CN115372104A - Device and method for preparing standard oil sample of dissolved gas in oil directly tracing to quality - Google Patents
Device and method for preparing standard oil sample of dissolved gas in oil directly tracing to quality Download PDFInfo
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- CN115372104A CN115372104A CN202211084169.0A CN202211084169A CN115372104A CN 115372104 A CN115372104 A CN 115372104A CN 202211084169 A CN202211084169 A CN 202211084169A CN 115372104 A CN115372104 A CN 115372104A
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- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 claims abstract description 34
- 239000007789 gas Substances 0.000 claims description 420
- 238000005303 weighing Methods 0.000 claims description 47
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 28
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 28
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 15
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 14
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 14
- 239000005977 Ethylene Substances 0.000 claims description 14
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 14
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 14
- 239000001569 carbon dioxide Substances 0.000 claims description 14
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 14
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 14
- 239000001257 hydrogen Substances 0.000 claims description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000007872 degassing Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000012544 monitoring process Methods 0.000 claims description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims 1
- 150000002431 hydrogen Chemical group 0.000 description 10
- 238000004321 preservation Methods 0.000 description 7
- 229910000831 Steel Inorganic materials 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 230000007613 environmental effect Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000009534 blood test Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 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
- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a device and a method for preparing a standard oil sample of gas dissolved in oil, which can directly trace to the quality, wherein the device for preparing the standard oil sample of the gas dissolved in the oil comprises an oil sample storage module, a gas sample storage module and a circulating pump; the oil sample storage module comprises a shell and an oil filling cavity arranged in the shell, and an inflation cavity is formed between the shell and the oil filling cavity; a first valve is arranged at a first port of the oil filling cavity, and a second valve is arranged at a second port of the oil filling cavity; a fifth valve is arranged on the inflation cavity; the gas sample storage module comprises a gas cavity, a first port of the gas cavity is provided with a third valve, a second port of the gas cavity is provided with a fourth valve, and the fourth valve is communicated with the second valve; and one end of the circulating pump is communicated with the first valve, and the other end of the circulating pump is communicated with the third valve. The invention can realize the preparation and the quantity value tracing of the standard oil sample and can directly quantify the concentration of the prepared standard oil sample.
Description
Technical Field
The invention belongs to the field of oil sample preparation, particularly relates to a device and a method for preparing a standard oil sample of gas dissolved in oil with quality directly traced to source, and more particularly relates to a device and a method for preparing a standard oil sample of gas dissolved in oil with quality directly traced to source based on gas dissolved in oil.
Background
The insulating oil plays the roles of insulation, cooling and arc extinction in the transformer, is equivalent to 'blood' of the transformer, and the analysis of dissolved gas in the insulating oil is equivalent to 'blood test' of the transformer, so that the method is a key means for evaluating whether the transformer is 'healthy'. Before analysis of dissolved gas in insulating oil is carried out, an instrument needs to be calibrated firstly to ensure the accuracy of the instrument, so that the preparation of a standard oil sample of the dissolved gas in the oil is a precondition for calibration. At present, when the preparation of the standard oil sample of the gas dissolved in the oil is carried out, a certain volume of standard gas is dissolved in the oil, or a certain volume of standard gas and oil are balanced in a gas-liquid two-phase state, and because of the particularity of the gas, the gas is easy to escape and lose, the content of the gas dissolved in the oil cannot be accurately quantified, or the gas is required to be quantified by an average value detected by an instrument, and the preparation of the standard oil sample of the gas dissolved in the oil is lack of a reliable quantity value tracing method. The quality method is the most classical quantity value tracing method in the preparation and use of standard substances, and if the oil sample and the gas sample dissolved in the oil sample used in the preparation process of the standard oil sample can be directly traced to the quality, the content of the dissolved gas in the prepared standard oil sample can be directly obtained.
Preparing a standard oil sample, wherein the mass of the required oil is thousands of grams or even dozens of kilograms and the mass of the required standard gas is only dozens of milligrams for subsequent use, if the standard gas is directly added into the oil sample, the change of the mass of the oil sample before and after the addition of the dozens of milligrams of standard gas is difficult to be accurately quantified, and even if a most advanced mass comparator is used, a relatively large error exists, so that a preparation device and a preparation method are required to trace the quantity of the standard oil sample, and the standard oil sample is required to be effectively stored so as to be convenient for subsequent use.
Disclosure of Invention
Aiming at the problems, the invention provides a device and a method for preparing a standard oil sample of dissolved gas in oil with direct tracing quality.
In order to achieve the technical purpose and achieve the technical effects, the invention is realized by the following technical scheme:
in a first aspect, the present invention provides a device for preparing a standard oil sample of dissolved gas in oil directly tracing to quality, comprising:
the oil sample storage module comprises a shell and an oil filling cavity arranged in the shell, and an inflation cavity is formed between the shell and the oil filling cavity; a first valve is arranged at a first port of the oil filling cavity, and a second valve is arranged at a second port of the oil filling cavity; a fifth valve is arranged on the inflation cavity;
the gas sample storage module comprises a gas cavity, a first port of the gas cavity is provided with a third valve, a second port of the gas cavity is provided with a fourth valve, and the fourth valve is communicated with the second valve;
and one end of the circulating pump is communicated with the first valve, and the other end of the circulating pump is communicated with the third valve.
Optionally, the device for preparing a standard oil sample of gas dissolved in oil further comprises a vacuum pump, wherein the vacuum pump is communicated with each valve and is used for vacuumizing the oil sample storage module and the gas sample storage module.
Optionally, the standard oil sample preparation device for gas dissolved in oil further comprises a mass comparator and an analytical balance, wherein the mass comparator is matched with the oil sample storage module and used for weighing the mass of the oil sample storage module, and the analytical balance is matched with the gas sample storage module and used for weighing the mass of the gas sample storage module.
Optionally, when the number of the gas sample storage modules is greater than 1, valves at two ends of each gas sample storage module are connected in parallel through corresponding first pipelines and second pipelines respectively;
the first pipeline is also used for being communicated with a circulating pump; the second line is also adapted to communicate with a second valve.
Optionally, the gas sample preservation module is used for storing standard gas;
when the gas components of the standard gas stored in a certain gas cavity meet all the gas component requirements required for preparing the standard oil sample, only starting the gas sample storage module;
when the gas components of the standard gas stored in a certain gas cavity do not meet all gas component requirements required for preparing the standard oil sample, starting a plurality of gas sample storage modules, wherein the gas components of the standard gas in the plurality of gas sample storage modules can meet all gas component requirements required for preparing the standard oil sample after being mixed.
Optionally, the gas composition of the standard gas in the gas sample preservation module is hydrogen, methane, ethane, ethylene, acetylene, carbon monoxide and/or carbon dioxide standard gas.
Optionally, the housing is made of a hard material; the oil-filled cavity is made of flexible materials, the volume of the oil-filled cavity is equal to that of the oil sample, and no cavity is generated.
Optionally, before the standard oil sample is prepared, the oil sample in the oil-filled cavity is blank oil subjected to degassing treatment, and the content of the standard gas in the blank oil is lower than a set threshold value, so that the result of the oil sample is not affected; and the total gas content is lower than a set threshold value, and standard gas in the preparation process can be completely dissolved in the white oil within a specified time.
Optionally, a pressure sensor is arranged in the inflation cavity and used for monitoring the real-time pressure in the inflation cavity.
Optionally, the first valve, the second valve, the third valve and the fourth valve are all of an internal tooth type structure, can be quickly connected with a pipeline, controls the on-off of the pipeline, and is small in dead volume.
In a second aspect, the invention provides a method for preparing a standard oil sample of dissolved gas in oil with directly traceable quality, which comprises the following steps:
respectively vacuumizing an oil filling cavity and an air charging cavity in the oil sample storage module, and weighing the oil sample storage module by using a mass comparator to obtain a first mass;
connecting a first valve connected with the oil filling cavity with a pipeline of an oil drum filled with white oil, opening the first valve to feed oil into the oil filling cavity, closing the first valve after the oil feeding is finished, and weighing on a same-mass comparator to obtain an oil sample storage module to obtain a second mass;
vacuumizing the gas sample storage module, and weighing the gas sample storage module by using an analytical balance to obtain a third mass;
connecting a third valve connected with the gas sample storage module with a standard gas container, opening the standard gas container and the third valve, allowing a certain amount of standard gas to enter the gas sample storage module, closing the standard gas container and the third valve, and weighing on the same analytical balance scale to obtain the gas sample storage module and obtain a fourth mass;
after the circulating pump is vacuumized, the first valve and the third valve are respectively connected with the circulating pump, and the second valve connected with the oil sample storage module is communicated with the fourth valve connected with the gas sample storage module;
starting a circulating pump, mixing the oil sample with the gas sample repeatedly until the gas in the gas sample storage module is completely dissolved in the oil, and closing all valves;
and filling a certain amount of air or nitrogen into the inflation cavity, and keeping the pressure in the inflation cavity greater than the standard atmospheric pressure.
Optionally, the oil filled cavity is filled with an oil sample having a concentration of each gas component:
in the formula, c (i) Sign board ) And m1 is the mass fraction of the i component in the standard mixed gas, m2 is the first mass, m3 is the third mass, and m4 is the fourth mass.
Optionally, the oil-filled cavity and the gas-filled cavity are respectively vacuumized, specifically:
opening a first valve connected with the oil filling cavity, closing a second valve connected with the oil filling cavity, connecting the first valve with a vacuum pump, and closing the first valve after the oil filling cavity is fully vacuumized;
and opening a fifth valve connected with the inflation cavity, and closing the fifth valve after vacuumizing the inflation cavity.
Optionally, the gas sample storage module is vacuumized, specifically:
and closing a fourth valve communicated with the gas sample storage module, opening a third valve communicated with the gas sample storage module, connecting a vacuum pump with the third valve for vacuumizing, and closing the third valve after fully vacuumizing the gas sample storage module.
Optionally, when the number of the gas sample storage modules is greater than 1, valves at two ends of each gas sample storage module are connected in parallel through corresponding first pipelines and second pipelines respectively;
the first pipeline is also used for being communicated with a circulating pump; the second line is also adapted to communicate with a second valve.
Optionally, the gas sample preservation module is used for storing standard gas;
when the gas components of the standard gas stored in a certain gas cavity meet all the gas component requirements required for preparing the standard oil sample, only starting the gas sample storage module;
when the gas components of the standard gas stored in a certain gas cavity do not meet all gas component requirements required for preparing the standard oil sample, starting a plurality of gas sample storage modules, wherein the gas components of the standard gas in the plurality of gas sample storage modules can meet all gas component requirements required for preparing the standard oil sample after being mixed;
and the analytical balance weighs each gas sample storage module to obtain a third mass and a fourth mass of each gas sample storage module.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the invention, the oil sample storage module and the gas sample storage module are respectively designed, so that the problem of accurate weighing of a gas sample with milligram magnitude added in a kilogram magnitude oil sample is solved, the direct tracing of the quality of the oil sample and the standard gas for preparing the standard oil sample is realized, and the concentration of the prepared standard oil sample can be directly obtained quantitatively through the quality.
(2) The blank oil is obtained by pretreating the oil sample, so that the standard gas is fully dissolved in the blank oil, the preparation method is simple and quick, and the introduced error is small.
(3) The invention skillfully provides a 'micro-positive pressure' storage environment for the prepared oil sample, so that the environmental pressure of the prepared standard oil sample during storage is greater than that during preparation, thus gas in the oil is less prone to escape and can be stored for a longer time.
Drawings
In order that the present disclosure may be more readily and clearly understood, reference is now made to the following detailed description of the present disclosure taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a schematic structural diagram of a standard oil sample preparation apparatus for dissolved gas in oil in example 1 of the present invention;
FIG. 2 is a schematic structural diagram of a standard oil sample preparation apparatus for gas dissolved in oil in example 2 of the present invention;
wherein:
1-an oil sample storage module, 101-an oil filling cavity, 102-a gas filling cavity, 103-a shell, 104-a first oil port, 105-a second oil port, 106-a first valve, 107-a second valve, 108-a fifth valve, 109-a gas filling port, 2-a circulating pump, 3-a gas sample storage module, 301-a gas cavity, 302-a first gas port, 303-a second gas port, 304-a third valve, 305-a fourth valve, 4-a pressure sensor, 5-a first pipeline and 6-a second pipeline.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the scope of the invention.
The following detailed description of the principles of the invention is provided in connection with the accompanying drawings.
Example 1
The invention provides a device and a method for preparing an oil sample by directly tracing the quality of a gas dissolved in oil, which are used for solving the problem that the quality of the oil sample and the quality of an added gas sample cannot be directly obtained, namely the concentration of the prepared oil sample is determined by detecting the content of the gas in the oil sample after the oil sample is prepared, the accurate theoretical concentration of the oil sample cannot be obtained by tracing the quantity value, the tracing of the quantity value is the most critical part for applying national standard substances, a national standard substance certificate cannot be applied if the tracing of the quantity value is not available, and in order to realize the tracing of the quantity value for preparing the oil sample, the invention provides the device and the method for preparing the oil sample by directly tracing the quality of the gas dissolved in oil.
Specifically, an embodiment of the present invention provides a standard oil sample preparation apparatus directly tracing to dissolved gas in oil of quality, as shown in fig. 1, including: the device comprises an oil sample storage module 1, a gas sample storage module 3 and a circulating pump 2;
the oil sample storage module 1 comprises a shell 103 and an oil filling cavity 101 arranged in the shell 103, and an inflation cavity 102 is formed between the shell 103 and the oil filling cavity; a first port (i.e. the first oil port 104 in fig. 1) of the oil charging chamber 101 is provided with a first valve 106, and a second port (i.e. the second oil port 105 in fig. 1) thereof is provided with a second valve 107; a fifth valve 108 is arranged on the inflation cavity 102; the first port and the second port of the oil sample storage module 1 are used for oil (gas) inlet and outlet;
the gas sample preservation module 3 comprises a gas cavity 301, wherein a first port (i.e. a first gas port 302 in fig. 1) of the gas cavity 301 is provided with a third valve 304, a second port (i.e. a second gas port 303 in fig. 1) thereof is provided with a fourth valve 305, and the fourth valve 305 is used for being communicated with the second valve 107; the first port and the second port of the gas sample preservation module 3 are used for air intake and exhaust (oil); the number of the gas sample storage modules 3 is 1, and the gas sample storage modules 3 are used for storing standard gas (national standard substance certificates); the gas components of the standard gas of the gas sample storage module 3 are hydrogen, methane, ethane, ethylene, acetylene, carbon monoxide and/or carbon dioxide standard gas, and the gas components can be adjusted according to needs without hard regulations as long as all gas component requirements required by preparing a standard oil sample can be met;
one end of the circulation pump 2 is adapted to communicate with the first valve 106, and the other end is adapted to communicate with the third valve 304.
Based on the above description, it can be seen that in the embodiment of the present invention, the oil sample storage module 1 and the gas sample storage module 3 are respectively designed, so that the problem of accurate weighing of a gas sample in milligram order added to a kilogram order oil sample is solved, the quality of an oil sample and a standard gas used for preparing a standard oil sample is directly traced, and the concentration of the prepared standard oil sample can be directly obtained quantitatively through the quality.
In a specific implementation manner of the embodiment of the present invention, in order to avoid the influence of air on the preparation process, the apparatus further includes a vacuum pump (not shown in the figure) for communicating with each valve and evacuating the oil sample storage module 1 and the gas sample storage module 3. Before the oil filling cavity 101, the gas sample storage module 3, the connecting pipeline, the first valve 106, the second valve 107, the third valve 304, the fourth valve 305, the fifth valve 108 and the circulating pump 2 are used, the vacuum pumping treatment is required.
In a specific implementation of the embodiment of the present invention, the apparatus further comprises a mass comparator (not shown in the figure) and an analytical balance (not shown in the figure), wherein the mass comparator is matched with the oil sample storage module 1 for weighing the mass of the oil sample storage module 1, and the analytical balance is matched with the gas sample storage module 3 for weighing the mass of the gas sample storage module 3. In making the mass comparator selection, the mass comparator with the maximum weight of 26kg and readability of 1mg can be selected. In the process of selecting the analytical balance, the analytical balance with the maximum weighing of 320g and the readability of 0.1mg can be selected, so that the problem of accurate weighing of a kilogram-magnitude oil sample and a milligram-magnitude gas sample is solved. The description of the mass comparator and the analytical balance is only one of the options, and in the practical application process, the selection standard can be set according to the practical situation, but the problem of accurately weighing the gas sample with the milligram level added into the oil sample with the kilogram level can be solved.
In a specific implementation manner of the embodiment of the present invention, the housing 103 is made of a hard material, and has good sealing performance, and a certain volume of nitrogen or air is filled into the inflation cavity 102 through the inflation inlet 109 provided on the housing 103, so as to control the pressure value of the inflation cavity 102 and keep the pressure in the inflation cavity 102 greater than the standard atmospheric pressure, so that the oil-filled cavity 101 is in a required pressure environment, that is, the oil-filled cavity 101 is in a "micro-positive pressure" environment, and the storage of the gas dissolved in the oil is more stable; the oil-filled cavity 101 is made of a flexible material, and the volume of the oil-filled cavity is equal to the volume of the added oil sample, so that no cavity is generated (namely, the volume is increased along with the increase of the volume of the added oil sample, and the maximum volume of the oil-filled cavity 101 is set according to requirements, such as 10L, 20L and the like).
In a specific implementation manner of the embodiment of the present invention, before the standard oil sample is prepared, the oil sample in the oil-filled cavity 101 is blank oil subjected to degassing treatment, and a content of a standard gas contained in the blank oil is lower than a set threshold, so as to achieve that a result of preparing the oil sample is not affected; and the total gas content is lower than a set threshold value, and standard gas in the preparation process can be completely dissolved in the white oil within a specified time. That is, the oil sample added into the oil filling cavity 101 of the oil sample storage module 1 is the blank oil which is processed in advance, and through degassing processing, it is ensured that the contents of hydrogen, methane, ethane, ethylene, acetylene, carbon monoxide, carbon dioxide and the like in the blank oil are all at a low level, and the results of oil sample preparation are not affected (for example, the hydrogen and acetylene are less than 0.1 microliter per liter, the methane, ethane and ethylene are less than 0.5 microliter per liter, the carbon monoxide is less than 1 microliter per liter, and the carbon dioxide is less than 30 microliter per liter), and the total content of dissolved gas in the blank oil is less than 2%, and the standard gas in the preparation process can be completely dissolved in the oil more rapidly. In the embodiment of the invention, the blank oil is obtained by pretreating the oil sample, so that the standard gas is fully dissolved in the blank oil, the preparation method is simple and quick, and the introduced error is small.
In a specific implementation manner of the embodiment of the present invention, in order to accurately provide a "micro-positive pressure" storage environment, a pressure sensor 4 is disposed in the inflation cavity 102, and is used for monitoring a real-time pressure in the inflation cavity 102, so that an environmental pressure when a prepared standard oil sample is stored is greater than an environmental pressure when the standard oil sample is prepared, and thus, gas in the oil is less prone to escape, and the standard oil sample can be stored for a longer time.
In a specific implementation manner of the embodiment of the present invention, the first valve 106, the second valve 107, the third valve 304, and the fourth valve 305 are all of an internal thread structure, and can be quickly connected to a pipeline, control the on/off of the pipeline, and have a small dead volume.
The working flow of the preparation of the standard oil sample of dissolved gas in oil directly tracing to quality in the embodiment 1 of the present invention is described in detail below with reference to the specific implementation manner, which includes the following steps:
(1) Closing a second valve 107 connected with the oil-filled cavity 101, opening a first valve 106, connecting the first valve 106 with a vacuum pump for vacuumizing, closing the first valve 106 after full vacuumizing, opening a fifth valve 108, closing the fifth valve 108 after vacuumizing, and weighing the mass of the oil sample storage module 1 by using a mass comparator (the mass comparator has the maximum weighing capacity of 26kg and readability of 1 mg) to obtain a first mass m1; connecting the first valve 106 with an oil drum pipeline filled with white oil, opening the first valve 106 to feed oil into the oil filling cavity 101, closing the first valve 106 after the oil feeding is finished, and weighing the mass of the oil sample storage module 1 on a same mass comparator to obtain a second mass m2.
(2) Closing a fourth valve 305 connected with the gas sample storage module 3, opening a third valve 304, connecting the third valve 304 with a vacuum pump for vacuumizing, closing the third valve 304 after full vacuumizing, and weighing the mass of the gas sample storage module 3 by an analytical balance (the maximum weighing of the analytical balance is 320g, and the readability is 0.1 mg) to obtain a third mass m3; connecting the third valve 304 with a standard gas cylinder containing seven gas components, opening the gas cylinder valve and the third valve 304, allowing a certain amount of gas to enter the gas sample storage module 3 from the gas port 1, closing the third valve 304 and the gas cylinder valve, and weighing the gas sample storage module 3 by using the same analytical balance to obtain a fourth mass m4.
(3) The method comprises the steps of vacuumizing a circulating pump 2 and a connecting pipeline, connecting a first valve 106 of an oil sample storage module 1 with the circulating pump 2, connecting a third valve 304 of a gas sample storage module 3 with the circulating pump 2, connecting a second valve 107 of the oil sample storage module 1 with a fourth valve 305 of the gas sample storage module 3, starting the circulating pump 2, mixing the oil sample with the gas sample repeatedly until the gas in the gas sample storage module 3 is completely dissolved into oil, and closing the first valve 106, the second valve 107, the third valve 304 and the fourth valve 305.
(4) The fifth valve 108 is opened, a certain amount of air or nitrogen is filled from the inflation port 109, the fifth valve 108 is closed, the pressure in the inflation cavity 102 is kept to be greater than the standard atmospheric pressure, namely the oil filling cavity 101 is in a micro-positive pressure environment, so that the storage of the dissolved gas in the oil is more stable. The finally obtained gas component concentrations of the prepared oil sample are as follows:
in the formula, c (i) Sign board ) And m1 is the mass fraction of the i component in the standard mixed gas, m2 is the first mass, m3 is the third mass, and m4 is the fourth mass.
Example 2
The embodiment of the invention provides a standard oil sample preparation device for directly tracing dissolved gas in oil with quality, as shown in fig. 2, comprising: the device comprises an oil sample storage module 1, a gas sample storage module 3 and a circulating pump 2;
the oil sample storage module 1 comprises a shell 103 and an oil-filled cavity 101 arranged in the shell 103, and an air-filled cavity 102 is formed between the shell 103 and the oil-filled cavity; a first port (i.e. the first oil port 104 in fig. 1) of the oil charging chamber 101 is provided with a first valve 106, and a second port (i.e. the second oil port 105 in fig. 2) thereof is provided with a second valve 107; a fifth valve 108 is arranged on the inflation cavity 102; the first port and the second port of the oil sample storage module 1 are used for oil (gas) inlet and oil (gas) outlet;
the number of the gas sample storage modules 3 is greater than 1, each gas sample storage module 3 comprises a gas cavity 301, a third valve 304 is arranged at a first port (i.e. a first gas port 302 in fig. 2) of the gas cavity 301, a fourth valve 305 is arranged at a second port (i.e. a second gas port 303 in fig. 2) of the gas cavity, and the valves (304, 305) at two ends of each gas sample storage module 3 are connected in parallel through a corresponding first pipeline 5 and a corresponding second pipeline 6; the first pipeline 5 is also used for being communicated with the circulating pump 2; the second circuit 6 is also intended to communicate with a second valve 107, see in particular fig. 2; the gas sample storage module 3 is used for storing standard gas (national standard substance certificate); the gas components of the standard gas in the gas sample storage module 3 are hydrogen, methane, ethane, ethylene, acetylene, carbon monoxide and/or carbon dioxide standard gas, and the gas components can be adjusted according to needs without hard regulation; when the gas components of the standard gas stored in a certain gas cavity 301 meet all the gas component requirements for preparing a standard oil sample, only the gas sample storage module 3 is started, so that the method has the advantages that only 1 gas sample storage module 3 is needed to be used conveniently, but the defect that the proportion of each gas component in the prepared standard oil sample is consistent with that of the standard gas, although the content can be adjusted to be low and high, the proportion among each gas component is always fixed; when the gas components of the standard gas stored in a certain gas cavity 301 do not meet all the gas component requirements required for preparing the standard oil sample, the plurality of gas sample storage modules 3 are started, and the gas components of the standard gas in the plurality of gas sample storage modules 3 can meet all the gas component requirements required for preparing the standard oil sample after being mixed. Therefore, although the number of the gas sample storage modules required to be used is large, the concentration of each gas component is more convenient to adjust, and in actual work, 7 standard gases, namely hydrogen, methane, ethane, ethylene, acetylene, carbon monoxide and carbon dioxide, can be respectively selected and loaded into the 7 gas sample storage modules 3 and then connected in parallel, so that the required amount of each component can be selected according to needs, and the concentration of the gas in the prepared standard oil sample can be really adjusted. If the number of the 7 gas sample storage modules is too large, 3-4 gas sample storage modules can be selected, such as 3 gas sample storage modules, and one gas sample storage module is filled with hydrogen and carbon monoxide; one gas sample storage module is filled with acetylene and carbon dioxide; one gas sample storage module contains methane, ethane and ethylene, and also contains 7 gas components, the component concentration is adjustable (but is not as flexible as the adjustment of 7 gas sample storage modules), and the number of used gas sample storage modules is not as large.
One end of the circulation pump 2 is used to communicate with the first valve 106, and the other end is used to communicate with the third valve 304.
Based on the above description, it can be seen that in the embodiment of the present invention, the oil sample storage module 1 and the gas sample storage module 3 are respectively designed, so that the problem of accurate weighing of a gas sample in a milligram order added to an oil sample in a kilogram order is solved, direct tracing to the quality of an oil sample and a standard gas used for preparing a standard oil sample is realized, and the concentration of the prepared standard oil sample can be directly obtained quantitatively through the quality.
In a specific implementation manner of the embodiment of the present invention, in order to avoid the influence of air on the preparation process, the apparatus further includes a vacuum pump (not shown in the figure) for communicating with each valve and evacuating the oil sample storage module 1 and the gas sample storage module 3. Before use, the oil-filled cavity 101, the gas sample storage module 3, the connecting pipeline, the first valve 106, the second valve 107, the third valve 304, the fourth valve 305, the fifth valve 108 and the circulating pump 2 in the embodiment of the invention are all subjected to vacuum pumping treatment.
In a specific implementation of the embodiment of the present invention, the apparatus further includes a mass comparator (not shown in the figure) and an analytical balance (not shown in the figure), wherein the mass comparator is matched with the oil sample storage module 1 for weighing the mass of the oil sample storage module 1, and the analytical balance is matched with the gas sample storage module 3 for weighing the mass of the gas sample storage module 3. In the process of making the mass comparator selection, the mass comparator with the maximum weighing of 26kg and readability of 1mg can be selected. In the process of selecting the analytical balance, the analytical balance with the maximum weighing of 320g and the readability of 0.1mg can be selected, so that the problem of accurate weighing of a kilogram-magnitude oil sample and a milligram-magnitude gas sample is solved. The description of the mass comparator and the analytical balance is only one of the options, and in the practical application process, the selection standard can be set according to the practical situation, but the problem of accurately weighing the gas sample with the milligram level added into the oil sample with the kilogram level can be solved.
In a specific implementation manner of the embodiment of the present invention, the housing 103 is made of a hard material, and has good sealing performance, and a certain volume of nitrogen or air is filled into the inflation cavity 102 through the inflation inlet 109 arranged on the housing 103, so as to control a pressure value of the inflation cavity 102, and keep the pressure in the inflation cavity 102 greater than a standard atmospheric pressure, so that the oil-filled cavity 101 is in a required pressure environment, that is, the oil-filled cavity 101 is in a "micro-positive pressure" environment, and the storage of the gas dissolved in the oil is more stable; the oil-filled cavity 101 is made of a flexible material, and the volume of the oil-filled cavity is in direct proportion to the volume of the added oil sample (namely, the volume increases with the increase of the volume of the added oil sample, and the maximum volume of the oil-filled cavity 101 is set according to requirements, such as 10L, 20L and the like).
In a specific implementation manner of the embodiment of the present invention, before the standard oil sample is prepared, the oil sample in the oil-filled cavity 101 is blank oil subjected to degassing treatment, and a content of a standard gas contained in the blank oil is lower than a set threshold, so as to achieve a purpose of not affecting a result of the oil sample preparation; and the total gas content is lower than a set threshold value, and standard gas in the preparation process can be completely dissolved in the white oil within a specified time. That is, the oil sample added into the oil filling cavity 101 of the oil sample storage module 1 is the blank oil which is processed in advance, and through degassing processing, it is ensured that the contents of hydrogen, methane, ethane, ethylene, acetylene, carbon monoxide, carbon dioxide and the like in the blank oil are all at a low level, and the results of oil sample preparation are not affected (for example, the hydrogen and acetylene are less than 0.1 microliter per liter, the methane, ethane and ethylene are less than 0.5 microliter per liter, the carbon monoxide is less than 1 microliter per liter, and the carbon dioxide is less than 30 microliter per liter), and the total content of dissolved gas in the blank oil is less than 2%, and the standard gas in the preparation process can be completely dissolved in the oil more rapidly. In the embodiment of the invention, the blank oil is obtained by pretreating the oil sample, so that the standard gas is fully dissolved in the blank oil, the preparation method is simple and quick, and the introduced error is small.
In a specific implementation manner of the embodiment of the present invention, in order to accurately provide a "micro-positive pressure" storage environment, a pressure sensor 4 is disposed in the inflation cavity 102, and is used for monitoring a real-time pressure in the inflation cavity 102, so that an environmental pressure when a prepared standard oil sample is stored is greater than an environmental pressure when the standard oil sample is prepared, and thus, gas in the oil is less prone to escape, and the standard oil sample can be stored for a longer time.
In a specific implementation manner of the embodiment of the present invention, the first valve 106, the second valve 107, the third valve 304, and the fourth valve 305 are all of an internal thread structure, and can be quickly connected to a pipeline, control the on/off of the pipeline, and have a small dead volume.
The working flow of the preparation of the standard oil sample of dissolved gas in oil directly tracing to quality in the embodiment 1 of the present invention is described in detail below with reference to the specific implementation manner, which includes the following steps:
(1) Closing a second valve 107 connected with the oil-filled cavity 101, opening a first valve 106, connecting the first valve 106 with a vacuum pump for vacuumizing, closing the first valve 106 after full vacuumizing, opening a fifth valve 108, closing the fifth valve 108 after vacuumizing, and weighing the mass of the oil sample storage module 1 by using a mass comparator (the mass comparator has the maximum weighing capacity of 26kg and readability of 1 mg) to obtain a first mass m1; connecting the first valve 106 with an oil drum pipeline filled with white oil, opening the first valve 106 to feed oil into the oil filling cavity 101, closing the first valve 106 after the oil feeding is finished, and weighing the mass of the oil sample storage module 1 on a same mass comparator to obtain a second mass m2.
(2) A proper number of gas sample storage modules 3 are selected, and each gas sample storage module 3 is used for containing hydrogen, methane, ethane, ethylene, ethane, acetylene, carbon monoxide and carbon dioxide single-component standard gas or mixed gas. Closing the fourth valves 305 connected with the gas sample storage modules 3, opening the third valves 304 in sequence, connecting the third valves 304 with a vacuum pump for vacuumizing, closing the third valves 304 after full vacuumizing, and weighing the mass m3 of each selected gas sample storage module 3 by an analytical balance (the maximum weighing capacity of the analytical balance is 320g, and the readability is 0.1 mg) j J represents the j-th gas sample storage module, j =1,2, … N (1 ≦ N ≦ 7,N is a positive integer); each third valve 304 is connected to a corresponding standard gas cylinder, each standard gas cylinderOne or more of hydrogen, methane, ethane, ethylene, ethane, acetylene, carbon monoxide and carbon dioxide are respectively stored in the bottle, the steel bottle valve and the third valve 304 are respectively opened, a certain amount of gas enters the corresponding gas sample storage module 3 from the corresponding gas port, the third valve 304 and the steel bottle valve are respectively closed, each selected gas sample storage module 3 is respectively weighed by the same analytical balance, and the mass at the moment is m4 j 。
(3) The method comprises the steps of vacuumizing a circulating pump 2 and a connecting pipeline, connecting a first valve 106 of an oil sample storage module 1 with the circulating pump 2, connecting a third valve 304 connected with a gas sample storage module 3 in parallel and then uniformly connecting the circulating pump 2, connecting fourth valves 305 connected with the gas sample storage module 3 in parallel and then connecting the fourth valves 305 with a second valve 107 of the oil sample storage module 1, starting the circulating pump 2, repeatedly mixing an oil sample with the gas sample until the gas in the gas sample storage module 3 is completely dissolved into oil, and closing the first valve 1061, the second valve 1072, the third valves 304 and the fourth valves 305.
(4) Opening the fifth valve 108, filling a certain amount of air or nitrogen from the inflation inlet 109, closing the fifth valve 108, and keeping the pressure in the inflation cavity 102 greater than the standard atmospheric pressure, that is, the oil filling cavity 101 is in a micro-positive pressure environment, so that the storage of the dissolved gas in the oil is more stable, and finally the mass m3 corresponding to each gas sample storage module 3 is based on the first mass, the second mass and the mass m3 corresponding to each gas sample storage module 3 j 、m4 j And the mass ratio of each component in the standard gas in each selected gas sample storage module 3, and calculating the concentration of each gas component of the oil sample to be distributed.
Example 3
The embodiment of the invention provides a preparation method of a standard oil sample of dissolved gas in oil with direct tracing to quality, which comprises the following steps:
(1) Respectively vacuumizing the oil filling cavity 101 and the gas filling cavity 102, and weighing the oil sample storage module 1 by using a mass comparator to obtain first mass;
(2) Connecting a first valve 106 connected with the oil filling cavity 101 with an oil drum pipeline filled with white oil, opening the first valve 106 to feed oil into the oil filling cavity 101, closing the first valve 106 after the oil feeding is finished, and weighing on a same-mass comparator to obtain an oil sample storage module 1 to obtain a second mass;
(3) Vacuumizing the gas sample storage module 3, and weighing the gas sample storage module 3 by using an analytical balance to obtain a third mass;
(4) Connecting a third valve 304 connected with the gas sample storage module 3 with a standard gas container, opening the standard gas container and the third valve 304, allowing a certain amount of standard gas to enter the gas sample storage module 3, closing the standard gas container and the third valve 304, weighing on the same analytical balance scale to obtain the gas sample storage module 3, and obtaining a fourth mass;
(5) After the circulating pump 2 is vacuumized, the first valve 106 and the third valve 304 are respectively connected with the circulating pump 2, and the second valve 107 connected with the oil sample storage module 1 is communicated with the fourth valve 305 connected with the gas sample storage module 3;
(6) Starting the circulating pump 2, mixing the oil sample with the gas sample repeatedly until the gas in the gas sample storage module 3 is completely dissolved in the oil, and closing all valves;
(7) A quantity of air or nitrogen is charged into the plenum 102 and the pressure within the plenum 102 is maintained above the normal atmospheric pressure.
In a specific implementation manner of the embodiment of the present invention, the concentrations of the gas components of the oil sample prepared in the oil-filled cavity 101 are as follows:
in the formula, c (i) Sign board ) And m1 is the mass fraction of the i component in the standard mixed gas, m2 is the first mass, m3 is the third mass, and m4 is the fourth mass.
In a specific implementation manner of the embodiment of the present invention, the oil-filled cavity 101 and the gas-filled cavity 102 are respectively vacuumized, which specifically includes:
opening a first valve 106 connected with the oil-filled cavity 101, closing a second valve 107 connected with the oil-filled cavity 101, connecting the first valve 106 by using a vacuum pump, and closing the first valve 106 after the oil-filled cavity 101 is fully vacuumized;
the fifth valve 108 associated with the plenum 102 is opened and the plenum 102 is evacuated and the fifth valve 108 is closed.
In a specific implementation manner of the embodiment of the present invention, the vacuumizing the gas sample storage module 3 specifically includes:
the fourth valve 305 communicating with the gas sample storage module 3 is closed, the third valve 304 communicating with the gas sample storage module 3 is opened, the third valve 304 is connected with a vacuum pump for vacuum pumping, and the third valve 304 is closed after the gas sample storage module 3 is fully evacuated.
The method for preparing the standard oil sample of gas dissolved in oil in the embodiment of the present invention can be implemented based on the apparatus for preparing the standard oil sample of gas dissolved in oil in embodiment 1.
Example 4
Based on embodiment 3, the embodiment of the present invention is different from embodiment 3 in that, as shown in fig. 2, when the number of the gas sample storage modules is greater than 1, valves at two ends of each gas sample storage module are connected in parallel through corresponding first pipelines and second pipelines, respectively; the first pipeline is also used for being communicated with a circulating pump; the second pipeline is also used for being communicated with a second valve; when the gas components of the standard gas stored in a certain gas cavity 301 meet all the gas component requirements required for preparing the standard oil sample, only the gas sample storage module 3 is started; when the gas components of the standard gas stored in a certain gas cavity 301 do not meet all the gas component requirements required for preparing the standard oil sample, starting a plurality of gas sample storage modules 3, wherein the gas components of the standard gas in the plurality of gas sample storage modules 3 can meet all the gas component requirements required for preparing the standard oil sample after being mixed; the analytical balance weighs each gas sample storage module 3 to obtain a third mass and a fourth mass of each gas sample storage module; the preparation method of the standard oil sample directly tracing to the dissolved gas in the oil with the quality comprises the following steps:
(1) Closing a second valve 107 connected with the oil-filled cavity 101, opening a first valve 106, connecting the first valve 106 with a vacuum pump for vacuumizing, closing the first valve 106 after full vacuumizing, opening a fifth valve 108, closing the fifth valve 108 after vacuumizing, and weighing the mass of the oil sample storage module 1 by using a mass comparator (the mass comparator has the maximum weighing capacity of 26kg and readability of 1 mg) to obtain a first mass m1; connecting the first valve 106 with an oil drum pipeline filled with white oil, opening the first valve 106 to feed oil into the oil filling cavity 101, closing the first valve 106 after the oil feeding is finished, and weighing the mass of the oil sample storage module 1 on a same mass comparator to obtain a second mass m2.
(2) A proper number of gas sample storage modules 3 are selected, and each gas sample storage module 3 is used for containing hydrogen, methane, ethane, ethylene, ethane, acetylene, carbon monoxide and carbon dioxide single-component standard gas or mixed gas. Closing the fourth valves 305 connected with the gas sample storage modules 3, opening the third valves 304 in sequence, connecting the third valves 304 with a vacuum pump for vacuumizing, closing the third valves 304 after full vacuumizing, and weighing the mass m3 of each selected gas sample storage module 3 by an analytical balance (the analytical balance has the maximum weighing capacity of 320g and the readability of 0.1 mg) j J represents the j-th gas sample storage module, j =1,2, … N (1 ≦ N ≦ 7,N is a positive integer); respectively connecting each third valve 304 to a corresponding standard gas steel cylinder, respectively storing one or more of hydrogen, methane, ethane, ethylene, ethane, acetylene, carbon monoxide and carbon dioxide in each standard gas steel cylinder, respectively opening the steel cylinder valve and the third valves 304, allowing a certain amount of gas to enter the corresponding gas sample storage module 3 through corresponding gas ports, respectively closing each third valve 304 and the steel cylinder valve, respectively weighing each selected gas sample storage module 3 by using the same analytical balance, and obtaining the mass m4 at the moment j 。
(3) The method comprises the steps of vacuumizing a circulating pump 2 and a connecting pipeline, connecting a first valve 106 of an oil sample storage module 1 with the circulating pump 2, connecting a third valve 304 connected with a gas sample storage module 3 in parallel and then uniformly connecting the circulating pump 2, connecting fourth valves 305 connected with the gas sample storage module 3 in parallel and then connecting the fourth valves 305 with a second valve 107 of the oil sample storage module 1, starting the circulating pump 2, repeatedly mixing an oil sample with the gas sample until the gas in the gas sample storage module 3 is completely dissolved into oil, and closing the first valve 1061, the second valve 1072, the third valves 304 and the fourth valves 305.
(4) Opening the fifth valve 108, filling a certain amount of air or nitrogen gas from the gas filling port 109, closing the fifth valve 108, and keeping the pressure in the gas filling cavity 102 greater than the standard atmospheric pressure, i.e. the oil filling cavity 101 is in the "micro-positive pressure" environment, so that the pressure in the gas filling cavity 102 is kept higher than the standard atmospheric pressure, and thus the oil filling cavity 101 is in the "micro-positive pressure" environment, and the fifth valve 108 is openedThe preservation of the dissolved gas in the oil is more stable, and finally the mass m3 corresponding to each gas sample preservation module 3 is based on the first mass, the second mass j 、m4 j And the mass ratio of each component in the standard gas in each selected gas sample storage module 3, and calculating the concentration of each gas component of the oil sample to be distributed.
The method for preparing the standard oil sample of gas dissolved in oil in the embodiment of the present invention can be implemented based on the apparatus for preparing the standard oil sample of gas dissolved in oil in embodiment 2.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (16)
1. A directly trace to gaseous standard oil appearance of dissolving and prepare device in oil of quality, its characterized in that includes:
the oil sample storage module comprises a shell and an oil filling cavity arranged in the shell, and an inflation cavity is formed between the shell and the oil filling cavity; a first valve is arranged at a first port of the oil filling cavity, and a second valve is arranged at a second port of the oil filling cavity; a fifth valve is arranged on the inflation cavity;
the gas sample storage module comprises a gas cavity, a first port of the gas cavity is provided with a third valve, a second port of the gas cavity is provided with a fourth valve, and the fourth valve is communicated with the second valve;
and one end of the circulating pump is communicated with the first valve, and the other end of the circulating pump is communicated with the third valve.
2. The device for preparing the standard oil sample of gas dissolved in oil with the quality directly traced to according to claim 1, further comprising a vacuum pump, wherein the vacuum pump is used for being communicated with each valve and vacuumizing the oil sample storage module and the gas sample storage module.
3. The device for preparing the standard oil sample of gas dissolved in oil according to claim 1, wherein the device for preparing the standard oil sample of gas dissolved in oil comprises a mass comparator and an analytical balance, the mass comparator is matched with the oil sample storage module and used for weighing the mass of the oil sample storage module, and the analytical balance is matched with the gas sample storage module and used for weighing the mass of the gas sample storage module.
4. The device for preparing the standard oil sample by dissolving the gas in the oil directly tracing to the quality according to claim 1, wherein when the number of the gas sample storage modules is greater than 1, valves at two ends of each gas sample storage module are respectively connected in parallel through a corresponding first pipeline and a corresponding second pipeline;
the first pipeline is also used for being communicated with a circulating pump; the second line is also adapted to communicate with a second valve.
5. The device for preparing the standard oil sample of the gas dissolved in the oil directly from the source to the quality as claimed in claim 4, wherein: the gas sample storage module is used for storing standard gas;
when the gas components of the standard gas stored in a certain gas cavity meet all the gas component requirements required for preparing the standard oil sample, only starting the gas sample storage module;
when the gas components of the standard gas stored in a certain gas cavity do not meet all gas component requirements required for preparing the standard oil sample, starting a plurality of gas sample storage modules, wherein the gas components of the standard gas in the plurality of gas sample storage modules can meet all gas component requirements required for preparing the standard oil sample after being mixed.
6. The device for preparing the standard oil sample by dissolving gas in oil directly tracing to quality according to claim 1 or 5, wherein the gas component of the standard gas in the gas sample storage module is hydrogen, methane, ethane, ethylene, acetylene, carbon monoxide and/or carbon dioxide standard gas.
7. The device for preparing the standard oil sample of the gas dissolved in the oil with the direct tracing quality as claimed in claim 1, wherein the shell is made of hard material; the oil-filled cavity is made of flexible materials, the volume of the oil-filled cavity is equal to that of the oil sample, and no cavity is generated.
8. The device for preparing the standard oil sample of the gas dissolved in the oil directly traced to the quality according to claim 1, is characterized in that: before the standard oil sample is prepared, the oil sample in the oil filling cavity is blank oil subjected to degassing treatment, and the content of standard gas contained in the blank oil is lower than a set threshold value and is used for realizing no influence on the result of the oil sample preparation; and the total gas content is lower than a set threshold value, and standard gas in the preparation process can be completely dissolved in the white oil within a specified time.
9. The device for preparing the standard oil sample of the gas dissolved in the oil directly traced to the quality according to claim 1, is characterized in that: and a pressure sensor is arranged in the inflation cavity and used for monitoring the real-time pressure in the inflation cavity.
10. The device for preparing the standard oil sample of the gas dissolved in the oil directly traced to the quality according to claim 1, is characterized in that: the first valve, the second valve, the third valve and the fourth valve are all of an internal tooth type structure, can be quickly connected with a pipeline, controls the on-off of the pipeline, and is small in dead volume.
11. A method for preparing a standard oil sample of dissolved gas in oil with directly traced quality is characterized by comprising the following steps:
respectively vacuumizing an oil filling cavity and an air charging cavity in the oil sample storage module, and weighing the oil sample storage module by using a mass comparator to obtain a first mass;
connecting a first valve connected with the oil filling cavity with an oil drum pipeline filled with white oil, opening the first valve to feed oil into the oil filling cavity, closing the first valve after the oil feeding is finished, and weighing on a same-mass comparator to obtain an oil sample storage module to obtain a second mass;
vacuumizing the gas sample storage module, and weighing the gas sample storage module by using an analytical balance to obtain a third mass;
connecting a third valve connected with the gas sample storage module with a standard gas container, opening the standard gas container and the third valve, allowing a certain amount of standard gas to enter the gas sample storage module, closing the standard gas container and the third valve, and weighing on the same analytical balance scale to obtain the gas sample storage module and obtain a fourth mass;
after the circulating pump is vacuumized, the first valve and the third valve are respectively connected with the circulating pump, and the second valve connected with the oil sample storage module is communicated with the fourth valve connected with the gas sample storage module;
starting a circulating pump, repeatedly mixing the oil sample with the gas sample until the gas in the gas sample storage module is completely dissolved in the oil, and closing all valves;
and filling a certain amount of air or nitrogen into the inflation cavity, and keeping the pressure in the inflation cavity to be greater than the standard atmospheric pressure.
12. The method for preparing the standard oil sample of dissolved gas in oil directly tracing to quality as claimed in claim 11, wherein the concentration of each gas component of the oil sample prepared in the oil-filled cavity is as follows:
in the formula, c (i) Sign board ) And m1 is the mass fraction of the i component in the standard mixed gas, m2 is the first mass, m3 is the third mass, and m4 is the fourth mass.
13. The method for preparing the standard oil sample of dissolved gas in oil directly tracing to quality according to claim 11, wherein the oil-filled cavity and the gas-filled cavity are respectively vacuumized, specifically:
opening a first valve connected with the oil filling cavity, closing a second valve connected with the oil filling cavity, connecting the first valve with a vacuum pump, and closing the first valve after the oil filling cavity is fully vacuumized;
and opening a fifth valve connected with the inflation cavity, and closing the fifth valve after vacuumizing the inflation cavity.
14. The method for preparing the standard oil sample by dissolving gas in oil according to the quality of the oil, as claimed in claim 11, wherein the gas sample storage module is evacuated, specifically:
and closing a fourth valve communicated with the gas sample storage module, opening a third valve communicated with the gas sample storage module, connecting a vacuum pump with the third valve for vacuumizing, and closing the third valve after fully vacuumizing the gas sample storage module.
15. The method for preparing the standard oil sample by dissolving the gas in the oil directly traced to the quality according to claim 11, wherein when the number of the gas sample storage modules is greater than 1, valves at two ends of each gas sample storage module are respectively connected in parallel through the corresponding first pipeline and second pipeline;
the first pipeline is also used for being communicated with a circulating pump; the second pipeline is also used for being communicated with a second valve.
16. The method for preparing the standard oil sample of gas dissolved in oil directly tracing to quality according to claim 15, wherein the gas sample storage module is used for storing standard gas;
when the gas components of the standard gas stored in a certain gas cavity meet all the gas component requirements required for preparing the standard oil sample, only starting the gas sample storage module;
when the gas components of the standard gas stored in a certain gas cavity do not meet all the gas component requirements required for preparing the standard oil sample, starting a plurality of gas sample storage modules, wherein the gas components of the standard gas in the plurality of gas sample storage modules can meet all the gas component requirements required for preparing the standard oil sample after being mixed;
and the analytical balance weighs each gas sample storage module to obtain a third mass and a fourth mass of each gas sample storage module.
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