CN207601025U - A kind of enriching apparatus that trace impurity in hydrogen is measured applied to gas chromatography - Google Patents
A kind of enriching apparatus that trace impurity in hydrogen is measured applied to gas chromatography Download PDFInfo
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- CN207601025U CN207601025U CN201721833667.5U CN201721833667U CN207601025U CN 207601025 U CN207601025 U CN 207601025U CN 201721833667 U CN201721833667 U CN 201721833667U CN 207601025 U CN207601025 U CN 207601025U
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Abstract
The utility model provides a kind of enriching apparatus that trace impurity in hydrogen is measured applied to gas chromatography, including air inlet pipe, air outlet pipe, evaporating column, six-way valve, wobble gear, jacking apparatus and Secure Shell, pressure reducing valve, the first shut-off valve and gaseous mass flowmeter, air inlet pipe are equipped in air inlet pipe successively to connect with six-way valve；Wobble gear is equipped with enrichment absorption position A and desorption desorption sites B, and enrichment absorption position A is equipped with low-temperature receiver Dewar cup, and desorption desorption sites B is equipped with heat source Dewar cup.The utility model is enriched with gas interior with respect to high-boiling-point impurity in a manner that gas is by low temperature evaporating column, and the gaseous impurity content after enrichment reaches corresponding instrument detection limit requirement；Gas gross is in opposite air-tight state, is increased safety using gas mass flow gauge control flow and accurate quantification, the switching of adsorption desorption, improves the accuracy of the gas chromatographic detection analysis of foreign gas.
Description
Technical field
The utility model is related to the gas chromatography detection fields of gas, and in particular to one kind is applied to gas chromatography and surveys
Determine the enriching apparatus of trace impurity in hydrogen.
Background technology
Gas chromatograph, which is directed to gas with various impurity in different hydrogen, different detection limit, as PH3 uses FPD
Detector is up to 0.1 × 10-6（Volume fraction）, CH4 is in 0.1 × 10-6 for FID measure（Volume fraction）, TCD measure hydrogen in N2,
O2 etc. is in 1 × 10-6（Volume fraction）More than.In hydrogen the gaseous impurity of trace on conventional gas phase chromatograph machine testing by
To the limitation of detection limit, it is impossible to meet the requirement of detector.Therefore it needs to be enriched with the sample gas for entering instrument, to reach
To the purpose of detection.
Invention content
It is applied to gas chromatography the technical problem to be solved by the utility model is to provide one kind and measures trace in hydrogen
The enriching apparatus of impurity, is enriched with and evaporating column under cryogenic by gaseous impurity, is desorbed at a temperature of being above the boiling point, is reached sample
The purpose of product enrichment, improves safety and foreign gas test accuracy.
In order to solve the above technical problems, technical solution is used by the utility model：One kind is applied to gas chromatography
The enriching apparatus of trace impurity in hydrogen is measured, including with lower component：
Air inlet pipe, air inlet pipe are equipped with pressure reducing valve, the first shut-off valve and gaseous mass flowmeter, and air inlet pipe connects with six-way valve
It connects；
Air outlet pipe, tracheae are connect with six-way valve, and air outlet pipe is equipped with the second shut-off valve；
Evaporating column, evaporating column are connect with six-way valve by pipeline；
Six-way valve, adjacent holes connects carrier gas pipe and gas chromatograph respectively on six-way valve；
Wobble gear, wobble gear are equipped with enrichment absorption position A and desorption desorption sites B, and enrichment absorption position A is equipped with
Low-temperature receiver Dewar cup, desorption desorption sites B are equipped with heat source Dewar cup；
Jacking apparatus, jacking apparatus are located at the lower section of evaporating column.
In preferred embodiment, Secure Shell, safety are equipped in the outside of evaporating column, six-way valve, wobble gear and jacking apparatus
Shell is externally provided with direction switch and Swinging switch.
In preferred embodiment, enrichment absorption position A and desorption desorption sites B on Swinging switch control wobble gear
Switching.
In preferred embodiment, the direction switch controls the lifting of jacking apparatus.
In preferred embodiment, the jacking apparatus is contacted with low-temperature receiver Dewar cup and heat source Dewar cup.
In preferred embodiment, the low-temperature receiver Dewar cup and heat source Dewar cup interior diameter are bigger than the diameter of evaporating column.
In preferred embodiment, the evaporating column and gas chromatograph can be selected according to dopant type.
In preferred embodiment, the Secure Shell uses the material of transparent thermal insulation.
In preferred embodiment, connected inside the six-way valve.
In preferred embodiment, liquid nitrogen, low-temperature oil etc. can be placed in the low-temperature receiver Dewar cup as low-temperature receiver；In heat source Dewar cup
Hot water etc. can be placed as heat source.
The utility model has the advantages that：
1）Under cryogenic some boiling temperatures are higher than with the foreign gas suction-operated of low-temperature receiver using evaporating column, to reach
To the enrichment to gaseous impurity；
2）The application of gas mass flow gauge, using the gas mass flow controller with integrating instrument, accurately to being enriched with
Hydrogen flowing quantity in journey is controlled, and calculates final total volume；
3）The use of jacking apparatus and wobble gear realizes automatic switchover of the evaporating column between adsorption-desorption；
4）Shell is protected, is related to the use of low temperature cold source, prevents the injury of personnel in detection process, increases and uses process
Personnel safety coefficient；
5）Gas after enrichment brings chromatograph detection into through carrier gas, further reduces the detection limit of corresponding defects inspecting, carries
Height automation efficiency improves the accuracy of the gas chromatographic detection analysis of foreign gas.
Description of the drawings
The utility model is described in further detail with reference to the accompanying drawings and examples：
Fig. 1 is the structure diagram of the utility model（When sample is adsorbed and is desorbed）.
Fig. 2 is the structure diagram of the utility model（During sample test）.
Fig. 3 is the wobble gear schematic top plan view of the utility model.
In figure：Air inlet pipe 1, pressure reducing valve 2, the first shut-off valve 3, gas mass flow gauge 4, evaporating column 5, six-way valve 6, second
Shut-off valve 7, air outlet pipe 8, carrier gas pipe 9, gas chromatograph 10, enrichment absorption position A 11, desorption desorption sites B 12 swing tooth
Wheel 13, jacking apparatus 14, direction switch 15, Swinging switch 16, low-temperature receiver Dewar cup 17, heat source Dewar cup 18, Secure Shell 19.
Specific embodiment
Fig. 3 is incomplete wobble gear schematic top plan view, and referring in Fig. 1 ~ 3, one kind is applied to gas chromatography and measures
The enriching apparatus of trace impurity in hydrogen, including with lower component：
Air inlet pipe 1, air inlet pipe 1 are equipped with pressure reducing valve 2, the first shut-off valve 3 and gaseous mass flowmeter 4, the first shut-off valve 3
Between pressure reducing valve 2 and gaseous mass flowmeter 4, gas pressure in 2 control device of pressure reducing valve protects rear end electric elements, control
System enters the gas pressure of evaporating column 5；Gas mass flow gauge 4 is connect by air inlet pipe 1 with six-way valve 6, and gas gross uses
Gas mass flow gauge control flow and accurate quantification；
Air outlet pipe 8, air outlet pipe 8 is equipped with the second shut-off valve 7, the second shut-off valve 7 is connect by air outlet pipe 8 with six-way valve 6；
Evaporating column 5, evaporating column 5 are connect with six-way valve 6 by pipeline, and air inlet pipe 1, air outlet pipe 8 and carrier gas pipe 9 can be used not
Become rusty steel pipe, and outer diameter can be used as eighth stainless steel tube in the pipeline that connection function is played in figure；
Six-way valve 6, adjacent holes connects carrier gas pipe 9 and gas chromatograph 10 respectively on six-way valve 6；
Wobble gear 13, wobble gear 13 are equipped with enrichment absorption position A 11 and desorption desorption sites B 12, and enrichment is inhaled
Attached position A 11 is equipped with low-temperature receiver Dewar cup 17, and desorption desorption sites B 12 is equipped with heat source Dewar cup 18；
Jacking apparatus 14, jacking apparatus 14 are located at the lower section of evaporating column 5, and wobble gear 13 and jacking apparatus 14 use cylinder
Control to be slowly steadily advisable, can automatically switch in absorption low-temperature receiver reconciliation heat sink, reduce manual operation, avoid the jelly of people
Wound etc..
In preferred embodiment, Secure Shell is equipped in the outside of evaporating column 5, six-way valve 6, wobble gear 13 and jacking apparatus 14
19, Secure Shell 19 is externally provided with direction switch 15 and Swinging switch 16, is conveniently operated, and avoids danger.
In preferred embodiment, enrichment absorption position A 11 and desorption desorption on the Swinging switch 16 control wobble gear 13
The switching of position B 12, can accurately switching position, when lifting low-temperature receiver Dewar cup 17, can fit together perfectly.
In preferred embodiment, the direction switch 15 controls the lifting of jacking apparatus 14, and control evaporating column 5 is in low-temperature receiver and heat
Switching in source.
In preferred embodiment, the jacking apparatus 14 contacts, but be not fixed with low-temperature receiver Dewar cup 17 and heat source Dewar cup 18.
In preferred embodiment, the low-temperature receiver Dewar cup 17 and 18 interior diameter of heat source Dewar cup are bigger than the diameter of evaporating column 5, just
It can be put into low-temperature receiver Dewar cup 17 and heat source Dewar cup 18 in evaporating column 5.
In preferred embodiment, the evaporating column 5 and gas chromatograph 10 can be selected according to dopant type, evaporating column 5
It is selected with gas absorption and gaseous impurity polarity, as SE-30 evaporating columns may be selected in the concentration of phosphine gas in hydrogen；If
Containing hydrogen phosphide impurity, GC-FPD can be selected in gas chromatograph 10, if aerobic, selects GC-TCD.
In preferred embodiment, the Secure Shell 19 using transparent thermal insulation material, protect low-temperature receiver, isolation manual operation and
People's frost bitten is prevented, can be designed using transparent organic glass material form, convenient for the observation in experimentation.
In preferred embodiment, 6 inside of six-way valve connects, and changes 6 inner connecting way of six-way valve by torsion.
In preferred embodiment, liquid nitrogen or low-temperature oil etc. can be placed in the low-temperature receiver Dewar cup 17 as low-temperature receiver；Heat source Dewar
Hot water etc. can be placed in cup 18 as heat source.
The operation principle and process of the utility model are as follows：
1）Pipeline purges：Such as Fig. 1, air inlet pipe 1 is passed through sample gas, pressure reducing valve 2 is adjusted and divides to 0.3 ~ 0.4MPa, beat
Open the first shut-off valve 3, setting gas mass flow gauge 4 controls 300 ~ 500mL of flow, opens the second shut-off valve 7, under test gas pair
Enriching apparatus is purged；It purges and completes the first shut-off valve 3 of closing, after flow back to zero, close the second shut-off valve 7；
2）Sample adsorbs：Such as Fig. 1 and Fig. 3, the first shut-off valve 3 is opened, cushion steam in evaporating column 5 is pressed on Swinging switch 16
A buttons, wobble gear 13 goes to enrichment absorption position A 11, presses the liter button of direction switch 15, jacking apparatus 14 will be cold
Source Dewar cup 17 rises, after column 5 to be concentrated is cooled to enrichment low temperature（It can be controlled by timing, more than 3min）, open the second cut-off
Valve 7, sample start to be enriched with；At this point, foreign gas is enriched in evaporating column 5, background gas is vented from air outlet pipe 8；Reach predetermined
After volume（Total volume is checked by gas mass flow gauge 4）The first shut-off valve 3 is closed, flow is returned in gas mass flow gauge 4
After zero, the second shut-off valve 7 is closed, absorption is completed；
3）Sample desorbs：Such as Fig. 1 and Fig. 3, the drop button of direction switch 15 is pressed, falls the low-temperature receiver of enrichment absorption position A 11
Dewar cup 17；The B buttons of Swinging switch 16 are pressed, wobble gear 13 is rocked to desorption desorption sites B 12, presses direction switch
15 liter button；Start timing desorption time（Desorption time is related with the type selecting and foreign gas type of evaporating column 5, general 1 ~
3min）, reach the drop button that direction switch 15 is pressed after desorption time, desorption is completed；
4）Sample test：Such as Fig. 2, six-way valve 6 is rotated, while press 10 START button of gas chromatograph, in carrier gas pipe 9
By gas by enriched sample brings gas chromatograph 10, sample test into evaporating column 5.
The above embodiments are only the optimal technical scheme of the utility model, and are not construed as the limit for the utility model
System, the technical solution that the scope of protection of the utility model should be recorded with claim, the technical solution recorded including claim
The equivalents of middle technical characteristic are protection domain.Equivalent replacement i.e. within this range is improved, also in the utility model
Protection domain within.
Claims (9)
1. a kind of enriching apparatus that trace impurity in hydrogen is measured applied to gas chromatography, it is characterized in that including with lower component：
Air inlet pipe（1）, air inlet pipe（1）It is equipped with pressure reducing valve（2）, the first shut-off valve（3）With gaseous mass flowmeter（4）, air inlet
Pipe（1）With six-way valve（6）Connection；
Air outlet pipe（8）, air outlet pipe（8）With six-way valve（6）Connection, air outlet pipe（8）Equipped with the second shut-off valve（7）；
Evaporating column（5）, evaporating column（5）With six-way valve（6）It is connected by pipeline；
Six-way valve（6）, six-way valve（6）Upper adjacent holes connects carrier gas pipe respectively（9）And gas chromatograph（10）；
Wobble gear（13）, wobble gear（13）It is equipped with enrichment absorption position A（11）With desorption desorption sites B（12）, enrichment
Absorption position A（11）Equipped with low-temperature receiver Dewar cup（17）, desorption desorption sites B（12）Equipped with heat source Dewar cup（18）；
Jacking apparatus（14）, jacking apparatus（14）It is located at evaporating column（5）Lower section.
2. a kind of enriching apparatus that trace impurity in hydrogen is measured applied to gas chromatography according to claim 1,
It is characterized in：In evaporating column（5）, six-way valve（6）, wobble gear（13）And jacking apparatus（14）Outside be equipped with Secure Shell
（19）, Secure Shell（19）It is externally provided with direction switch（15）And Swinging switch（16）.
3. a kind of enriching apparatus that trace impurity in hydrogen is measured applied to gas chromatography according to claim 2,
It is characterized in：The Swinging switch（16）Control wobble gear（13）Upper enrichment absorption position A（11）With desorption desorption sites B
（12）Switching.
4. a kind of enriching apparatus that trace impurity in hydrogen is measured applied to gas chromatography according to claim 2,
It is characterized in：The direction switch（15）Control jacking apparatus（14）Lifting.
5. a kind of enriching apparatus that trace impurity in hydrogen is measured applied to gas chromatography according to claim 1,
It is characterized in：The jacking apparatus（14）With low-temperature receiver Dewar cup（17）With heat source Dewar cup（18）Contact.
6. a kind of enriching apparatus that trace impurity in hydrogen is measured applied to gas chromatography according to claim 1,
It is characterized in：The low-temperature receiver Dewar cup（17）With heat source Dewar cup（18）Interior diameter compares evaporating column（5）Diameter it is big.
7. a kind of enriching apparatus that trace impurity in hydrogen is measured applied to gas chromatography according to claim 2,
It is characterized in：The Secure Shell（19）Using the material of transparent thermal insulation.
8. a kind of enriching apparatus that trace impurity in hydrogen is measured applied to gas chromatography according to claim 1,
It is characterized in：The six-way valve（6）Inside connection.
9. a kind of enriching apparatus that trace impurity in hydrogen is measured applied to gas chromatography according to claim 1,
It is characterized in：The low-temperature receiver Dewar cup（17）Middle placement liquid nitrogen or low-temperature oil are as low-temperature receiver；Heat source Dewar cup（18）It is middle to place heat
Water is as heat source.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721833667.5U CN207601025U (en) | 2017-12-25 | 2017-12-25 | A kind of enriching apparatus that trace impurity in hydrogen is measured applied to gas chromatography |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721833667.5U CN207601025U (en) | 2017-12-25 | 2017-12-25 | A kind of enriching apparatus that trace impurity in hydrogen is measured applied to gas chromatography |
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| Publication Number | Publication Date |
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| CN207601025U true CN207601025U (en) | 2018-07-10 |
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| CN201721833667.5U Active CN207601025U (en) | 2017-12-25 | 2017-12-25 | A kind of enriching apparatus that trace impurity in hydrogen is measured applied to gas chromatography |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112557122A (en) * | 2020-12-07 | 2021-03-26 | 唐山中浩化工有限公司 | Sampling device for measuring trace sulfide in hydrogen |
| CN114441282A (en) * | 2020-11-02 | 2022-05-06 | 中国石油化工股份有限公司 | Concentration and enrichment device and method for rare gas in soil gas and application |
-
2017
- 2017-12-25 CN CN201721833667.5U patent/CN207601025U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114441282A (en) * | 2020-11-02 | 2022-05-06 | 中国石油化工股份有限公司 | Concentration and enrichment device and method for rare gas in soil gas and application |
| CN114441282B (en) * | 2020-11-02 | 2024-05-07 | 中国石油化工股份有限公司 | Concentration and enrichment device for rare gas in soil gas, concentration and enrichment method and application |
| CN112557122A (en) * | 2020-12-07 | 2021-03-26 | 唐山中浩化工有限公司 | Sampling device for measuring trace sulfide in hydrogen |
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