CN113884645A - Device is prepared to methane henry constant standard in experimental water - Google Patents
Device is prepared to methane henry constant standard in experimental water Download PDFInfo
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- CN113884645A CN113884645A CN202111079038.9A CN202111079038A CN113884645A CN 113884645 A CN113884645 A CN 113884645A CN 202111079038 A CN202111079038 A CN 202111079038A CN 113884645 A CN113884645 A CN 113884645A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 126
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 239000007789 gas Substances 0.000 claims abstract description 82
- 239000007788 liquid Substances 0.000 claims abstract description 72
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 229910052786 argon Inorganic materials 0.000 claims abstract description 8
- 238000009826 distribution Methods 0.000 claims description 46
- 238000005070 sampling Methods 0.000 claims description 31
- 238000012512 characterization method Methods 0.000 claims description 19
- 238000012545 processing Methods 0.000 claims description 14
- 230000007246 mechanism Effects 0.000 claims description 13
- 230000001502 supplementing effect Effects 0.000 claims description 11
- 238000007789 sealing Methods 0.000 claims description 9
- 230000010355 oscillation Effects 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
- 239000000243 solution Substances 0.000 description 15
- 238000002474 experimental method Methods 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- 238000002372 labelling Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 238000000638 solvent extraction Methods 0.000 description 5
- 239000011550 stock solution Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005192 partition Methods 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002457 bidirectional effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011067 equilibration Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002500 ions Chemical group 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000009489 vacuum treatment Methods 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
- G01N33/18—Water
-
- 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—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
- G01N33/0047—Organic compounds
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Medicinal Chemistry (AREA)
- Food Science & Technology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Pathology (AREA)
- Combustion & Propulsion (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a device for preparing a methane Henry constant standard in experimental water, which comprises: a raw water treatment module which is provided with a raw water treatment tank and a heating module which is arranged in the raw water treatment tank and heats liquid in the raw water treatment tank; the mark adding treatment module is provided with a treatment cavity, a mark adding assembly, an oscillating device and a constant temperature device, the treatment cavity is connected with the raw water treatment tank through a pipeline, and the mark adding assembly is used for performing methane mark gas with preset solubility on the solution in the treatment cavity; the oscillating device is used for oscillating the solution in the treatment cavity added with the methane standard gas with preset concentration, and the constant temperature device is used for heating or preserving the solution in the treatment cavity added with the methane standard gas with preset concentration at a set temperature; the gas supply module is communicated with the raw water treatment tank and the treatment cavity through pipelines and is used for introducing argon into the solutions in the raw water treatment tank and the treatment cavity.
Description
Technical Field
The invention relates to the technical field of measuring methane water solution, in particular to a preparation device for a Henry constant standard of methane in experimental water.
Background
With the continuous upgrading and deepening of water environment, marine environment and resource investigation, the content of dissolved methane in water draws the attention of many scientists. The solubility of gas in water mainly depends on the strength of gap filling and hydration, the composition of solute is different, the strength of gap filling and hydration is different, and the corresponding henry constants under different temperatures and pressures are different. Various types of water such as river water, lake water, sea water, distilled water, purified water, ultrapure water, deionized water, tap water, sewage, and the like, in which the components are not completely the same, are precisely solutes of different kinds, in which the henry constant of methane is not completely the same, and the size of the henry constant is closely related to the components of the solutes, and thus it is difficult to characterize the henry constant of methane in water using uniform data.
In order to measure the methane concentration in water with high precision, the content of methane in the water needs to be measured in advance, and the henry constant is represented according to the set parameter conditions. The experimental determination process of the henry constant of methane in different solutes is complex, and the preparation and treatment methods of experimental raw water with different solutes in different environments are different, so that the henry constant parameters of methane in different solutes are difficult to accurately express under different parameter standards and environments due to different settings.
It is therefore difficult to obtain a universal standard experimental stock of aqueous methane solution to characterize the henry constant measurements.
Disclosure of Invention
The invention aims to provide a device for preparing a standard of a Henry constant of methane in experimental water, which aims to solve the technical problem that parameters of the Henry constant of methane in different solutes are not uniformly characterized in the prior art.
In order to solve the technical problems, the invention specifically provides the following technical scheme:
a device for preparing a methane Henry constant standard in experimental water comprises:
a raw water treatment module which is provided with a raw water treatment tank and a heating module which is arranged in the raw water treatment tank and heats liquid in the raw water treatment tank;
the system comprises a mark adding treatment module, a mark adding assembly, an oscillation device and a constant temperature device, wherein the mark adding treatment module is provided with a treatment cavity, a mark adding assembly, an oscillation device and a constant temperature device, the treatment cavity is connected with a raw water treatment tank through a pipeline with a valve, the treatment cavity is used for receiving a solution transferred by the raw water treatment tank, and the mark adding assembly is used for performing methane mark gas with preset solubility on the solution in the treatment cavity;
the oscillating device is arranged at the bottom of the treatment cavity and is used for oscillating the solution in the treatment cavity added with the methane standard gas with preset concentration, the constant temperature device is arranged in the treatment cavity and is used for heating or preserving the solution in the treatment cavity added with the methane standard gas with preset concentration at a set temperature;
the gas supply module, through the pipeline with in the raw water treatment tank with the process chamber intercommunication, just the gas supply module be used for to the raw water treatment tank with the solution in the process chamber lets in argon gas.
As a preferred scheme of the invention, the raw water treatment tank comprises a raw water tank body and a raw water tank cover body arranged on the raw water tank body, a liquid distribution cavity is arranged in the raw water tank body, the gas supply module is used for supplying gas into the liquid distribution cavity, and the liquid distribution cavity is communicated with the treatment cavity through a pipeline with a valve;
and the cover body of the raw water tank is provided with a pressure control valve which is used for changing the pressure of a cavity positioned at the upper part of the liquid level in the liquid distribution cavity by matching with the pressure in the liquid distribution cavity provided by the gas supply module.
As a preferable scheme of the present invention, the raw water tank includes, from top to bottom, a first liquid distribution cavity containing the experimental raw water and a second liquid distribution cavity not containing the experimental raw water, the two liquid distribution cavities are connected by a balance structure, the balance structure is configured to transport the experimental raw water treated in the first liquid distribution cavity to the second liquid distribution cavity, and the second liquid distribution cavity is connected to the treatment cavity by a pipeline with a valve.
As a preferable scheme of the invention, the treatment cavity comprises a tank body and a cover body arranged on the tank body, the bottom of the tank body is provided with a water inlet valve pipe and a gas inlet, the cover body is radially provided with a gas outlet valve, a vacuum pumping valve and a first sampling valve arranged in the middle of the tank body, and the tank body is internally provided with a pressure supplementing mechanism which is used for forcing gas in the tank body to escape from the first sampling valve in an inflation mode.
As a preferable scheme of the present invention, a partitioning assembly is disposed inside the tank body, the partitioning assembly is configured to partition a cavity inside the tank body into an error characterization cavity located at an upper portion of the partitioning assembly and an experiment operation cavity located at a lower portion of the partitioning assembly, the partitioning assembly is configured to actively or passively communicate the error characterization cavity and the experiment operation cavity, and the pressure compensating mechanism is disposed in the experiment operation cavity.
As a preferable scheme of the present invention, the dividing assembly includes a plate body hermetically connected to an inner wall of the tank body, an edge of the plate body is connected to the inner wall of the tank body through a movable sealing rubber ring, the plate body is provided with an array valve group, and a circle center of the plate body is provided with a second sampling valve located on the same axis as the first sampling valve.
As a preferable scheme of the present invention, the valve set operates by receiving an external control signal, so that the error characterization chamber is communicated with the experimental operation chamber;
or the valve group works after the relative pressure of the error representation cavity and the experiment operation cavity reaches a set limit value, so that the error representation cavity is communicated with the experiment operation cavity.
As a preferable scheme of the present invention, the dividing assembly is movably mounted on an inner wall of the tank body through an adjusting assembly, the adjusting assembly is used for adjusting the dividing assembly to be located at upper and lower positions in the tank body, and the dividing assembly is provided with a second sampling valve used for being matched with the first sampling valve.
As a preferable scheme of the invention, the pressure supplementing mechanism comprises a bag body located in the experiment operation cavity, and an air inlet opening of the bag body is hermetically mounted on the inner wall of the tank body through a two-way valve.
Compared with the prior art, the invention has the following beneficial effects:
the method is characterized in that raw water for testing and standard methane gas are placed in an environment assembly in a gas-liquid balance manner, trace amount and preparation of raw water for testing are carried out in a single environment, and under the condition that the composition of ions and gas in the raw water is controlled in a single manner, the raw water for testing is added and calibrated with methane standard gas with various calibration concentrations, so that the standard Henry constants of the methane standard gas with various calibration concentrations in the raw water for testing are obtained, and the representation of the Henry constants of other existing solutes can be realized through the standard Henry constants.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary, and that other embodiments can be derived from the drawings provided by those of ordinary skill in the art without inventive effort.
FIG. 1 is a schematic structural diagram of a raw liquid water preparing apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a preparation apparatus having a first liquid preparation chamber and a second liquid preparation chamber according to an embodiment of the present invention;
fig. 3 is a schematic structural diagram of a tagging processing element according to an embodiment of the present invention.
The reference numerals in the drawings denote the following, respectively:
1-tank body; 2-a raw water tank cover body; 3-a water inlet valve pipe; 4-an air inlet; 5-an exhaust valve; 6-vacuum-pumping valve; 7-a first sampling valve; 8-a pressure supplementing mechanism; 9-a segmentation component; 10-a regulating component; 11-a second sampling valve; 12-raw water treatment module; 13-a gas supply module; 14-a first liquid preparation cavity; 15-a second liquid preparation cavity; 16-a balanced structure; 17-heating module; 18-a tagging processing module; 19-a treatment chamber; 20-a tagging component; 21-an oscillating device; 22-raw water treatment tank; 23-a thermostatic device; 121-liquid preparation cavity; 122-a raw water tank cover body; 123-a raw water tank body;
81-capsule body; 82-an air inlet opening; 83-a two-way valve;
91-error characterization chamber; 92-experimental operation cavity; 93-a plate body; 94-movable sealing rubber ring; 95-valve set.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in FIG. 1, the invention provides a device for preparing a methane Henry constant standard in experimental water, which comprises:
a raw water treatment module 12 including a raw water treatment tank 22 and a heating module 17 provided in the raw water treatment tank for heating a liquid in the raw water treatment tank 22;
the labeling processing module 18 is provided with a processing cavity 19, a labeling component 20, an oscillating device 21 and a constant temperature device 23, the processing cavity 19 is connected with a raw water processing tank 22 through a pipeline with a valve, the processing cavity 19 is used for receiving a solution transferred by the raw water processing tank 22, and the labeling component 20 is used for performing methane labeling gas with preset solubility on the solution in the processing cavity;
the oscillating device 21 is arranged at the bottom of the processing cavity 19, the oscillating device 21 is used for oscillating the solution in the processing cavity added with the methane standard gas with preset concentration, the constant temperature device 23 is arranged in the processing cavity 19, and the constant temperature device 23 is used for heating or preserving the solution in the processing cavity 22 added with the methane standard gas with preset concentration at a set temperature;
the gas supply module 13 is communicated with the interior of the raw water treatment tank 22 and the treatment cavity 19 through pipelines, and the gas supply module 13 is used for introducing argon gas into the solutions in the raw water treatment tank 22 and the treatment cavity 19.
The raw water treatment tank 12 comprises a raw water tank body 123 and a raw water tank cover body 122 arranged on the raw water tank body 123, a liquid distribution cavity 121 is arranged in the raw water tank body 122, the gas supply module 13 is used for supplying gas into the liquid distribution cavity 121, and the liquid distribution cavity 121 is communicated with the treatment cavity 19 through a pipeline with a valve;
the raw water tank cover 122 is provided with a pressure control valve for changing the pressure of a cavity positioned above the liquid level in the liquid distribution cavity 121 in cooperation with the pressure in the liquid distribution cavity 121 provided by the gas supply module 13.
The raw water tank 123 comprises a first liquid distribution cavity 14 containing experimental raw water and a second liquid distribution cavity 15 not containing experimental raw water from top to bottom, the two liquid distribution cavities 121 are connected through a balance structure 16, the balance structure 16 is used for conveying the treated experimental raw water in the first liquid distribution cavity 14 to the second liquid distribution cavity 15, and the second liquid distribution cavity 15 is connected with a treatment cavity 19 through a pipeline with a valve.
When the stock solution water is prepared, the raw water treatment tank 22 and the treatment cavity 19 are pumped to vacuum negative pressure through a vacuum system, air in the cavities of the raw water treatment tank 22 and the treatment cavity 19 is displaced and removed through an argon gas supply system provided by the gas supply module 13, the raw water treatment module 12 is heated through the heating module 17 to carry out boiling dissipation on experimental raw water (specifically pure water), and then the gas supply module 13 carries out argon purging on the solution in the raw water treatment tank 22 to remove methane, so that the experimental stock solution is obtained.
Collecting gas in the raw water treatment module 12, detecting the gas content through gas chromatography, repeating the heating step if carbon dioxide is detected, repeating purging in the raw water treatment module 12 through the gas supply module 13 if methane is detected, then introducing the stock solution into the treatment cavity 19 of the labeling treatment module 18, adding methane standard gas with preset concentration into the experimental stock solution through the labeling assembly 20, starting heating by the constant temperature water device 23 after oscillation of the oscillation device to reach the set constant temperature target temperature, keeping the target stable for a period of time, and enabling the treatment cavity 19 to reach a gas-liquid equilibrium state to prepare stock solution water for measuring the Henry constant.
The raw water treatment module 12 comprises at least one liquid distribution cavity 121 connected with the gas supply module 13 and a raw water tank cover 122 used for sealing the liquid distribution cavity, and the gas supply module 13 is used for supplying ambient gas into the liquid distribution cavity 121;
the raw water tank cover 122 is used for actively or passively changing the pressure of a cavity located above the liquid level in the liquid distribution cavity 121 in cooperation with the pressure change in the liquid distribution cavity 121 provided by the gas supply module 13.
As shown in fig. 2 and fig. 3, further, the raw water treatment tank 123 of the present invention includes a first liquid distribution cavity 14 containing experimental raw water and a second liquid distribution cavity 15 not containing experimental raw water, the two liquid distribution cavities 121 are connected by a balance structure 16, wherein the balance structure 16 may be specifically a peristaltic pump or a micro pump capable of performing bidirectional transportation, a pipeline connecting the two liquid distribution cavities 121 is a circulating pipeline capable of performing circulating transportation of liquid in the two liquid distribution cavities, and the balance structure 16 is configured to transport the treated experimental raw water to the second liquid distribution cavity 15 after the gas supply module 13 performs gas supply and heating of the ambient gas to the first liquid distribution cavity 14.
The treatment cavity 19 specifically comprises a tank body 1 and a cover body 2 arranged on the tank body 1, wherein the bottom of the tank body 1 is provided with a water inlet valve pipe 3 and an air inlet 4 connected with a labeling component 20, the cover body 2 is radially provided with an exhaust valve 5, a vacuum pumping valve 6 and a first sampling valve 7 arranged in the middle of the tank body 1, the tank body 1 is internally provided with a pressure supplementing mechanism 8, and the pressure supplementing mechanism 8 is used for forcing gas in the tank body to escape from the first sampling valve 7 in an inflation mode.
The marking assembly 20 may be a needle tube or a sampling needle.
The pressure supplementing mechanism 8 is specifically an air bag with a port arranged on the inner wall of the tank body 1, the air bag is arranged on the inner wall of the tank body 1 through a two-way valve, the air bag and a cavity in the tank body 1 are in an absolutely independent sealing state, and air supply is carried out through an external air source.
Furthermore, in the invention, in order to enable the measuring device to adapt to the gradient variation of the headspace methane content in a wider range during balance, and to change the experimental parameters in a variable tank volume mode to obtain more accurate measuring parameters, the data error can be rapidly and conveniently calculated.
The inner part of the tank body 1 is provided with a dividing assembly 9, the dividing assembly 9 is used for dividing the cavity in the tank body 1 into an error representation cavity 91 positioned at the upper part of the dividing assembly 9 and an experiment operation cavity 92 positioned at the lower part of the dividing assembly 9, the dividing assembly 9 is used for communicating the error representation cavity 91 and the experiment operation cavity 92 in an active or passive mode, and the pressure supplementing mechanism 8 is arranged in the experiment operation cavity 92;
the dividing component 9 is movably arranged on the inner wall of the tank body 1 through an adjusting component 10, the adjusting component 10 is used for adjusting the upper position and the lower position of the dividing component 9 in the tank body, and a second sampling valve 11 used for being matched with the first sampling valve 7 is arranged on the dividing component 9.
In S200, then injecting high-purity argon into the cavities at the upper part of the liquid until the pressure of all the cavities reaches a set value, exhausting through an exhaust valve to enable the error characterization cavity to be in a negative pressure state until the error characterization cavity and the experimental operation cavity are just not communicated, and enabling the pressure in the experimental operation cavity to reach the set value.
The cutting assembly 9 comprises a plate body 93 which is connected with the inner wall of the tank body in a sealing way, the edge of the plate body 93 is connected on the inner wall of the tank body 1 through a movable sealing rubber ring 94, an array valve group 95 is arranged on the plate body 93, and the circle center of the plate body 93 is provided with a second sampling valve 11 which is positioned on the same axis with the first sampling valve 7;
wherein, the valve group 95 works by receiving an external control signal, so that the error characterization cavity is communicated with the experiment operation cavity;
or, the valve set 95 works after the relative pressures of the error characterization chamber 91 and the experimental operation chamber 92 reach the set limit value, so that the error characterization chamber 91 is communicated with the experimental operation chamber 92.
The specific principle is that, at a constant capacity, the pressure increase caused by filling with an inert gas such as a rare gas does not affect the balance. When other conditions are unchanged, the rising temperature equilibrium shifts in the direction of the endothermic reaction and the lower temperature equilibrium shifts in the direction of the exotherm. The catalyst can only shorten the time required to reach equilibrium and cannot change the equilibrium state.
In a reaction in which a gas participates, a gas is generated, and the number of gas molecules before and after the reaction changes, when other conditions are not changed, the pressure increases (the pressure of the compressed gas volume increases), and the equilibrium moves in the direction of the gas volume decreasing; decreasing the pressure (increasing the gas volume to decrease the pressure) the equilibrium shifts in the direction of increasing gas volume. Therefore, the invention does not consider the weight of the plate body.
In the invention, when the CH4 sampling measuring instrument is used for sampling the headspace gas in the experimental operation cavity, the needle head part of the sampling instrument can sequentially pass through the first sampling valve 7 and the second sampling valve 11 to sample and measure the headspace gas in the experimental operation cavity, when the sampling instrument is taken out, the headspace gas can be sequentially taken out from the second sampling valve 11 and the first sampling valve 7, the first sampling valve 7 and the second sampling valve 11 are immediately closed when being separated from the needle head part, and the gas possibly generated in the experimental operation cavity 92 can escape into the error characterization cavity to become the error parameter in the error characterization cavity 91.
Further, the adjusting assembly 10 of the present invention may be a permanent magnet ring structure disposed on the tank body 1, and the plate body 93 is made of metal, so that the position of the plate body 93 can be adjusted by the adjusting assembly 10, and the plate body 93 can be in a suspended state, and can more specifically represent the pressure changes in the error characterization chamber and the experimental operation chamber, and the position changes when the plate body is in a gas-liquid balance system in the experimental process, and further represent the volume changes of the error characterization chamber and the experimental operation chamber in the experimental process, and by superimposing a hall sensor on the permanent magnet ring structure, the adjusting position of the plate body 93 can be known.
Or, the adjusting assembly 10 in the present invention is a screw-nut pair transmission assembly, and the position of the plate body 93 is adjusted manually, so that a measurer manually changes the position of the plate body 93, thereby changing experimental parameters, rapidly obtaining experimental parameters under different gas-liquid equilibrium volumes, and reducing steps of error calibration.
In this experimental protocol. The measuring device has the advantages of good sealing performance, capability of monitoring the headspace pressure in the bin in real time, capability of conveniently adding quantitative standard gas and capability of realizing the transfer of the headspace gas on the premise of not changing the headspace gas pressure and the whole volume. Without destroying the balance of gas and liquid in the closed system.
The CH4 analyzer can measure tens to thousands of times for the same error characterization chamber, and the average value of the most stable data part is taken as the measured value of the sample. As opposed to gas chromatography. Has higher accuracy and lower detection limit. The method is suitable for mixed gas samples with methane content lower than or higher than 1 x 10 < -6 >.
Due to the difference in the equilibration time. The effect of headspace gas-liquid balance in the balance system can be influenced, and the concentration of the gas in the gas-phase mixed gas can be influenced. The time is too short. The target gas cannot be effectively volatilized into the gas phase. A stable equilibrium is not reached. Too long a time can extend the time and error of the experimental analysis.
For example: taking 6 gas-liquid equilibrium liquid distribution devices which are subjected to vacuum treatment. 2.5L of test water were introduced. And 99.999% of high-purity argon gas is filled. To an internal pressure of 101325 Pa. Shaking for 30 min. Then simultaneously placing the mixture into a constant-temperature water tank at 25 ℃ for standing. Every interval of 1 h. A headspace gas sample was taken from a dispensing unit for methane content testing. And (6) displaying the result. The variation range of the headspace methane content is large within the range of 1-2 h, which indicates that the time is within the range. The methane gas in the closed system does not reach the gas-liquid balance yet. And after 2 h. The headspace methane concentration in the closed system remained essentially constant. Indicating that the system had reached equilibrium after 2 h. Therefore, 25 ℃ was one atmosphere. The methane gas in the closed system needs at least 2 hours to reach gas-liquid balance. In the invention, the volume of the experimental operation cavity can be synchronously adjusted through the partition assembly 9, so that the system balance time can be accelerated or increased or more gas-liquid balance parameter synchronous adjustment modes can be provided.
Illustratively, the pressure compensating mechanism 8 comprises a bladder 81 located in the experimental operation chamber 92, and an air inlet 82 of the bladder 81 is hermetically mounted on the inner wall of the tank 1 through a two-way valve 83.
The above embodiments are only exemplary embodiments of the present application, and are not intended to limit the present application, and the protection scope of the present application is defined by the claims. Various modifications and equivalents may be made by those skilled in the art within the spirit and scope of the present application and such modifications and equivalents should also be considered to be within the scope of the present application.
Claims (9)
1. A device for preparing a methane Henry constant standard in experimental water is characterized by comprising:
a raw water treatment module (12) which is provided with a raw water treatment tank (22) and a heating module (17) which is arranged in the raw water treatment tank and heats liquid in the raw water treatment tank (22);
the mark adding treatment module (18) is provided with a treatment cavity (19), a mark adding assembly (20), an oscillating device (21) and a constant temperature device (23), the treatment cavity (19) is connected with the raw water treatment tank (22) through a pipeline with a valve, the treatment cavity (19) is used for receiving a solution transferred by the raw water treatment tank (22), and the mark adding assembly (20) is used for performing methane mark gas with preset solubility on the solution in the treatment cavity;
the oscillation device (21) is arranged at the bottom of the treatment cavity (19), the oscillation device (21) is used for oscillating the solution in the treatment cavity added with the methane standard gas with preset concentration, the constant temperature device (23) is arranged in the treatment cavity (19), and the constant temperature device (23) is used for heating or preserving the solution in the treatment cavity (22) added with the methane standard gas with preset concentration at a set temperature;
the gas supply module (13) is communicated with the interior of the raw water treatment tank (22) and the treatment cavity (19) through a pipeline, and the gas supply module (13) is used for introducing argon into the solution in the raw water treatment tank (22) and the treatment cavity (19).
2. The device for preparing the standard of the Henry constant of methane in experimental water as claimed in claim 1, wherein the raw water treatment tank (12) comprises a raw water tank body (123) and a raw water tank cover body (122) arranged on the raw water tank body (123), a liquid distribution cavity (121) is arranged in the raw water tank body (122), the gas supply module (13) is used for supplying gas into the liquid distribution cavity (121), and the liquid distribution cavity (121) is communicated with the treatment cavity (19) through a pipeline with a valve;
the raw water tank cover body (122) is provided with a pressure control valve which is used for matching with the pressure in the liquid distribution cavity (121) provided by the gas supply module (13) to change the pressure of a cavity in the liquid distribution cavity (121) above the liquid level.
3. The device for preparing the standard of the henry constant of methane in the experimental water as claimed in claim 2, wherein the raw water tank (123) comprises a first liquid distribution chamber (14) containing the experimental raw water and a second liquid distribution chamber (15) not containing the experimental raw water from top to bottom, the two liquid distribution chambers (121) are connected through a balance structure (16), the balance structure (16) is used for conveying the treated experimental raw water in the first liquid distribution chamber (14) to the second liquid distribution chamber (15), and the second liquid distribution chamber (15) is connected with the treatment chamber (19) through a pipeline with a valve.
4. The device for preparing the standard of the Henry constant of methane in experimental water as claimed in claim 3, wherein said processing chamber (19) comprises a tank body (1) and a cover body (2) arranged on said tank body (1), the bottom of said tank body (1) is provided with a water inlet valve pipe (3) and a gas inlet (4), the radial direction of said cover body (2) is provided with a gas outlet valve (5), a vacuum pumping valve (6) and a first sampling valve (7) arranged in the middle of said tank body (1), the interior of said tank body (1) is provided with a pressure supplementing mechanism (8), said pressure supplementing mechanism (8) is used for forcing the gas in the tank body to escape from said first sampling valve (7) by inflation.
5. The device for preparing the standard of the henry constant of methane in experimental water as claimed in claim 4, wherein a dividing assembly (9) is arranged inside the tank body (1), the dividing assembly (9) is used for dividing the cavity inside the tank body (1) into an error characterization cavity (91) positioned at the upper part of the dividing assembly (9) and an experimental operation cavity (92) positioned at the lower part of the dividing assembly (9), the dividing assembly (9) is used for communicating the error characterization cavity (91) and the experimental operation cavity (92) in an active or passive mode, and the pressure supplementing mechanism (8) is arranged in the experimental operation cavity (92).
6. The device for preparing the standard of the Henry constant of methane in experimental water as claimed in claim 5, wherein the dividing assembly (9) comprises a plate body (93) connected with the inner wall of the tank body in a sealing manner, the edge of the plate body (93) is connected with the inner wall of the tank body (1) through a movable sealing rubber ring (94), the plate body (93) is provided with an array valve set (95), and the center of the plate body (93) is provided with a second sampling valve (11) which is on the same axis with the first sampling valve (7).
7. The apparatus for preparing a standard of henry constant of methane in experimental water as claimed in claim 6, wherein said valve set (95) is operated by receiving an external control signal to connect said error characterization chamber and said experimental operation chamber;
or the valve group (95) works after the relative pressure of the error characterization cavity (91) and the experimental operation cavity (92) reaches a set limit value, so that the error characterization cavity (91) is communicated with the experimental operation cavity (92).
8. The device for preparing the standard of the Henry constant of methane in experimental water as claimed in claim 5, wherein said dividing assembly (9) is movably mounted on the inner wall of said tank body (1) through an adjusting assembly (10), said adjusting assembly (10) is used for adjusting the upper and lower positions of said dividing assembly (9) in said tank body, and said dividing assembly (9) is provided with a second sampling valve (11) which is used for being matched with said first sampling valve (7).
9. The device for preparing the standard of the Henry constant of methane in experimental water as claimed in claim 5, wherein said pressure supplementing mechanism (8) comprises a bladder (81) located in said experimental operation chamber (92), and an air inlet opening (82) of said bladder (81) is hermetically mounted on the inner wall of said tank (1) through a two-way valve (83).
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Cited By (1)
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CN116448532A (en) * | 2023-04-17 | 2023-07-18 | 防灾科技学院 | Piston type automatic fixed gas and liquid distribution device and experimental method thereof |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN116448532A (en) * | 2023-04-17 | 2023-07-18 | 防灾科技学院 | Piston type automatic fixed gas and liquid distribution device and experimental method thereof |
CN116448532B (en) * | 2023-04-17 | 2024-01-12 | 防灾科技学院 | Piston type automatic fixed gas and liquid distribution device and experimental method thereof |
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