. a flow display instrument II; 23. a flow display instrument III; 31. a tee joint I; 32. a tee joint II; 33. a tee joint III; 34. a tee joint IV; 51. a nitrogen purifier I; 52. and a nitrogen purifier II.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
Example 1
As shown in fig. 1, in the trace dynamic standard gas preparation device for calibrating a nitrogen oxide analyzer of the present embodiment, a zero gas source nitrogen gas steel cylinder 2 and a NO standard gas steel cylinder 1 are respectively communicated with a gas dilution device; the gas diluting device comprises a first gas circuit, a second gas circuit and a third gas circuit, and the communicating pipelines of the gas diluting device are stainless steel EP material anti-adsorption pipelines 7.
One end of the first gas path is communicated with the NO standard gas steel cylinder 1, and the other end of the first gas path is connected with a tee joint I31; the gas circuit is provided with a gas flowmeter I11, and the gas flowmeter I11 is electrically connected with a flow display instrument I21; a pressure reducing valve I3 is arranged between the NO standard gas steel cylinder 1 and the gas flowmeter I11.
One end of the second gas path is communicated with the zero gas source nitrogen steel cylinder 2, and the other end of the second gas path is connected with a tee joint I31; the gas circuit is provided with a gas flowmeter II 12, and the gas flowmeter II 12 is electrically connected with a flow display instrument II 22; a nitrogen purification device 5 is arranged between the zero gas source nitrogen steel cylinder 2 and the gas flowmeter II 12; a pressure reducing valve II 4 is arranged between the zero gas source nitrogen steel cylinder 2 and the nitrogen purifying device 5; the nitrogen purification device 5 is formed by connecting a nitrogen purifier I51 and a nitrogen purifier II 52 in series in a gas path, wherein the nitrogen purifier I51 is a 7N purifier, and the nitrogen purifier II 52 is a 9N purifier.
One end of the third gas path is connected with a tee joint I31, the other end of the third gas path is communicated with a nitrogen oxide analyzer 6, a tee joint IV 34 is arranged on the third gas path, and one port of the tee joint IV 34 is communicated with the atmosphere. The tee joint I and the tee joint IV are both made of stainless steel materials.
When this nitrogen oxide analysis appearance calibration is with trace dynamic standard gas preparation facilities use, nitrogen oxide analysis appearance start-up back, at first open its zero gas source nitrogen gas steel bottle 2 and NO standard gas steel bottle 1, adjust the relief pressure valve respectively, then set up the flow of flowmeter respectively, set up trace dynamic standard gas set point, stable air feed. And a negative pressure gas path is arranged between the tee joint IV 34 and the nitrogen oxide analyzer 6 in the third gas path, one part of the trace dynamic standard gas formed by mixing the first gas path and the second gas path enters the nitrogen oxide analyzer 6, and the redundant part of the trace dynamic standard gas is discharged through a port of the tee joint IV 34.
Example 2
As shown in fig. 2, in the trace dynamic standard gas preparation device for calibrating a nitrogen oxide analyzer of the present embodiment, a zero gas source nitrogen gas steel cylinder 2 and a NO standard gas steel cylinder 1 are respectively communicated with a gas dilution device; the gas diluting device comprises a first gas circuit, a second gas circuit, a third gas circuit and a fourth gas circuit, and the communicating pipelines of the gas diluting device are stainless steel EP material anti-adsorption pipelines 7.
One end of the first gas path is communicated with the NO standard gas steel cylinder 1, and the other end of the first gas path is connected with a tee joint I31; the gas circuit is provided with a gas flowmeter I11, and the gas flowmeter I11 is electrically connected with a flow display instrument I21; a pressure reducing valve I3 is arranged between the NO standard gas steel cylinder 1 and the gas flowmeter I11.
One end of the second gas path is communicated with the zero gas source nitrogen steel cylinder 2, and the other end of the second gas path is connected with a tee joint I31; the gas circuit is provided with a gas flowmeter II 12, and the gas flowmeter II 12 is electrically connected with a flow display instrument II 22; a nitrogen purification device 5 is arranged between the zero gas source nitrogen steel cylinder 2 and the gas flowmeter II 12; a tee joint II 32 is arranged between the gas flowmeter II 12 and the nitrogen purification device 5; a pressure reducing valve II 4 is arranged between the zero gas source nitrogen steel cylinder 2 and the nitrogen purifying device 5; the nitrogen purification device 5 is formed by connecting a nitrogen purifier I51 and a nitrogen purifier II 52 in series in a gas path, wherein the nitrogen purifier I51 is a 7N purifier, and the nitrogen purifier II 52 is a 9N purifier.
One end of the third gas path is connected with a tee joint I31, the other end of the third gas path is communicated with a nitrogen oxide analyzer 6, a tee joint IV 34 is arranged on the third gas path, and one port of the tee joint IV 34 is communicated with the atmosphere. A tee joint III 33 is arranged between the tee joint I31 and the tee joint IV 34.
One end of the fourth air path is communicated with the second air path through a tee joint II 32, the other end of the fourth air path is communicated with the third air path through a tee joint III 33, a gas flowmeter III 13 is arranged on the fourth air path, and the gas flowmeter III 13 is electrically connected with a flow display instrument III 23. The tee joint I31, the tee joint II 32, the tee joint III 33 and the tee joint IV 34 are all stainless steel tee joints.
The difference between this embodiment and embodiment 1 is that there is one more re-dilution gas path, i.e. the fourth gas path.
When this nitrogen oxide analysis appearance calibration is with trace dynamic standard gas preparation facilities use, nitrogen oxide analysis appearance start-up back, at first open its zero gas source nitrogen gas steel bottle 2 and NO standard gas steel bottle 1, adjust two relief pressure valves respectively, then set up the flow of three flowmeter respectively, adjust trace dynamic standard gas set value, stable air feed. And a negative pressure gas path is arranged between the tee joint IV 34 and the nitrogen oxide analyzer 6 in the third gas path, one part of the trace dynamic standard gas formed by mixing the first gas path, the second gas path and the fourth gas path enters the nitrogen oxide analyzer 6, and the redundant part of the trace dynamic standard gas is discharged through a port of the tee joint IV 34.
The trace dynamic standard gas preparation device for calibrating the nitrogen oxide analyzer of each embodiment,the problem of the purity of the matrix gas is solved first. 99.9999% nitrogen is used as substrate gas, a nitrogen purification device is arranged on a low-pressure pipeline, and NO in outlet gas2,H2O,02,CO,CO2,H2The NMHC aliquot was less than 1 ppb. And secondly, the gas pipeline is an all-welded EP material pipeline, is sealed by all metal and has no clamping sleeve and interface, so that gas adsorption is reduced to the maximum extent. The device can fully mix the mixed trace gas uniformly, further dilute the mixed trace gas and obtain the dynamic standard gas with the minimum concentration of 1ppb, and the trace dynamic standard gas preparation device has the advantages of reasonable uncertainty of the prepared standard gas, uniform mixing, stable quantity value and capability of tracing to the national standard, can provide calibration for a nitrogen oxide analyzer by a chemiluminescence method in the ppb (5-10) order, ensures the accuracy of instrument measurement and has stronger practicability.
In particular, the trace dynamic standard gas preparation apparatus for calibration of the nitrogen oxide analyzer of example 2,
99.9999% nitrogen was used as the matrix gas, which was filled using a 25 liter 10MPa dedicated nitrogen cylinder. After the substrate gas is decompressed, the substrate gas enters a gas purification device on a low-pressure pipeline of 0.2MPa, a 0.003-micron nitrogen purifier is arranged in the purification device, and the purification device is a first-rate purifier sold by Beijing Bernark science and technology Limited company and has rated gas flow: 30L/Min, maximum gas pressure: 1.0MPa, maximum gas pressure difference: 0.1MPa, the purity of the inlet gas is not lower than the national standard 5N, and NO in the outlet gas2,H2O,02,CO,CO2,H2The NMHC aliquot was less than 1 ppb. The NO standard gas is a certified standard substance obtained by a weighing method, the nominal value is 10 liters of 10MPa steel cylinder gas with 1000ppb, a gas flowmeter adopts a mass flowmeter, the upper limit of the flow rate of the gas flowmeter is 20ml/min, the upper limit of the flow rate of the gas flowmeter is 2L/min, the accuracy is +/-1.0 percent FS, the linearity is +/-0.5 percent, the differential pressure range is less than 0.02MPa, the gas flowmeter is sealed by all metals, the gas flowmeters are calibrated by 0.2-level standard flowmeters, and the uncertainty of the corrected value is less than 0.5 percent. The gas pipeline adopts the all-welded EP pipeline, does not have cutting ferrule and interface, but furthest reduces gas adsorption. NO standard gas mixed with substrate gasAnd finally, obtaining dynamic trace standard gas, and adding matrix gas again through a fourth gas path, so that the mixed trace gas can be further uniformly mixed and further diluted, and the dynamic standard gas with the minimum concentration of 1ppb can be obtained.

Claims (6)

1. A trace dynamic standard gas preparation device for calibrating a nitrogen oxide analyzer comprises a gas dilution device; the zero gas source nitrogen steel cylinder and the NO standard gas steel cylinder are respectively communicated with a gas diluting device; the method is characterized in that: the gas diluting device comprises a first gas circuit, a second gas circuit and a third gas circuit, and the communicating pipelines of the gas diluting device are anti-adsorption pipelines;
one end of the first gas path is communicated with an NO standard gas steel cylinder, and the other end of the first gas path is connected with a tee joint I; the gas circuit is provided with a gas flowmeter I which is electrically connected with a flow display instrument I; a pressure reducing valve I is arranged between the NO standard gas steel cylinder and the gas flowmeter I;
one end of the second gas path is communicated with a zero gas source nitrogen steel cylinder, and the other end of the second gas path is connected with a tee joint I; the gas path is provided with a gas flowmeter II which is electrically connected with a flow display instrument II; a nitrogen purification device is arranged between the zero gas source nitrogen steel cylinder and the gas flowmeter II; a pressure reducing valve II is arranged between the zero gas source nitrogen steel cylinder and the nitrogen purifying device;
one end of the third gas path is connected with a tee joint I, the other end of the third gas path is communicated with a nitrogen oxide analyzer, a tee joint IV is arranged on the gas path, and one port of the third gas path is communicated with the atmosphere.
2. The trace dynamic standard gas preparation device according to claim 1, wherein: the gas diluting device also comprises a fourth gas path; one end of the second gas path is communicated with the second gas path through a tee joint II, and the tee joint II is arranged between the gas flowmeter II and the nitrogen purification device on the second gas path; the other end of the third gas path is communicated with a third gas path through a tee joint III, and the tee joint III is arranged between the tee joint I and the tee joint IV on the third gas path; and a gas flowmeter III is arranged on the fourth gas path and is electrically connected with a flow display instrument III.
3. The trace dynamic standard gas preparation device according to claim 2, wherein: the nitrogen purification device is formed by connecting a nitrogen purifier I and a nitrogen purifier II in series in a gas path.
4. The trace dynamic standard gas preparation device according to claim 3, wherein: the nitrogen purifier I is a 7N purifier, and the nitrogen purifier II is a 9N purifier.
5. The trace dynamic standard gas preparation device according to claim 4, wherein: and the anti-adsorption pipelines are all stainless steel EP material pipelines.
6. The trace dynamic standard gas preparation device according to claim 4, wherein: and the tee joint I, the tee joint II, the tee joint III and the tee joint IV are all stainless steel tee joints.
CN202022195221.2U 2020-09-30 2020-09-30 Trace dynamic standard gas preparation device for calibrating nitrogen oxide analyzer Expired - Fee Related CN213275507U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114527217A (en) * 2022-02-24 2022-05-24 山东星菲化学有限公司 Preparation method of quality control standard substance in adsorption tube

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114527217A (en) * 2022-02-24 2022-05-24 山东星菲化学有限公司 Preparation method of quality control standard substance in adsorption tube

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