CN114019101A - High-pressure gas trace moisture analysis device and analysis method - Google Patents
High-pressure gas trace moisture analysis device and analysis method Download PDFInfo
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- 238000004458 analytical method Methods 0.000 title claims abstract description 44
- 239000007789 gas Substances 0.000 claims abstract description 43
- 230000009467 reduction Effects 0.000 claims abstract description 37
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 24
- 239000010959 steel Substances 0.000 claims abstract description 24
- 239000011261 inert gas Substances 0.000 claims abstract description 18
- 238000010926 purge Methods 0.000 claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 21
- 230000006837 decompression Effects 0.000 claims description 16
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 238000004891 communication Methods 0.000 claims description 2
- 230000006641 stabilisation Effects 0.000 claims 1
- 238000011105 stabilization Methods 0.000 claims 1
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- WMIYKQLTONQJES-UHFFFAOYSA-N hexafluoroethane Chemical compound FC(F)(F)C(F)(F)F WMIYKQLTONQJES-UHFFFAOYSA-N 0.000 description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 4
- 239000005977 Ethylene Substances 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000000087 stabilizing effect Effects 0.000 description 3
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- XPDWGBQVDMORPB-UHFFFAOYSA-N Fluoroform Chemical compound FC(F)F XPDWGBQVDMORPB-UHFFFAOYSA-N 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- RWRIWBAIICGTTQ-UHFFFAOYSA-N difluoromethane Chemical compound FCF RWRIWBAIICGTTQ-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- -1 diborane Chemical compound 0.000 description 1
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229910000042 hydrogen bromide Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—Specially adapted to detect a particular component
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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Abstract
The invention discloses a high-pressure gas trace moisture analysis device, which comprises a main pipeline, wherein a steel cylinder to be detected, a fixed pipe, a protection box, a multi-stage pressure reduction system, a flowmeter and a moisture meter are sequentially arranged on the main pipeline; the invention also discloses an analysis method for analyzing trace moisture of high-pressure gas by using the device, which comprises the following steps: firstly, adjusting the pressure value of a pressure relief valve in each stage of pressure reduction system according to the pressure of the high-pressure gas to be detected in the steel cylinder to be detected; then opening a valve on a main pipeline and adjusting the opening of the valve until the reading of the flowmeter is analyzed within the allowable range of the moisture meter, and closing the valve after the reading of the moisture meter is stable; after the analysis is finished, introducing inert gas to purge the pipeline system, and vacuumizing; the above operation was repeated 20 times and then stopped. The invention solves the problem of low-temperature environment caused by pressure reduction by grading pressure reduction, and has high analysis accuracy and high analysis efficiency.
Description
Technical Field
The invention belongs to the technical field of chemical analysis, and particularly relates to a high-pressure gas trace moisture analysis device and method.
Background
The requirement of high-purity gas on moisture is strict, the moisture is the most important index of the high-purity gas, but the high-purity gas is influenced by gas characteristics, system cleanliness and the like, the accuracy of trace moisture analysis is poor, and the judgment of production and the quality of products are seriously influenced.
At present, all used trace moisture analyzers cannot resist high pressure, high-pressure gas needs to pass through a pressure reducer and then enters the analyzer when being analyzed, the pressure reduction process is a process of doing work by gas expansion, the temperature in the pressure reducer can be rapidly reduced, moisture is gathered at the pressure reducer, and the accuracy and the stability of analysis are affected.
Disclosure of Invention
The invention aims to solve the technical problem of providing a high-pressure gas trace moisture analysis device and an analysis method aiming at the defects of the prior art. The method adopts a multistage decompression system, can solve the problem of low-temperature environment caused by decompression, is suitable for measuring trace moisture in high-purity high-pressure gas, and has the characteristics of high measurement efficiency and good stability.
In order to solve the technical problems, the invention adopts the technical scheme that: the utility model provides a high-pressure gas trace moisture analytical equipment, a serial communication port, including the main pipeline, main pipeline is last to have set gradually the steel bottle that awaits measuring, fixed pipe, protection box, multistage depressurization system, flowmeter and moisture meter, and every stage of depressurization system all is connected with vacuum line including the inert gas connecting pipe, relief valve, pressure gauge, relief pipe and the second valve that set gradually, and the one end of a plurality of relief pipes is connected with the vacuum line jointly, and the one end of a plurality of nitrogen gas connecting pipes is connected with inert gas pipeline jointly, all install first valve on the inert gas connecting pipe.
Preferably, multistage depressurization system includes first order depressurization system, second level depressurization system, third level depressurization system, first order depressurization system is including the inert gas connecting pipe, relief valve, pressure gauge, first decompression pipe and the second valve that set gradually, second level depressurization system is including the inert gas connecting pipe, relief valve, pressure gauge, second decompression pipe and the second valve that set gradually, third level depressurization system is including the inert gas connecting pipe, relief valve, pressure gauge, third decompression pipe and the second valve that set gradually.
Preferably, first decompression pipe, second decompression pipe and third decompression pipe are located one side and the equidistance setting of total pipeline, and three inert gas connecting pipe is located opposite side and the equidistance setting of total pipeline.
Preferably, be equipped with clarification plant in the protection box, fixed pipe with the steel bottle of awaiting measuring can be dismantled and be connected.
Preferably, a fourth valve is installed on the fixed pipe.
Preferably, the first pressure reducing pipe, the second pressure reducing pipe and the third pressure reducing pipe are all provided with third valves.
The invention also provides an analysis method for analyzing trace moisture of high-pressure gas by using the device, which is characterized by comprising the following steps of:
s1, adjusting the pressure value of the pressure relief valve in each stage of pressure reduction system on the main pipeline according to the pressure of the high-pressure gas to be detected in the steel cylinder to be detected;
s2, opening the steel cylinder to be tested, opening the fourth valve and all the second valves, adjusting the opening degrees of the fourth valve and all the second valves until the readings of the flow meters are analyzed within the allowable range of the moisture meter, and closing the fourth valve after the readings of the moisture meter are stable;
s3, after the analysis is finished, opening all the first valves, introducing inert gas to purge the pipeline, closing the first valves after purging, and opening all the third valves to vacuumize;
s4, repeating the steps S1-S3 for 20 times and stopping.
Preferably, when the number of the stages of the pressure reducing system is more than or equal to 2, the pressure reducing amount of the pressure reducing valve in each stage of the pressure reducing system is uniformly distributed according to the pressure of the high-pressure gas to be detected in the steel cylinder to be detected, and the deviation is considered to be normal within 30%.
Preferably, the temperature inside the main line in S1 is constantly 15 ℃ to 30 ℃; the moisture meter reading in S2 stabilized for 20 minutes.
Compared with the prior art, the invention has the following advantages:
1. the invention solves the problem of low-temperature environment caused by pressure reduction through a grading pressure reduction system, and the analysis system established by the method has the advantages of high analysis accuracy, high analysis efficiency and the like, is suitable for measuring trace moisture in high-purity high-pressure gas, has the characteristics of high measurement efficiency and good stability, and is suitable for measuring high-purity gas with the moisture content lower than 0.0001%.
2. According to the invention, through the purification equipment, particle impurities in the high-pressure gas to be analyzed can be intercepted, and the particle impurities are prevented from entering a subsequent analysis system to influence the analysis of the analysis system on trace moisture.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 is a schematic view of the structure of an analyzing apparatus of the present invention.
Description of reference numerals:
1-ultra-high purity nitrogen gas delivery line; 2-nitrogen connecting pipe; 3-a first valve; 4, a pressure relief valve; 5-a first pressure gauge; 6, a flow meter; 7-a second valve; 8-main line; 9-moisture meter; 10-a third valve; 11-vacuum line; 12-a second pressure reducing tube; 13-steel cylinder to be tested; 14-a protection box; 15-fixing the tube; 16-a fourth valve; 17-a third pressure reducing tube; 18-first pressure relief duct.
Detailed Description
Example 1
High-pressure gas trace moisture analytical equipment in this embodiment, including total pipeline 8, total pipeline 8 is last to have set gradually the steel bottle 13 that awaits measuring, fixed pipe 15, protection box 14, multistage depressurization system, flowmeter 6 and moisture meter 9, and every stage of depressurization system all includes nitrogen gas connecting pipe 2, relief valve 4, pressure gauge 5, relief pipe and the second valve 7 that sets gradually, and the one end of a plurality of relief pipes is connected with vacuum pipeline 11 jointly, and the one end of a plurality of nitrogen gas connecting pipes 2 is connected with super high pure nitrogen gas pipeline 1 jointly, all install first valve 3 on the nitrogen gas connecting pipe 2.
In this embodiment, multistage depressurization system includes first order depressurization system, second level depressurization system, third level depressurization system, first order depressurization system is including nitrogen gas connecting pipe 2, relief valve 4, pressure gauge 5, first relief pipe 18 and the second valve 7 that sets gradually, second level depressurization system is including nitrogen gas connecting pipe 2, relief valve 4, pressure gauge 5, second relief pipe 12 and the second valve 7 that sets gradually, third level depressurization system is including nitrogen gas connecting pipe 2, relief valve 4, pressure gauge 5, third relief pipe 17 and the second valve 7 that sets gradually. The first decompression tube 18, the second decompression tube 12 and the third decompression tube 17 are located on one side of the main line 8, and the three nitrogen connecting tubes 2 are located on the other side of the main line 8; a purifying device is arranged in the protection box 14, and the fixed tube 15 is detachably connected with the steel cylinder 13 to be detected; a fourth valve 16 is arranged on the fixed pipe 15; the first pressure reducing pipe 18, the second pressure reducing pipe 12 and the third pressure reducing pipe 17 are all provided with a third valve 10.
The high-pressure gas analyzed by the analysis device of the embodiment comprises hydrogen chloride, hydrogen bromide, chlorine, silicon tetrafluoride, diborane, trifluoromethane, hexafluoroethane, difluoromethane, dichlorosilane, ethane and ethylene.
In this embodiment, the purification device is a filter, and is used to prevent particles in the gas from entering the analysis system and affecting the analysis of the analysis system.
Example 2
The method for analyzing trace moisture in high-purity hexafluoroethane by using the analysis device in example 1 in the present example comprises the following steps:
s1, adjusting the pressure value of the pressure relief valve 4 in each stage of pressure reduction system on the main pipeline 8 according to the pressure of the standard gas hexafluoroethane in the steel cylinder 13 to be detected, adjusting the pressure before entering a first pressure reduction pipe 18 in a first stage of pressure reduction system to 2MPa, adjusting the pressure before entering a second pressure reduction pipe 12 in a second stage of pressure reduction system to 1MPa, adjusting the pressure before entering a third pressure reduction pipe 17 in a third stage of pressure reduction system to 0.2MPa, wherein the moisture content in the standard gas hexafluoroethane is 0.00005%, and the temperature inside the main pipeline 8 is constantly 15 ℃;
when the number of stages of the pressure reducing system is more than or equal to 2, the pressure reducing amount of the pressure reducing valve 4 in each stage of the pressure reducing system is uniformly distributed according to the pressure of the high-pressure gas to be detected in the steel cylinder 13 to be detected, and the deviation is considered to be normal within 30%;
s2, opening the steel cylinder 13 to be tested, opening the fourth valve 16 and all the second valves 7, adjusting the opening degrees of the fourth valve 16 and all the second valves 7 until the readings of the flow meters 6 are within the allowable range of the moisture meter 9 for analysis, stabilizing the readings of the moisture meter 9 at 0.49ppm (0.000049%), and closing the fourth valve 16 after the readings of the moisture meter 9 are stabilized for 20 minutes;
s3, after the analysis is finished, opening the first valve 3, introducing nitrogen, purging the pipeline, closing the first valve 3 after purging, and then opening all the third valves 10 for vacuumizing;
s4, repeating the steps S1-S3 for 20 times and stopping;
comparative example 1
The method for analyzing trace moisture in high-purity hexafluoroethane in this comparative example was the same as in example 2 except that a single-stage pressure reducing system was used.
Through detection, the temperature of a pressure release valve 4 in a single-stage pressure reduction system is too low due to pressure reduction of the moisture meter, the reading irregularly fluctuates within the range of 0.001% -0.00005%, and the stable value cannot be reached after 3 hours.
Example 3
In this example, the method for analyzing trace moisture in high purity ethylene using the analysis apparatus of example 1 comprises the following steps:
s1, adjusting the pressure value of the pressure relief valve 4 in each stage of pressure reduction system on the main pipeline 8 according to the pressure of the standard gas ethylene in the steel cylinder 13 to be detected, adjusting the pressure before entering the first pressure reduction pipe 18 in the first stage of pressure reduction system to 3.5MPa, adjusting the pressure before entering the second pressure reduction pipe 12 in the second stage of pressure reduction system to 2MPa, adjusting the pressure before entering the third pressure reduction pipe 17 in the third stage of pressure reduction system to 0.4MPa, wherein the moisture content in the standard gas ethylene is 0.00008%, and the temperature inside the main pipeline 8 is constant to 30 ℃;
when the number of stages of the pressure reducing system is more than or equal to 2, the pressure reducing amount of the pressure reducing valve 4 in each stage of the pressure reducing system is uniformly distributed according to the pressure of the high-pressure gas to be detected in the steel cylinder 13 to be detected, and the deviation is considered to be normal within 30%;
s2, opening the steel cylinder 13 to be tested, opening the fourth valve 16 and all the second valves 7, adjusting the opening degrees of the fourth valve 16 and all the second valves 7 until the readings of the flow meters 6 are within the allowable range of the moisture meter 9 for analysis, stabilizing the readings of the moisture meter 9 at 0.5ppm (0.00005%), and closing the fourth valve 16 after the readings of the moisture meter 9 are stabilized for 20 minutes;
s3, after the analysis is finished, opening the first valve 3, introducing nitrogen, purging the pipeline, closing the first valve 3 after purging, and then opening all the third valves 10 for vacuumizing;
s4, repeating the steps S1-S3 for 20 times and stopping;
example 4
In this embodiment, the method for analyzing trace moisture in high-purity boron trichloride by using the analysis device in embodiment 1 includes the following steps:
s1, using a two-stage pressure reducing system, adjusting the pressure value of a pressure relief valve 4 in each stage of pressure reducing system on a main pipeline 8 according to the pressure of standard gas boron trichloride in the steel cylinder 13 to be detected, adjusting the pressure before entering a first pressure reducing pipe 18 in a first stage pressure reducing system to 1.3MPa, adjusting the pressure before entering a second pressure reducing pipe 12 in a second stage pressure reducing system to 0.2MPa, wherein the moisture content in the standard gas boron trichloride is 0.00003%, and the temperature inside the main pipeline 8 is constant to 23 ℃;
when the number of stages of the pressure reducing system is more than or equal to 2, the pressure reducing amount of the pressure reducing valve 4 in each stage of the pressure reducing system is uniformly distributed according to the pressure of the high-pressure gas to be detected in the steel cylinder 13 to be detected, and the deviation is considered to be normal within 30%;
s2, opening the steel cylinder 13 to be tested, opening the fourth valve 16 and all the second valves 7, adjusting the opening degrees of the fourth valve 16 and all the second valves 7 until the readings of the flow meters 6 are within the allowable range of the moisture meter 9 for analysis, stabilizing the readings of the moisture meter 9 at 0.8ppm (0.00008%), and closing the fourth valve 16 after the readings of the moisture meter 9 are stabilized for 20 minutes;
s3, after the analysis is finished, opening the first valve 3, introducing nitrogen, purging the pipeline, closing the first valve 3 after purging, and then opening all the third valves 10 for vacuumizing;
s4, repeating the steps S1-S3 for 20 times and stopping;
the inert gas for purging in the above embodiment may be not only nitrogen but also one of helium and argon.
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 (9)
1. The utility model provides a high-pressure gas trace moisture analytical equipment, includes main pipeline (8), a serial communication port, main pipeline (8) are gone up and are set gradually steel bottle (13) that await measuring, fixed pipe (15), protection box (14), multistage depressurization system, flowmeter (6) and moisture meter (9), every stage of depressurization system all is including inert gas connecting pipe (2), relief valve (4), pressure gauge (5), decompression pipe and second valve (7) that set gradually, and the one end of a plurality of decompression pipes is connected with vacuum line (11) jointly, and the one end of a plurality of nitrogen gas connecting pipes (2) is connected with inert gas conveying line (1) jointly, all install first valve (3) on inert gas connecting pipe (2).
2. The high-pressure gas trace moisture analysis device according to claim 1, wherein the multistage pressure reduction system comprises a first-stage pressure reduction system, a second-stage pressure reduction system and a third-stage pressure reduction system, the first-stage pressure reduction system comprises an inert gas connecting pipe (2), a pressure release valve (4), a pressure gauge (5), a first pressure reduction pipe (18) and a second valve (7) which are sequentially arranged, the second-stage pressure reduction system comprises an inert gas connecting pipe (2), a pressure release valve (4), a pressure gauge (5), a second pressure reduction pipe (12) and a second valve (7) which are sequentially arranged, and the third-stage pressure reduction system comprises an inert gas connecting pipe (2), a pressure release valve (4), a pressure gauge (5), a third pressure reduction pipe (17) and a second valve (7) which are sequentially arranged.
3. The high pressure gas trace moisture analysis device according to claim 2, wherein the first pressure reducing pipe (18), the second pressure reducing pipe (12) and the third pressure reducing pipe (17) are positioned on one side of the main pipeline (8) and are equidistantly arranged, and the three inert gas connecting pipes (2) are positioned on the other side of the main pipeline (8) and are equidistantly arranged.
4. The high-pressure gas trace moisture analysis device according to claim 1, wherein a purifying device is arranged in the protection box (14), and the fixing tube (15) is detachably connected with the steel cylinder (13) to be detected.
5. The high pressure gas trace moisture analysis device according to claim 1, wherein a fourth valve (16) is installed on the fixed pipe (15).
6. The high-pressure gas trace moisture analysis device according to claim 3, wherein the first decompression pipe (18), the second decompression pipe (12) and the third decompression pipe (17) are provided with a third valve (10).
7. A method for analyzing trace moisture in a high pressure gas using the apparatus of any one of claims 1 to 6, comprising the steps of:
s1, adjusting the pressure value of the pressure relief valve (4) in each stage of pressure reduction system on the main pipeline (8) according to the pressure of the high-pressure gas to be detected in the steel cylinder (13);
s2, opening the steel cylinder (13) to be tested, opening the fourth valve (16) and all the second valves (7), adjusting the opening degrees of the fourth valve (16) and all the second valves (7) until the reading of the flowmeter (6) is within the allowable range of the moisture meter (9) for analysis, and closing the fourth valve (16) after the reading of the moisture meter (9) is stable;
s3, after the analysis is finished, opening all the first valves (3), introducing inert gas to purge the pipeline, closing the first valves (3) after purging, and opening all the third valves (10) to vacuumize;
s4, repeating the steps S1-S3 for 20 times and stopping.
8. The method for analyzing trace moisture in high-pressure gas according to claim 7, wherein when the number of the pressure reduction systems is greater than or equal to 2, the pressure reduction amount of the pressure release valve (4) in each pressure reduction system is uniformly distributed according to the pressure of the high-pressure gas to be detected in the steel cylinder (13) to be detected, and the deviation is considered to be normal within 30%.
9. The high pressure gas trace moisture analysis method according to claim 7, wherein the temperature inside the main pipeline (8) in S1 is constantly 15-30 ℃; the moisture meter (9) in S2 read a stabilization time of 20 minutes.
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