CN213397846U - Sampling device for measuring trace sulfide in hydrogen - Google Patents
Sampling device for measuring trace sulfide in hydrogen Download PDFInfo
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- CN213397846U CN213397846U CN202022932535.6U CN202022932535U CN213397846U CN 213397846 U CN213397846 U CN 213397846U CN 202022932535 U CN202022932535 U CN 202022932535U CN 213397846 U CN213397846 U CN 213397846U
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Abstract
The utility model discloses a sampling device of trace sulphide in survey hydrogen, including the gas conduit, the gas conduit communicates the needle valve in proper order, gas flowmeter and concentrated enrichment pipe, the one end of concentrated enrichment pipe is provided with enrichment union coupling head, the other end of concentrated enrichment pipe is provided with the gas chromatography connector, concentrated enrichment pipe sets up the inside at cold hydrazine liquid nitrogen container, the top of cold hydrazine liquid nitrogen container is provided with liquid nitrogen container apron, the higher authority of liquid nitrogen container apron is provided with fills the liquid nitrogen hole, enrichment union coupling head and gas chromatography connector set up the top at liquid nitrogen container apron, be provided with the electrical heating line joint on the enrichment union coupling. The utility model discloses with the sulphide solidification in the hydrogen of certain volume, concentration in the concentrated enrichment pipe that is filled with the adsorbent under the low temperature effect, let in the chromatogram carrier gas and add concentrated enrichment pipe to concentrated enrichment pipe in, evaporate, isolate the concentrated sulphide of solidification, get into gas chromatograph and then detect sulphide content along with the carrier gas.
Description
Technical Field
The utility model relates to a chemical production sampling technical field especially relates to a sampling device of trace sulphide in survey hydrogen.
Background
In some chemical processes, the requirement on the content of sulfides in hydrogen is high, the content of the sulfides is required to be controlled at ppb level, the sample introduction amount of gas chromatography is limited by volume, the detection limit of the chromatography cannot meet the detection requirement on ppb level trace sulfides in the hydrogen, and the sulfides are easily adsorbed by using sampling articles such as air bag bladders and the like.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a sampling device of trace sulphide in survey hydrogen solves the easy sulphide that adsorbs of current sample articles for use, can't reach the problem that detects the requirement.
In order to solve the technical problem, the utility model adopts the following technical scheme:
the utility model relates to a sampling device of trace sulphide in survey hydrogen, including the gas conduit, the gas conduit communicates needle valve, gas flowmeter and concentrated enrichment pipe in proper order, the one end of concentrated enrichment pipe is provided with enrichment union coupling head, the other end of concentrated enrichment pipe is provided with the gas chromatography connector, concentrated enrichment pipe sets up the inside at cold hydrazine liquid nitrogen container, the top of cold hydrazine liquid nitrogen container is provided with liquid nitrogen tank apron, the higher authority of liquid nitrogen tank apron is provided with fills the liquid nitrogen hole, enrichment union coupling head with the gas chromatography connector sets up the top of liquid nitrogen tank apron, be provided with the electrical heating line joint on the enrichment union coupling head.
Furthermore, the concentration and enrichment pipe comprises a wavy hollow glass pipe, an electric heating wire is arranged on the outer side of the glass pipe, heat insulation cotton is arranged on the outer side of the electric heating wire, and fillers in the enrichment pipe are filled in the glass pipe.
Still further, a temperature control sensor is arranged inside the electric heating wire, and 25% beta' -dicyanoethyl ether is adopted as a filler in the enrichment tube.
Still further, the gas conduit is provided as a transparent polytetrafluoroethylene hose.
Still further, the gas chromatography connector is set as a stainless steel needle.
Still further, the enriching tube connector is made of stainless steel.
Compared with the prior art, the utility model discloses a beneficial technological effect:
the utility model relates to a sampling device for measuring trace sulfide in hydrogen, which comprises a gas conduit, a needle valve, a gas flowmeter, a concentration pipe connector, a gas chromatography connector, a cold hydrazine liquid nitrogen tank, a liquid nitrogen tank cover plate, an electric heating wire connector, heat preservation cotton, an electric heating wire and a filler in the concentration pipe, wherein the needle valve is used for controlling the flow rate of gas entering the sampling device; the gas flow meter is used for monitoring the flow velocity and flow of gas entering the sampling device; the cold hydrazine liquid nitrogen tank is used for cooling hydrogen, prolonging the retention time of the gas in the enrichment tube and ensuring that sulfides in the gas are adsorbed; the concentration enrichment tube is made of glass materials, so that the sulfide in hydrogen is prevented from being adsorbed, and 25% beta-dicyanoethyl ether is adopted as a filler in the enrichment tube, so that the sulfide in the hydrogen is completely adsorbed; the gas chromatography connector is a stainless steel needle head, can be conveniently connected to a chromatograph, and has good adaptability with the instrument; the utility model discloses with the sulphide enrichment concentration in the hydrogen, solved the gas chromatograph and detected the detection requirement that trace ppb level sulfur content can't satisfy in the hydrogen limit, enrichment pipe glass material has avoided the problem that gas sampling articles for use such as air pocket, ball courage adsorbed sulphur, and sampling device uses the back, detects repeatability good.
Drawings
The present invention will be further explained with reference to the following description of the drawings.
FIG. 1 is a schematic structural view of the utility model during sampling;
FIG. 2 is a schematic structural diagram of the present invention for detecting sulfide in a sample;
FIG. 3 is a horizontal sectional view of the concentrating and enriching tube of the present invention;
description of reference numerals: 1. a gas conduit; 2. a needle valve; 3. a gas flow meter; 4. filling a liquid nitrogen hole; 5. a gas chromatography connector; 6. a cover plate of the liquid nitrogen tank; 7. a concentration enrichment pipe; 8. a cold hydrazine liquid nitrogen tank; 9. a enriching pipe connector; 10. an electrical heater wire connector; 7-1, heat preservation cotton; 7-2, an electric heating wire; 7-3, enriching the filler in the tube; 7-4, glass tube.
Detailed Description
As shown in fig. 1-3, a sampling device for measuring trace sulfides in hydrogen comprises a gas conduit 1, wherein the gas conduit 1 is sequentially communicated with a needle valve 2, a gas flowmeter 3 and a concentration and enrichment pipe 7, an enrichment pipe connector 9 is installed at one end of the concentration and enrichment pipe 7, a gas chromatography connector 5 is installed at the other end of the concentration and enrichment pipe 7, the concentration and enrichment pipe 7 is arranged inside a cold hydrazine liquid nitrogen tank 8, a liquid nitrogen tank cover plate 6 is arranged at the top of the cold hydrazine liquid nitrogen tank 8, a liquid nitrogen filling hole 4 is formed in the liquid nitrogen tank cover plate 6, the enrichment pipe connector 9 and the gas chromatography connector 5 are arranged above the liquid nitrogen tank cover plate 6, and an electric heating wire connector 10 is arranged on the enrichment pipe connector 9; the needle valve 2 is used for controlling the flow rate of gas entering the sampling device; the gas flowmeter 3 is used for monitoring the flow velocity and flow of gas entering the sampling device; the cold hydrazine liquid nitrogen tank 8 is used for cooling hydrogen, prolonging the retention time of the gas in the concentration and enrichment pipe 7 and ensuring that sulfide in the gas is completely adsorbed.
Specifically, as shown in fig. 3, the concentration and enrichment pipe 7 comprises a wavy hollow glass pipe 7-4, the glass material is adopted to avoid adsorption on sulfides in hydrogen, an electric heating wire 7-2 is arranged on the outer side of the glass pipe 7-4, heat insulation cotton 7-1 is arranged on the outer side of the electric heating wire 7-2, and filling materials 7-3 in the concentration pipe are filled in the glass pipe 7-4.
A temperature control sensor is arranged in the electric heating wire 7-2, and 25% beta' -dicyanoethyl ether is adopted as the filler 7-3 in the enrichment tube, so that the sulfide in the hydrogen is completely adsorbed.
The gas conduit 1 is provided as a transparent polytetrafluoroethylene hose.
The gas chromatography connector 5 is a stainless steel needle head, can be conveniently connected to a chromatograph, and has good adaptability to the instrument.
The enriching pipe connector 9 is made of stainless steel.
A sampling mode for measuring trace sulfide in hydrogen is characterized in that: the sampling mode adopts the sampling device for measuring the trace sulfide in the hydrogen to realize the sampling of the trace sulfide in the hydrogen, and the specific process steps are as follows:
the first step is as follows: before sampling, the gas conduit 1 is communicated with the needle valve 2, the gas flowmeter 3 and the concentration enrichment pipe 7 in sequence;
the second step is that: during sampling, the gas conduit 1 is communicated with a hydrogen sampling point;
the third step: opening a hydrogen valve, and allowing the gas to be detected to sequentially flow into the needle valve 2, the gas flowmeter 3 and the concentration and enrichment pipe 7 through the gas guide pipe 1;
the fourth step: adjusting the needle valve 2, and controlling the gas flow rate to be 0.2L/min;
the fifth step: after the gas flow rate is stable, placing the concentration and enrichment pipe 7 in the cold hydrazine liquid nitrogen tank 8, and covering the liquid nitrogen tank cover plate 6;
and a sixth step: stopping sampling when the sampling volume reaches 2L, closing a hydrogen valve, disconnecting the enrichment pipe connector 9 and the gas guide pipe 1, immediately plugging the gas chromatography connector 5 by a silica gel pad, preventing air from being sucked back into the sampling device, and disconnecting all connection points of the gas guide pipe 1;
the seventh step: when detecting sample sulphide, the concentrated enrichment pipe 7 is taken out of the cold trap liquid nitrogen tank 8, the gas chromatography connector 5 and the enrichment pipe connector 9 are connected to the gas chromatography, then the electric heating wire connector 10 is powered on, carrier gas is introduced, the heating function is started, and the sulphide solidified and concentrated in the concentrated enrichment pipe 7 is evaporated by heating and enters a gas chromatograph along with the carrier gas for detection.
The utility model solidifies and concentrates the sulfides in the hydrogen with a certain volume in the concentration enrichment pipe filled with the adsorbent under the action of low temperature, and introduces chromatographic carrier gas into the concentration enrichment pipe and heats the concentration enrichment pipe, so as to evaporate and separate the sulfides which are solidified and concentrated, and then the sulfides enter a gas chromatograph along with the carrier gas to detect the sulfide content; the utility model provides a gas chromatograph detect the limit and can't satisfy the detection requirement of trace ppb level sulphur content in the hydrogen, the problem of gas sampling articles for use absorption sulphur such as air pocket, ball courage has been avoided to concentrated enrichment pipe glass material, and sampling device uses the back, detects repeatability good.
The above-mentioned embodiments are only intended to describe the preferred embodiments of the present invention, but not to limit the scope of the present invention, and those skilled in the art should also be able to make various modifications and improvements to the technical solution of the present invention without departing from the spirit of the present invention, and all such modifications and improvements are intended to fall within the scope of the present invention as defined in the appended claims.
Claims (6)
1. A sampling device for measuring trace sulfide in hydrogen is characterized in that: including gas conduit (1), gas conduit (1) communicates needle valve (2), gas flowmeter (3) and concentrated enrichment pipe (7) in proper order, the one end of concentrated enrichment pipe (7) is provided with enrichment union coupling head (9), the other end of concentrated enrichment pipe (7) is provided with gas chromatography connector (5), concentrated enrichment pipe (7) set up the inside at cold hydrazine liquid nitrogen container (8), the top of cold hydrazine liquid nitrogen container (8) is provided with liquid nitrogen tank cover board (6), be provided with on liquid nitrogen tank cover board (6) and fill liquid nitrogen hole (4), enrichment union coupling head (9) with gas chromatography connector (5) set up the top of liquid nitrogen container cover board (6), be provided with electric heating line joint (10) on enrichment union coupling head (9).
2. The sampling device for measuring trace sulfides in hydrogen according to claim 1, wherein: the concentration and enrichment pipe (7) comprises a wave-shaped hollow glass pipe (7-4), an electric heating wire (7-2) is arranged on the outer side of the glass pipe (7-4), heat insulation cotton (7-1) is arranged on the outer side of the electric heating wire (7-2), and an enrichment pipe inner filler (7-3) is filled in the glass pipe (7-4).
3. The sampling device for measuring trace sulfides in hydrogen according to claim 2, wherein: a temperature control sensor is arranged in the electric heating wire (7-2), and 25% beta' -dicyanoethyl ether is adopted as the filler (7-3) in the enrichment tube.
4. The sampling device for measuring trace sulfides in hydrogen according to claim 1, wherein: the gas conduit (1) is arranged as a transparent polytetrafluoroethylene hose.
5. The sampling device for measuring trace sulfides in hydrogen according to claim 1, wherein: the gas chromatography connector (5) is a stainless steel needle.
6. The sampling device for measuring trace sulfides in hydrogen according to claim 1, wherein: the enriching pipe connector (9) is made of stainless steel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202022932535.6U CN213397846U (en) | 2020-12-07 | 2020-12-07 | Sampling device for measuring trace sulfide in hydrogen |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202022932535.6U CN213397846U (en) | 2020-12-07 | 2020-12-07 | Sampling device for measuring trace sulfide in hydrogen |
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| Publication Number | Publication Date |
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| CN213397846U true CN213397846U (en) | 2021-06-08 |
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| CN202022932535.6U Active CN213397846U (en) | 2020-12-07 | 2020-12-07 | Sampling device for measuring trace sulfide in hydrogen |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114383903A (en) * | 2021-12-24 | 2022-04-22 | 同方威视技术股份有限公司 | Trace gas sampling equipment and detection system |
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2020
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114383903A (en) * | 2021-12-24 | 2022-04-22 | 同方威视技术股份有限公司 | Trace gas sampling equipment and detection system |
| CN114383903B (en) * | 2021-12-24 | 2023-05-09 | 同方威视技术股份有限公司 | Trace gas sampling device and detection system |
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