CN212610476U - A device for extracting dissolved gas from water samples in high-vacuum double-valve glass bottles - Google Patents
A device for extracting dissolved gas from water samples in high-vacuum double-valve glass bottles Download PDFInfo
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- CN212610476U CN212610476U CN202021311677.4U CN202021311677U CN212610476U CN 212610476 U CN212610476 U CN 212610476U CN 202021311677 U CN202021311677 U CN 202021311677U CN 212610476 U CN212610476 U CN 212610476U
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- 239000011521 glass Substances 0.000 title claims abstract description 137
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 239000002184 metal Substances 0.000 claims abstract description 22
- 229910052751 metal Inorganic materials 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 239000005337 ground glass Substances 0.000 claims description 65
- 238000007872 degassing Methods 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 11
- 238000004458 analytical method Methods 0.000 abstract description 9
- 238000000605 extraction Methods 0.000 abstract description 8
- 238000005259 measurement Methods 0.000 abstract description 6
- 230000000007 visual effect Effects 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 81
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 20
- 239000000203 mixture Substances 0.000 description 11
- 238000005070 sampling Methods 0.000 description 9
- 239000003345 natural gas Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 230000018109 developmental process Effects 0.000 description 6
- 230000005484 gravity Effects 0.000 description 6
- 238000009849 vacuum degassing Methods 0.000 description 5
- 238000004817 gas chromatography Methods 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 239000008398 formation water Substances 0.000 description 3
- 239000005431 greenhouse gas Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 230000001050 lubricating effect Effects 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000005442 atmospheric precipitation Substances 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 239000001272 nitrous oxide Substances 0.000 description 1
- 229910052756 noble gas Inorganic materials 0.000 description 1
- 150000002835 noble gases Chemical group 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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Abstract
The utility model relates to an extraction element of solution gas in high vacuum bivalve glass bottle water sample, the device include bivalve glass bottle I, bivalve glass bottle II, high vacuum system and gas measurement appearance ware. The lower end of the double-valve glass bottle I is connected with a high vacuum system through a high vacuum joint I, and the upper end of the double-valve glass bottle I is connected with a double-valve glass bottle II through a high vacuum joint II; a heating sheet is arranged on the outer side of the double-valve glass bottle I; the upper end of the double-valve glass bottle II is connected with a gas measuring instrument through a high vacuum joint III and a metal high vacuum valve in sequence; and locking devices are arranged on the double-valve glass bottle I and the double-valve glass bottle II. The utility model discloses can realize deviating from under the high vacuum and collect dissolved gas in bivalve glass bottle water sample, analysis aquatic dissolved gas's chemistry and stable isotope constitute's purpose, not only simple, convenient, economy, the degasification process is visual moreover, and it is all available to deviate from gas, and measuring result is more accurate.
Description
Technical Field
The utility model relates to a preparation and analysis method of dissolved gas in water in the field of gas geochemistry, in particular to an extraction device of dissolved gas in a high-vacuum double-valve glass bottle water sample.
Background
The water-soluble gas is an important unconventional natural gas resource and is abundant in resource quantity worldwide. In the process of natural gas exploitation, water-soluble gas can become the supply gas of the gas reservoir, and contributes to the total reserve and recovery ratio of the gas reservoir. The solubility of natural gas in water is influenced by temperature, pressure and formation water mineralization, and the chemical composition and stable isotope composition of the dissolved gas in water have practical significance for analyzing the dissolution mechanism of natural gas in water and researching the solubility of natural gas in formation water and the influence of water-soluble gas on gas reservoir reserves and recovery ratio.
For water-bearing oil and gas reservoirs, the content of water-soluble gas in formation water cannot be ignored, particularly for high-temperature and high-pressure gas reservoirs, the release of the water-soluble gas in the decompression exploitation process can affect the development indexes of gas fields including natural gas components, and corrosive gas (such as hydrogen sulfide) dissolved in water needs to be evaluated for a gas reservoir development method. For water-flooding natural gas development, the influence of water-soluble gas on the development indexes of a gas field is not negligible.
The research of the dissolved gas in water also relates to the cause of geothermal fluid, and the chemical composition and the stable isotope composition of the dissolved gas in water can judge that geothermal water comes from atmospheric precipitation, sedimentary rock or mantle, obtain the information of geothermal water circulation mechanism, heat source and the like, and have important significance for the exploration, development and comprehensive utilization of geothermal resources.
The hydraulic fracturing and wastewater reinjection in the shale gas exploitation process can bring environmental problems, and the identification of potential underground water pollution is of great significance. Potential pollution of groundwater by shale gas development is mainly pollution by gas components and dissolved metal or nonmetal compound components. The chemical composition of methane and rare gas dissolved in underground water and the stable isotope composition thereof can be used for judging the source of methane gas, analyzing the share of different source substances, and researching the pollution of dissolved metal or nonmetal compound components by comparing and analyzing the geochemical characteristics of shale water and the dissolved gas in shallow underground water.
Research on the absorption and emission of greenhouse gases (such as methane, carbon dioxide and nitrous oxide) by rainwater and surface water is also an important aspect of ecological environment improvement and improvement research, and the analysis of the concentration and stable isotope composition of the greenhouse gases dissolved in the water helps to trace the sources of the greenhouse gases and adopt targeted management.
The analysis method of dissolved gas in water is more, and the field collection of water samples and the indoor degassing analysis are important modes. In order to facilitate vacuum degassing of water samples, metal (such as red copper) tubes or double-valve glass sampling tubes are commonly used at home and abroad to collect the water samples. The operation of collecting water samples by a metal (such as red copper) pipe is complex, and the requirement on an indoor vacuum degassing device is high. The double-valve glass sampling tube is simple and convenient in water sample collection and the indoor degassing device is low in cost, and the degassing process is visual.
The prior double-valve glass bottle adopts a rubber tube connection mode and a low vacuum system for degassing, has the defects of long degassing time, incomplete degassing, incapability of collecting all the degassing gas for analysis and research and the like, reduces the reliability of a measurement result due to air mixed dyeing generated by low vacuum degree, and has no locking device for a ground glass valve.
SUMMERY OF THE UTILITY MODEL
The utility model aims to solve the technical problem that an extraction device of dissolved gas in high vacuum double-valve glass bottle water sample that is simple, convenient, economic, measure accurate is provided.
In order to solve the problem, the utility model relates to an extraction element of dissolved gas in high vacuum bivalve glass bottle water sample, its characterized in that: the device comprises a double-valve glass bottle I, a double-valve glass bottle II, a high vacuum system and a gas measuring instrument; the lower end of the double-valve glass bottle I is connected with the high vacuum system through a high vacuum joint I, and the upper end of the double-valve glass bottle I is connected with the double-valve glass bottle II through a high vacuum joint II; a heating sheet is arranged on the outer side of the double-valve glass bottle I; the upper end of the double-valve glass bottle II is connected with the gas measuring instrument sequentially through the high vacuum joint III and the metal high vacuum valve; and the double-valve glass bottle I and the double-valve glass bottle II are both provided with locking devices.
The locking device comprises a clamp and a spring; the clamp is arranged at the tail end of a handle rod of a ground glass valve on the double-valve glass bottle I or the double-valve glass bottle II, and the spring is arranged on the handle rod between the clamp and a valve body of the ground glass valve.
The lower end of the double-valve glass bottle I is provided with a ground glass valve I, and the upper end of the double-valve glass bottle I is provided with a ground glass valve II; and the ground glass valve I and the ground glass valve II are both provided with the locking devices.
A ground glass valve III is arranged at the lower end of the double-valve glass bottle II, and a ground glass valve IV is arranged at the upper end of the double-valve glass bottle II; and the ground glass valve III and the ground glass valve IV are both provided with the locking devices.
Compared with the prior art, the utility model has the following advantage:
1. the utility model discloses a high vacuum system and high vacuum connected mode have reduced the air and have mixed the dyeing.
2. The utility model discloses the degasification in-process, to the bivalve glass bottle heating of lower part, make during the bivalve glass bottle that deviates from gas all shifts to upper portion to the water in the bivalve glass bottle is whole to be replaced for gas, makes the aquatic solution gas deviate from more completely, deviates from the gas all on the upper portion of water, and the high-usage.
3. The utility model discloses well ground glass valve is equipped with locking device, makes valve (piston) of bivalve glass bottle not hard up or drop in sampling, transportation, storage and analytic process.
4. The utility model discloses can realize deviating from under the high vacuum and collect dissolved gas in bivalve glass bottle water sample, analysis aquatic dissolved gas's chemistry and stable isotope constitute's purpose, not only simple, convenient, economy, the degasification process is visual moreover, and it is all available to deviate from gas, and measuring result is more accurate.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
Fig. 1 is a schematic structural diagram of the present invention.
Fig. 2 is a schematic view of the middle locking device of the present invention.
In the figure: 1-double-valve glass bottle I; 11-ground glass valve I; 12-ground glass valve II; 2-double-valve glass bottle II; 21-ground glass valve III; 22-ground glass valve IV; 3-high vacuum system; 31-high vacuum joint I; 32-high vacuum joint II; 33-high vacuum connection III; 4-a gas measuring instrument; 5-metal high vacuum valve; 6-heating plate; 7, a clamp; 8, a spring; 9-handle stem.
Detailed Description
As shown in fig. 1-2, the device for extracting the dissolved gas in the water sample of the high-vacuum double-valve glass bottle comprises a double-valve glass bottle I1, a double-valve glass bottle II 2, a high-vacuum system 3 and a gas measuring instrument 4. The double-valve glass bottle I1 and the double-valve glass bottle II 2 are of customized standard sizes. The gas measurement instrument 4 operates in a vacuum sample injection mode.
The lower end of the double-valve glass bottle I1 is connected with a high vacuum system 3 through a high vacuum joint I31, and the upper end of the double-valve glass bottle I1 is connected with a double-valve glass bottle II 2 through a high vacuum joint II 32; and a heating sheet 6 is arranged on the outer side of the double-valve glass bottle I1. The upper end of the double-valve glass bottle II 2 is connected with a gas measuring instrument 4 sequentially through a high vacuum joint III 33 and a metal high vacuum valve 5; and locking devices are arranged on the double-valve glass bottle I1 and the double-valve glass bottle II 2.
Wherein: the locking device comprises a clamp 7 and a spring 8; the clamp 7 is arranged at the tail end of a handle rod 9 of the ground glass valve on the double-valve glass bottle I1 or the double-valve glass bottle II 2, and a spring 8 is arranged on the handle rod 9 between the clamp 7 and the valve body of the ground glass valve.
The lower end of the double-valve glass bottle I1 is provided with a ground glass valve I11, and the upper end of the double-valve glass bottle is provided with a ground glass valve II 12; and locking devices are arranged on the ground glass valve I11 and the ground glass valve II 12.
A ground glass valve III 21 is arranged at the lower end of the double-valve glass bottle II 2, and a ground glass valve IV 22 is arranged at the upper end of the double-valve glass bottle II; and locking devices II are arranged on the ground glass valve III 21 and the ground glass valve IV 22.
The high vacuum joint I31, the high vacuum joint II 32 and the high vacuum joint III 33 are all U-Torr type ultrahigh vacuum joints.
The joint positions of the double-valve glass bottle I1, the double-valve glass bottle II 2, the high-vacuum joint I31, the high-vacuum joint II 32 and the high-vacuum joint III 33 are all standard sizes.
The double-valve glass bottle I1, the double-valve glass bottle II 2, the high vacuum joint I31, the high vacuum joint II 32, the high vacuum joint III 33, the ground glass valve I11, the ground glass valve II 12, the ground glass valve III 21 and the ground glass valve IV 22 all have high vacuum airtightness.
An extraction method of a device for extracting dissolved gas in a high-vacuum double-valve glass bottle water sample comprises the following steps:
the method comprises the steps of installing an empty double-valve glass bottle I1 and a double-valve glass bottle II 2 filled with a water sample to be detected in place.
Opening the high vacuum system 3, opening a ground glass valve I11 and a ground glass valve II 12, and simultaneously enabling the gas measuring instrument 4 to be in a state of vacuumizing a sample inlet; and opening the metal high vacuum valve 5 and vacuumizing.
After the vacuum degree meets the set requirement, the ground glass valve I11 is closed, the ground glass valve III 21 is opened, water in the double-valve glass bottle II 2 flows into the double-valve glass bottle I1 under the driving of pressure difference and gravity, and vacuum degassing is realized at the same time.
When the water in the double-valve glass bottle II 2 does not flow into the double-valve glass bottle I1 any more, the heating sheet 6 is adopted to slightly heat the double-valve glass bottle I1, and the gas in the double-valve glass bottle I1 flows into the double-valve glass bottle II 2.
And fifthly, heating the double-valve glass bottle I1 is cancelled, and water in the double-valve glass bottle II 2 flows into the double-valve glass bottle I1 again under the driving of pressure difference and gravity.
Sixthly, repeating the fourth step and the fifth step until all water in the double-valve glass bottle II 2 is replaced by gas; and water in the double-valve glass bottle II 2 is completely replaced by gas, so that dissolved gas in water is completely removed, the removed gas is completely arranged on the upper part of the water, and the utilization rate is high.
And closing the metal high vacuum valve 5, and opening the ground glass valve IV 22 to enable the gas measuring instrument 4 to be in a sample injection state.
And opening the metal high vacuum valve 5, introducing the gas sample into the gas measuring instrument 4, and measuring the geochemical parameters of each gas.
Example 1 illustrates the measurement of the chemical composition of the solution gas in water of a geothermal water sample.
The joint positions of a 250mL double-valve glass bottle, a double-valve glass bottle I1, a double-valve glass bottle II 2, a high vacuum joint I31, a high vacuum joint II 32 and a high vacuum joint III 33 are all suitable for 8mm pipe diameters, and high vacuum silicone grease is smeared on the ground surfaces of all ground glass valves to play a role in sealing and lubricating.
During sampling, the double-valve glass bottle II 2 can be vertically or obliquely placed, the ground glass valve III 21 and the ground glass valve IV 22 of the double-valve glass bottle II 2 are opened, a liquid sampling pump is used for introducing a water sample into the double-valve glass bottle II 2, after the water sample is fully sampled, the liquid sampling pump is closed, the ground glass valve III 21 is closed, and then the ground glass valve IV 22 is closed. The gas measuring instrument 4 is a high vacuum and pulse discharge gas chromatography combined device. The degassing analysis was performed indoors, using a three-legged table, a retaining clip, and a flask clip to mount the components of fig. 1.
An extraction method of a device for extracting dissolved gas in a high-vacuum double-valve glass bottle water sample comprises the following steps:
the method comprises the steps of installing an empty double-valve glass bottle I1 and a double-valve glass bottle II 2 filled with a water sample to be detected in place. The metal high vacuum valve 5 is connected with a gas sample inlet of the high vacuum and pulse discharge gas chromatography combined device through a high vacuum metal pipeline.
Opening a high vacuum system 3, opening a ground glass valve I11 and a ground glass valve II 12, and simultaneously enabling the high vacuum and pulse discharge gas chromatography combined device to be in a vacuum pumping state on a gas injection port of the high vacuum and pulse discharge gas chromatography combined device; and opening the metal high vacuum valve 5 and vacuumizing.
Thirdly, when the vacuum degree of the high vacuum system 3 reaches less than 0.01Pa, the ground glass valve I11 is closed, the ground glass valve III 21 is opened, water in the double-valve glass bottle II 2 flows into the double-valve glass bottle I1 under the driving of pressure difference and gravity, and vacuum degassing is realized.
When the water in the double-valve glass bottle II 2 does not flow into the double-valve glass bottle I1 any more, the heating sheet 6 is adopted to slightly heat the double-valve glass bottle I1, and the gas in the double-valve glass bottle I1 flows into the double-valve glass bottle II 2.
The heating temperature is below 60 ℃, the heating time is only 1min, and attention is paid to avoid boiling of water in the double-valve glass bottle I1 caused by overhigh heating temperature. Description of the drawings: the heating sheet can also be replaced by an electric heating blower.
And fifthly, heating the double-valve glass bottle I1 is cancelled, and water in the double-valve glass bottle II 2 flows into the double-valve glass bottle I1 again under the driving of pressure difference and gravity.
Sixthly, repeating the fourth step and the fifth step until all water in the double-valve glass bottle II 2 is replaced by gas.
And closing the metal high vacuum valve 5, and opening the ground glass valve IV 22 to enable the gas measuring instrument 4 to be in a sample injection state.
And opening the metal high vacuum valve 5, introducing the gas sample into the gas measuring instrument 4, and analyzing the chemical composition of the gas.
Example 2 illustrates the measurement of the chemical and stable isotope composition of noble gases in water of geothermal water samples.
The joint positions of a 250mL double-valve glass bottle, a double-valve glass bottle I1, a double-valve glass bottle II 2, a high vacuum joint I31, a high vacuum joint II 32 and a high vacuum joint III 33 are all suitable for 8mm pipe diameters, and high vacuum silicone grease is smeared on the ground surfaces of all ground glass valves to play a role in sealing and lubricating.
During sampling, the double-valve glass bottle II 2 can be vertically or obliquely placed, the ground glass valve III 21 and the ground glass valve IV 22 of the double-valve glass bottle II 2 are opened, a liquid sampling pump is used for introducing a water sample into the double-valve glass bottle II 2, after the water sample is fully sampled, the liquid sampling pump is closed, the ground glass valve III 21 is closed, and then the ground glass valve IV 22 is closed. The gas measurement instrument 4 is a noblese rare gas mass spectrometer system. The degassing analysis was performed indoors, using a three-legged table, a retaining clip, and a flask clip to mount the components of fig. 1.
An extraction method of a device for extracting dissolved gas in a high-vacuum double-valve glass bottle water sample comprises the following steps:
the method comprises the steps of installing an empty double-valve glass bottle I1 and a double-valve glass bottle II 2 filled with a water sample to be detected in place. The metal high vacuum valve 5 is connected with a sample introduction and purification device of a noblese rare gas mass spectrometer system through a high vacuum metal pipeline.
Opening the high vacuum system 3, opening a ground glass valve I11 and a ground glass valve II 12, and simultaneously enabling a sample introduction and purification device of the nobilese rare gas mass spectrometer system to be in a vacuum pumping state; and opening the metal high vacuum valve 5 and vacuumizing.
Thirdly, when the vacuum degree of the high vacuum system 3 reaches less than 0.01Pa, the ground glass valve I11 is closed, the ground glass valve III 21 is opened, water in the double-valve glass bottle II 2 flows into the double-valve glass bottle I1 under the driving of pressure difference and gravity, and vacuum degassing is realized.
When the water in the double-valve glass bottle II 2 does not flow into the double-valve glass bottle I1 any more, the heating sheet 6 is adopted to slightly heat the double-valve glass bottle I1, and the gas in the double-valve glass bottle I1 flows into the double-valve glass bottle II 2.
The heating temperature is below 60 ℃, the heating time is only 1min, and attention is paid to avoid boiling of water in the double-valve glass bottle I1 caused by overhigh heating temperature. Description of the drawings: the heating sheet can also be replaced by an electric heating blower.
And fifthly, heating the double-valve glass bottle I1 is cancelled, and water in the double-valve glass bottle II 2 flows into the double-valve glass bottle I1 again under the driving of pressure difference and gravity.
Sixthly, repeating the fourth step and the fifth step until all water in the double-valve glass bottle II 2 is replaced by gas.
And closing the metal high vacuum valve 5, and opening a ground glass valve IV 22 to enable a sample introduction purification device of the noble rare gas mass spectrometer system to be in a sample introduction state.
And opening a metal high vacuum valve 5, introducing the gas sample into a sample introduction and purification device of a noblese rare gas mass spectrometer system, and purifying and analyzing the rare gas chemistry and stable isotope composition of the dissolved gas in the water.
Claims (4)
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113908591A (en) * | 2020-07-07 | 2022-01-11 | 中国科学院西北生态环境资源研究院 | Device and method for extracting dissolved gas in water sample of high-vacuum double-valve glass bottle |
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2020
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113908591A (en) * | 2020-07-07 | 2022-01-11 | 中国科学院西北生态环境资源研究院 | Device and method for extracting dissolved gas in water sample of high-vacuum double-valve glass bottle |
CN113908591B (en) * | 2020-07-07 | 2023-03-17 | 中国科学院西北生态环境资源研究院 | Device and method for extracting dissolved gas in water sample of high-vacuum double-valve glass bottle |
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