CN218157736U - Liquid sample introduction cooling device for realizing chromatographic analysis requirement of liquefied petroleum gas - Google Patents
Liquid sample introduction cooling device for realizing chromatographic analysis requirement of liquefied petroleum gas Download PDFInfo
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- CN218157736U CN218157736U CN202221955558.1U CN202221955558U CN218157736U CN 218157736 U CN218157736 U CN 218157736U CN 202221955558 U CN202221955558 U CN 202221955558U CN 218157736 U CN218157736 U CN 218157736U
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Abstract
The utility model discloses a liquid sample introduction cooling device for realizing the chromatographic analysis requirement of liquefied petroleum gas, which comprises a liquefied petroleum gas sampling steel cylinder, wherein a steel cylinder valve and a first conveying pipe are arranged on the outlet of the liquefied petroleum gas sampling steel cylinder; cooling mechanism for send into the sample cooling in the chromatogram liquid injection valve to liquefied petroleum gas sampling steel bottle, include: the top of the cooling pipe is provided with an emptying exhaust port, and the bottom of the cooling pipe is communicated with a chromatographic liquid sample injection valve through a second conveying pipe with a needle valve; and the pipeline is arranged in the cooling pipe, one end of the pipeline penetrates out from the left end of the cooling pipe, the penetrating end is communicated with the first conveying pipe, the other end of the pipeline penetrates out from the right end of the cooling pipe, and the penetrating end is connected with the chromatographic liquid sample injection valve through the third conveying pipe. The utility model is simple in operation, do not need extra refrigeration plant to cool down and can satisfy the higher or the higher complete liquid of the higher sample of ethane content of vapor pressure and advance the appearance requirement.
Description
Technical Field
The utility model relates to a natural gas treatment and petroleum refining product technical field, concretely relates to realize liquid of liquefied petroleum gas chromatographic analysis requirement and advance a kind heat sink.
Background
A liquefied petroleum gas sampling steel cylinder (requiring pressure resistance of 2.5 MPa) is connected to a storage tank of a production device, and a liquid liquefied petroleum gas sample (the vapor pressure is less than or equal to 1380 kPa) with the volume of 80% is taken. The sample has a certain pressure in the storage tank and the sampling steel cylinder, and the liquid is discharged from the steel cylinder and contacts with air to be instantly gasified and absorb a large amount of heat (the injection pressure is larger when the sample is discharged).
And when the liquefied petroleum gas is measured, a gas chromatograph with an analysis standard number of NB/SH/T0230-2019 is used, and the national standard sample introduction of the gas chromatograph requires liquid sample introduction or flash evaporation instrument sample introduction. The liquefied petroleum gas is measured by using a gas chromatograph capable of carrying out liquid sample injection or a gas chromatograph equipped with a flash evaporator, so that the requirements of NB/SH/T0230-2019 standards can be met. The flash evaporator has high failure rate, and the liquid sampling technology is superior to that of the flash evaporator, for example, agilent adopts a liquid window technology (a nitrogen source of 0.8MPa needs to be added at the tail end of a steel cylinder), and PE company adopts a damping type liquid sampling window.
We have found that this injection technique cannot stably measure a sample having a high vapor pressure, particularly a sample having about 15% ethane and a vapor pressure higher than the quality requirement, using a liquid injection technique. It is discovered by accident through multiple experiments that when the temperature of the transparent polytetrafluoroethylene tube used as a window is lower, the sample is directly emptied, so that liquefied petroleum gas entering the polytetrafluoroethylene tube is directly gasified to obtain the temperature of the polytetrafluoroethylene tube with lower temperature, the liquid containing bubbles in the inlet tube can disappear in a very short time to realize complete liquid filling, the low temperature of the sample is the key for realizing liquid sampling, and by utilizing the phenomenon, the spiral sampling pipeline is soaked in the iced saline water, the sample and the pipeline are cooled down under continuous sample blowing, the needle valve is closed, the sample bubbles in the pipeline between the spiral sampling tube and the valve disappear, and the chromatograph is started to obtain good parallel data.
Although the method obtained in the test can meet the requirement of liquid sample injection to a certain extent, additional energy is needed for cooling, and the operation is complex, so that a sample which is simple to operate, does not need additional refrigeration equipment for cooling, can meet the requirement of higher vapor pressure or higher ethane content is designed, and the complete liquid sample injection requirement is realized.
SUMMERY OF THE UTILITY MODEL
The utility model aims at overcoming the problems existing in the prior art and providing a liquid sample introduction and cooling device for realizing the chromatographic analysis requirement of liquefied petroleum gas.
The utility model provides a realize liquid of liquefied petroleum gas chromatographic analysis requirement and advance a kind heat sink, include: the liquefied petroleum gas sampling steel cylinder is provided with a steel cylinder valve and a first delivery pipe at an outlet; cooling mechanism for send into the sample cooling in the chromatogram liquid sampling valve to liquefied petroleum gas sampling steel bottle, include: the top of the cooling pipe is provided with an emptying exhaust port, and the bottom of the cooling pipe is communicated with a chromatographic liquid sample injection valve through a second conveying pipe with a needle valve; and the pipeline is arranged in the cooling pipe, one end of the pipeline is penetrated out from the left end of the cooling pipe, the penetrating end is communicated with the first conveying pipe, the other end of the pipeline is penetrated out from the right end of the cooling pipe, and the penetrating end is connected with the chromatographic liquid sample injection valve through the third conveying pipe.
Preferably, the pipeline in the cooling pipe is of a spiral structure.
Preferably, a filter head is arranged on a pipeline which is positioned outside the cooling pipe and connected with the first conveying pipe.
Preferably, the first conveying pipe and the third conveying pipe are both sleeved with transparent polytetrafluoroethylene pipes for heat preservation.
Preferably, the cooling pipe includes: a cylindrical tube; the two cylindrical pipe pressing caps are respectively in threaded connection with two ends of the cylindrical pipe, and are also provided with first through holes for the pipeline to penetrate out; the two pipeline sealing pressure caps are in threaded connection with the cylindrical pipe pressure cap, and a second through hole communicated with the first through hole is formed in each pipeline sealing pressure cap; the two sealing gaskets I are respectively arranged between the cylindrical pipe and the cylindrical pipe pressing cap; and two sealing gaskets II are arranged between the pipeline sealing pressing cap and the pipeline sleeved with the transparent polytetrafluoroethylene pipe.
Preferably, the sealing gasket I and the sealing gasket II are both made of copper or aluminum.
Preferably, the cylindrical pipe pressing cap and the pipeline sealing pressing cap are all made of stainless steel or copper materials.
Preferably, the first delivery pipe, the second delivery pipe, the pipeline and the third delivery pipe are all made of metal materials.
Compared with the prior art, the beneficial effects of the utility model are that:
1. the utility model discloses do not need the extra energy to cool down, easy operation. When the sampling device is used, a steel cylinder valve on a sampling steel cylinder is opened, liquefied petroleum gas starts to enter a first conveying pipe, a filter head filters large-particle impurities and enters a cooling pipe through a pipeline, a chromatographic liquid sample introduction valve is sent into the third conveying pipe, the opening degree of a needle valve is adjusted, the liquefied petroleum gas sent into the cooling pipe through a second conveying pipe is sprayed into the cooling pipe, the liquefied petroleum gas in a liquid state or not is the liquefied petroleum gas in the liquid state completely, the liquefied petroleum gas in a low-pressure state can be gasified, and the gasification needs to absorb heat. The liquefied petroleum gas sprays and gasifies and is discharged by the evacuation gas vent in the cooling tube, can make the interior ambient temperature of cooling tube reduce to make the interior pipeline cooling of cooling tube, consequently the liquefied petroleum gas in the pipeline also obtains the cooling, closes the needle valve, and the liquefied petroleum gas bubble of suppressing pressure in the pipeline will disappear, makes the sample all be the liquid state in the dosing pipe of liquid sampling valve.
2. The utility model discloses to be located the intraductal pipeline of cooling and establish to helical structure is in order to increase the area of contact of pipeline cooling.
3. The utility model discloses in, through set up the filter head on the pipeline outside the cooling tube for particulate matter in the filtration sample avoids the wearing and tearing of chromatographic valve body.
4. The utility model discloses in, through filling up sealed pad at the dress of column pipe both ends to go up the column pipe and press the cap to guarantee sealed pad sealed and difficult not hard up, press the cap again at the column pipe and go up sealed pipeline seal and press the cap, guarantee the overall seal of column pipe.
5. The utility model discloses a liquid-gaseous state's physical phenomenon cools down the processing to the sample of high vapor pressure, guarantees the liquid sampling technique that meets the standard requirement, and easy operation does not need extra refrigeration plant, utilizes the liquefied petroleum gas that the replacement sweeps to realize the sample and the cooling of mechanism of cooling down.
Drawings
FIG. 1 is a flow chart of the actual production process of the present invention;
fig. 2 is a sectional view of the cooling tube of the present invention.
Description of the reference numerals:
1. the device comprises a liquefied petroleum gas sampling steel cylinder, 2 a steel cylinder valve, 3 a first delivery pipe, 4 a cooling mechanism, 4-1 a cooling pipe, 4-11 a cylindrical pipe, 4-12 a cylindrical pipe pressing cap, 4-13 a pipeline sealing pressing cap, 4-2 a needle valve, 4-3 a second delivery pipe, 4-4 a pipeline, 5 a chromatographic liquid sample injection valve, 6 a third delivery pipe and 7 a filter head.
Detailed Description
The following detailed description of the present invention is provided in conjunction with the accompanying drawings, but it should be understood that the scope of the present invention is not limited by the following detailed description. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
Examples
The problem that in the prior art, complete liquid sample introduction cannot be realized by sample introduction of a sample with high vapor pressure or high ethane content, and additional ice-making refrigeration equipment is needed to cool pipelines is solved.
As shown in fig. 1-2, the utility model provides a pair of realize liquid sampling heat sink of liquefied petroleum gas chromatographic analysis requirement, include: the device comprises a liquefied petroleum gas sampling steel cylinder 1 and a cooling mechanism 4, wherein a steel cylinder valve 2 and a first delivery pipe 3 are arranged on an outlet of the liquefied petroleum gas sampling steel cylinder 1; cooling mechanism 4 is used for the sample cooling in the chromatogram liquid injection valve 5 is sent into to liquefied petroleum gas sampling steel bottle 1, and cooling mechanism 4 includes: the device comprises a cooling pipe 4-1, a needle valve 4-2, a second delivery pipe 4-3 and a pipeline 4-4, wherein the top of the cooling pipe 4-1 is provided with an emptying exhaust port, and the bottom of the cooling pipe 4-1 is communicated with a chromatographic liquid sampling valve 5 through the second delivery pipe 4-3 with the needle valve 4-2; the pipeline 4-4 is arranged in the cooling pipe 4-1, one end of the pipeline 4-4 penetrates out from the left end of the cooling pipe 4-1, the penetrating end is communicated with the first conveying pipe 3, the other end of the pipeline 4-4 penetrates out from the right end of the cooling pipe 4-1, and the penetrating end is connected with the chromatographic liquid sample injection valve 5 through the third conveying pipe 6.
The liquefied petroleum gas sampling steel cylinder 1 stores liquefied petroleum gas in a liquid state (or not completely in the liquid state), and the liquefied petroleum gas is gasified in a low-pressure state, so that the gasification process absorbs heat.
The designed liquid sample introduction cooling device for realizing the chromatographic analysis requirement of the liquefied petroleum gas utilizes the principle of liquefied petroleum gas gasification heat absorption, the liquid petroleum gas which is blown into a sample introduction system of a chromatographic liquid sample introduction valve 5 before sample introduction firstly enters a cooling pipe 4-1 of a cooling mechanism 4 to be gasified, the temperature of the cooling pipe 4-1, a pipeline 4-4 in the cooling pipe 4-1 and a sample in the pipeline 4-4 are cooled, the cooled sample flows into a third conveying pipe 6 and is also cooled, the low-temperature sample and the low-temperature pipeline 4-4 can realize the phenomenon found in a window pipe, so that the pipeline between the third conveying pipe 6 and a second conveying pipe 4-3 is completely filled with liquid, and the temperature of the pipeline between the third conveying pipe 6 and the second conveying pipe 4-3 is low, so that bubbles can disappear in a short time.
The method comprises the following specific operations: the cylinder valve 2 is opened, the liquefied petroleum gas in the liquefied petroleum gas sampling cylinder 1 enters the first delivery pipe 3 and is delivered into a pipeline 4-4 communicated with the first delivery pipe 3, the liquefied petroleum gas is delivered into the chromatographic liquid sample injection valve 5 through the third delivery pipe 6, the needle valve 4-2 is adjusted, the liquid petroleum gas which is blown into the sample injection system of the chromatographic liquid sample injection valve 5 before sample injection is delivered into the cooling pipe 4-1 through the second delivery pipe 4-3, the liquid petroleum gas is sprayed into the cooling pipe 4-1 to be rapidly gasified and is discharged through the vent exhaust port, under the continuous sample blowing, the samples in the pipeline 4-4 and the pipeline 4-4 in the cooling pipe 4-1 are cooled, the cooled samples flow into the third delivery pipe 6, the third delivery pipe 6 is cooled, the needle valve 4-2 is closed, and the bubbles of the samples in the third delivery pipe 6 between the cooling pipe 4-1 and the needle valve 4-2 disappear, so that the quantitative pipe of the chromatographic liquid sample injection valve 5 is completely filled with liquid, and the accuracy of quantitative data is ensured.
Specifically, the pipeline 4-4 in the cooling pipe 4-1 is of a spiral structure and is used for increasing the contact area of the pipeline 4-4.
Specifically, a filter head 7 is arranged on a pipeline 4-4 which is positioned outside the cooling pipe 4-1 and connected with the first conveying pipe 3, and is used for filtering particles in a sample and avoiding abrasion of a chromatographic valve body.
Specifically, transparent polytetrafluoroethylene tubes for heat preservation are sleeved on the first conveying pipe 3 and the third conveying pipe 6 respectively.
Specifically, the cooling pipe 4-1 includes: 4-11 parts of a cylindrical pipe, 4-12 parts of a cylindrical pipe pressing cap, 4-13 parts of a pipeline sealing pressing cap and a sealing gasket; the two cylindrical pipe pressure caps 4-12 are respectively in threaded connection with two ends of the cylindrical pipe 4-11, and the two cylindrical pipe pressure caps 4-12 are also provided with a first through hole for the pipeline 4-4 to penetrate out; the number of the pipeline sealing pressure caps 4-13 is two, the two pipeline sealing pressure caps 4-13 are in threaded connection with the cylindrical pipe pressure cap 4-12, and a second through hole communicated with the first through hole is formed in the pipeline sealing pressure cap 4-13; the two sealing gaskets I are respectively arranged between the cylindrical pipe 4-11 and the cylindrical pipe pressing cap 4-12 and are used for sealing the cylindrical pipe 4-11; and two sealing gaskets II are arranged and are respectively arranged between the pipeline sealing pressing cap 4-13 and the pipeline 4-4 sleeved with the transparent polytetrafluoroethylene tube and used for sealing the gaps of the peripheral walls of the pipeline 4-4 penetrated by the first through hole and the second through hole.
The emptying exhaust port can be connected to an outer discharge pipeline of a laboratory, and is provided with an emptying exhaust pipe with the outer diameter of 6mm, the inner diameter and the wall thickness of 4mm and 1mm respectively, and the length of 20mm, and the emptying exhaust pipe is communicated with the outer discharge pipeline;
the inner diameter of the cylindrical pipe 4-11 is 10-12mm, and the length of the cylindrical pipe 4-11 is 80mm;
the diameter of line 4-4 may be 1/16 inch and the diameter of the clear polytetrafluoroethylene tube may be 1/8 inchOr3mm, wherein the diameter of the third duct 6 needs to be consistent with the diameter of the lines 4-4, the diameter may be 1/16 inch, 1/8 inch or 3mm pipe.
Installation operation of the cooling pipe 4-1: the 1/16 inch spiral pipeline 4-4 is sent into a cylindrical pipe 4-11, the two ends of the pipeline 4-4 penetrate through the two ends of the cylindrical pipe 4-11, each sealing gasket I penetrates through the pipeline 4-4 positioned outside the cylindrical pipe 4-11 and is sleeved on the penetrating end of the pipeline 4-4, the penetrating end of the pipeline 4-4 penetrates through a first through hole, then a cylindrical pipe pressing cap 4-12 is connected with the inner wall of the cylindrical pipe 4-11 in a threaded mode, the sealing gasket I is not easy to loosen when the cylindrical pipe pressing cap 4-12 is tightened, the sealing gasket I, the cylindrical pipe 4-11 and the cylindrical pipe pressing cap 4-12 are sealed, then the penetrating end of the pipeline 4-4 penetrates through a second through hole, then the pipeline sealing pressing cap 4-13 is connected with the cylindrical pipe pressing cap 4-12 in a threaded mode, and the sealing gasket II is arranged between the pipeline sealing pressing cap 4-13 and the pipeline 4-4 sleeved with the transparent polytetrafluoroethylene pipe and used for ensuring the integral sealing of the cylindrical pipe 4-11.
Specifically, the sealing gasket I and the sealing gasket II are both made of copper or aluminum.
Specifically, the cylindrical pipe 4-11, the cylindrical pipe press cap 4-12 and the pipeline sealing press cap 4-13 are all made of stainless steel or copper materials.
Specifically, first delivery pipe 3, second delivery pipe 4-3, pipeline 4-4, and third delivery pipe 6 are made of a metal material.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A liquid sample introduction cooling device for realizing the chromatographic analysis requirement of liquefied petroleum gas is characterized by comprising:
the device comprises a liquefied petroleum gas sampling steel cylinder (1), wherein a steel cylinder valve (2) and a first conveying pipe (3) are arranged on an outlet of the liquefied petroleum gas sampling steel cylinder (1);
cooling mechanism (4) for send into the sample cooling in chromatogram liquid injection valve (5) to liquefied petroleum gas sampling steel bottle (1), include:
the top of the cooling pipe (4-1) is provided with an emptying exhaust port, and the bottom of the cooling pipe is communicated with a chromatographic liquid sample injection valve (5) through a second conveying pipe (4-3) with a needle valve (4-2);
and the pipeline (4-4) is arranged inside the cooling pipe (4-1), one end of the pipeline penetrates out from the left end of the cooling pipe (4-1), the penetrating end of the pipeline is communicated with the first conveying pipe (3), the other end of the pipeline penetrates out from the right end of the cooling pipe (4-1), and the penetrating end of the pipeline is connected with the chromatographic liquid sample injection valve (5) through the third conveying pipe (6).
2. The device for reducing the temperature of a liquid sample injection for realizing the chromatographic analysis requirement of liquefied petroleum gas as claimed in claim 1, wherein the pipeline (4-4) positioned in the temperature reducing pipe (4-1) is of a spiral structure.
3. The liquid sample introduction cooling device for realizing the chromatographic analysis requirement of the liquefied petroleum gas as claimed in claim 2, wherein a filter head (7) is arranged on the pipeline (4-4) which is positioned outside the cooling pipe (4-1) and connected with the first conveying pipe (3).
4. The device for reducing the temperature of the liquid sample injection for realizing the chromatographic analysis requirement of the liquefied petroleum gas as claimed in claim 3, wherein the first delivery pipe (3) and the third delivery pipe (6) are respectively sleeved with a transparent polytetrafluoroethylene pipe for heat preservation.
5. The liquid sample introduction cooling device for realizing the chromatographic analysis requirement of the liquefied petroleum gas as claimed in any one of claims 1 to 4, wherein the cooling tube (4-1) comprises:
a cylindrical tube (4-11);
the two cylindrical pipe pressure caps (4-12) are arranged, the two cylindrical pipe pressure caps (4-12) are respectively in threaded connection with the two ends of the cylindrical pipe (4-11), and the two cylindrical pipe pressure caps (4-12) are also provided with first through holes for the pipeline (4-4) to penetrate out;
the number of the pipeline sealing pressure caps (4-13) is two, the two pipeline sealing pressure caps (4-13) are in threaded connection with the cylindrical pipe pressure cap (4-12), and a second through hole communicated with the first through hole is formed in each pipeline sealing pressure cap (4-13);
the number of the sealing gaskets I is two, and the two sealing gaskets I are respectively arranged between the cylindrical pipe (4-11) and the cylindrical pipe pressing cap (4-12);
and two sealing gaskets II are arranged and are respectively arranged between the pipeline sealing pressing cap (4-13) and the pipeline (4-4) sleeved with the transparent polytetrafluoroethylene tube.
6. The device for reducing the temperature of a liquid sample injection for realizing the chromatographic analysis requirement of liquefied petroleum gas according to claim 5, wherein the sealing gasket I and the sealing gasket II are both made of copper or aluminum.
7. The liquid sample introduction and temperature reduction device for realizing the chromatographic analysis requirement of the liquefied petroleum gas as claimed in claim 5, wherein the cylindrical tube (4-11), the cylindrical tube pressing cap (4-12) and the pipeline sealing pressing cap (4-13) are all made of stainless steel or copper material.
8. The device for reducing the temperature of a liquid sample for implementing the chromatographic analysis requirement on liquefied petroleum gas according to claim 1, wherein the first delivery pipe (3), the second delivery pipe (4-3), the pipeline (4-4) and the third delivery pipe (6) are made of a metal material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202221955558.1U CN218157736U (en) | 2022-07-27 | 2022-07-27 | Liquid sample introduction cooling device for realizing chromatographic analysis requirement of liquefied petroleum gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202221955558.1U CN218157736U (en) | 2022-07-27 | 2022-07-27 | Liquid sample introduction cooling device for realizing chromatographic analysis requirement of liquefied petroleum gas |
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| Publication Number | Publication Date |
|---|---|
| CN218157736U true CN218157736U (en) | 2022-12-27 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202221955558.1U Active CN218157736U (en) | 2022-07-27 | 2022-07-27 | Liquid sample introduction cooling device for realizing chromatographic analysis requirement of liquefied petroleum gas |
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| CN (1) | CN218157736U (en) |
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- 2022-07-27 CN CN202221955558.1U patent/CN218157736U/en active Active
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