CN102628846A - Gas chromatography detection system and method for analyzing trace impurities in ultrahigh pure gas - Google Patents
Gas chromatography detection system and method for analyzing trace impurities in ultrahigh pure gas Download PDFInfo
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- CN102628846A CN102628846A CN201210115679XA CN201210115679A CN102628846A CN 102628846 A CN102628846 A CN 102628846A CN 201210115679X A CN201210115679X A CN 201210115679XA CN 201210115679 A CN201210115679 A CN 201210115679A CN 102628846 A CN102628846 A CN 102628846A
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- 239000012535 impurity Substances 0.000 title claims abstract description 37
- 238000001514 detection method Methods 0.000 title claims abstract description 28
- 238000004817 gas chromatography Methods 0.000 title claims abstract description 22
- 239000007789 gas Substances 0.000 claims abstract description 136
- 239000002808 molecular sieve Substances 0.000 claims abstract description 77
- 239000001307 helium Substances 0.000 claims abstract description 29
- 229910052734 helium Inorganic materials 0.000 claims abstract description 29
- -1 helium ion Chemical class 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000005070 sampling Methods 0.000 claims abstract description 7
- 238000004587 chromatography analysis Methods 0.000 claims description 78
- 238000000926 separation method Methods 0.000 claims description 70
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 58
- 229910052757 nitrogen Inorganic materials 0.000 claims description 29
- 238000004458 analytical method Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000010926 purge Methods 0.000 claims description 8
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium(0) Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 230000035945 sensitivity Effects 0.000 claims description 6
- 206010037544 Purging Diseases 0.000 claims description 4
- 150000003568 thioethers Chemical class 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000011010 flushing procedure Methods 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 7
- 239000012159 carrier gas Substances 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000004450 types of analysis Methods 0.000 description 4
- 238000007664 blowing Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000001536 pulsed discharge helium ionisation detection Methods 0.000 description 3
- 238000001223 reverse osmosis Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000004868 gas analysis Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N oxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 210000004369 Blood Anatomy 0.000 description 1
- 108060003095 GAS2 Proteins 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 201000007197 atypical autism Diseases 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000000875 corresponding Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atoms Chemical class [H]* 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000004801 process automation Methods 0.000 description 1
- 230000001105 regulatory Effects 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
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Abstract
The invention relates to detection equipment and technology for a gas chromatography instrument, in particular to a gas chromatography detection system and method for analyzing trace impurities in ultrahigh pure gas. A first molecular sieve chromatographic column (51) is arranged between a switching valve VI (1) and a switching valve VII (2); a second molecular sieve chromatographic column (52) is arranged between a switching valve VII (2) and a switching valve VIV (4); and a second column separator (62) is arranged between the switching valve VIII (3) and switching valve VIV (4). A secondary sampling way is adopted for sample gas, and a main component is pre-cut during primary sample feeding of a ten-way switching valve VI (1) and subjected to back flushing during secondary sample feeding of the ten-way switching valve VI (1); and the main component is separated and switched, and enters a helium ion detector (8) for analyzing. The gas chromatography detecting system is controlled through each valve, the sequence of actions is executed by using an event draw-up program, the entire analyzing process is controlled automatically, actions are rapid, consistent and reliable, and the data repeatability and accuracy of the system are ensured through a stable flow gas channel and accurate valve switching.
Description
Technical field
The present invention relates to a kind of gas chromatograph checkout equipment and detection technique, relate in particular to trace impurity is analyzed in ultra-pure gas gas-chromatography detection system and method.
Background technology
At present, the domestic gas chromatograph that is used for Analysis of Gases of High Purity is generally all used and is adopted traditional T CD and FID or zirconia detecting device; Their detecting device is technology tradition or backwardness mostly; And very strong to impurity analysis selectivity in the gas, a kind of gas is often wanted many stratographic analyses, and the flow process abbreviated analysis component of analyzing repeatedly; System is less demanding to gas circuit, makes the big reduction of detection sensitivity of system; Gas chromatographic analysis is in multi-dimensional chromatograph isolation technics scheme, and often requiring nearly, 5-6 props up the chromatographic resolution pillar; And the special-purpose again transfer valve of the connection of the gas circuit between the multi-dimensional chromatograph pillar is realized; Particularly be applied in the gas separate colors spectrometer requirement that the design of many gas circuits independence temperature control post case has solved different column temperatures.
Fast development along with China's industrial economy; Gas has the title of " blood " in commercial production; Supply and demand two is prosperous; The production of high-purity gas and ultra-pure gas and supply make new in recent years gas industry national standard, in the standard that promulgation is carried out after particularly 2006,2008,2009 etc., like high (superelevation) pure hydrogen, height (superelevation) purity nitrogen, high-purity (superelevation) argon, high-purity (superelevation) helium, high-purity (superelevation) oxygen; Industrial gasses and used in electronic industry gas such as liquid nitrogen, liquid argon, liquid oxygen; In the standard because of having stipulated use ng/g (ppb) level highly sensitive PDHID helium ionization detector (being called for short PDD among this paper); This guarantees especially in the gas that to whole chromatographic analysis system trace or vestige component get into the PDHID detector response effectively, is that present pendulum is researched and developed a new problem in face of the Analysis of Gases of High Purity chromatogram at home; Company's design one cover is fit to national conditions for this reason, the user accepts, analyzes required ultra-pure gas chromatographic analysis flow process that is exclusively used in, and improves the gas-chromatography detection method that trace impurity is analyzed in ultra-pure gas.
Summary of the invention
The present invention is directed to gas chromatograph detector technologies tradition common in the prior art or backward; And it is very strong to impurity analysis selectivity in the gas; A kind of gas is often wanted many stratographic analyses; And the flow process abbreviated analysis component of analyzing repeatedly, and system is less demanding to gas circuit, makes the shortcomings such as the big reduction of detection sensitivity of system that a kind of ultra high purity gas analysis chromatography processes flow process of accomplishing all impurity compositions analyses in ultra-pure gas through the sub-sampling switching gas circuit is provided.
In order to solve the problems of the technologies described above, the present invention is able to solve through following technical proposals:
The gas-chromatography detection system that trace impurity is analyzed in ultra-pure gas; Comprise and carry 1, carry 2, carry 3, carry 4 gas circuits; Transfer valve V I and transfer valve V II, transfer valve V III and transfer valve V IV are provided with the first molecular sieve chromatography post between transfer valve V I and the transfer valve V II; Be provided with the second molecular sieve chromatography post between transfer valve V II and the transfer valve V IV; Be provided with needle-valve between transfer valve V I and the transfer valve V III, be provided with the second pillar separation vessel between transfer valve V III and the transfer valve V IV.
As preferably, carry that 1 gas circuit is connected with the 4. number interface of transfer valve V I, year 2 gas circuits are connected with the 7. number interface of transfer valve V I; Sample inlet is connected with the 1. number interface of transfer valve V I, and sample export is connected with the 2. number interface of transfer valve V I, and the 10. number interface of transfer valve V I is connected through pipeline with 3. number interface, also is provided with quantity tube on this pipeline; Carry 1 gas circuit and be connected with the 4. number interface of transfer valve V I, the pipeline that the 5. number interface of transfer valve V I is connected with 9. number interface is provided with the first pillar separation vessel; The upper end of needle-valve is connected with the 8. number interface of transfer valve V I, and the lower end is connected with the 1. number interface of transfer valve V III; Carrying 2 gas circuits is connected with the 7. number interface of transfer valve V I; One end of the first molecular sieve chromatography post is connected with the 6. number interface of transfer valve V I, and the other end is connected with the 1. number interface of transfer valve V II.
As preferably, carry 3 gas circuits and be connected with the 3. number interface of transfer valve V II; One end of the second molecular sieve chromatography post is connected with the 2. number interface of transfer valve V II, and the other end is connected with the 3. number interface of transfer valve V IV; 4. number interface of transfer valve V II is connected through pipeline with 5. number interface, and No. six interfaces of transfer valve V II are connected with variable valve A.
As preferably, carry 4 gas circuits and be connected with the 3. number interface of transfer valve V III; 4. number interface of transfer valve V III is connected through pipeline with 5. number interface, and the 6. number interface of transfer valve V III is connected with variable valve B; One end of the second pillar separation vessel is connected with the 2. number interface of transfer valve V III, and the other end is connected with the 1. number interface of transfer valve V IV.
As preferably, the 2. number interface of transfer valve V IV is connected with the helium ion detector, and the 4. number interface of transfer valve V IV is connected through pipeline with 5. number interface, and the 6. number interface of transfer valve V IV is connected with variable valve C.
As preferably, transfer valve V I is ten logically to purge pneumatic transfer valves, and transfer valve V II, V III, V IV are six logically to purge pneumatic transfer valves, carries 1, carries 2, carries 3, carries on 4 gas circuits and be respectively equipped with damper tube.Adopt the Valco band to purge pneumatic transfer valve; Guarantee the counter-infiltration of gas circuit handoff procedure air; Adopt Valco six direction changeover valves, four-way valve makes that the gas circuit stroke in the valve body is the shortest relatively; Adopting 316LValco 1/16 " 0.13mm makes the damping pipeline, the good and stability of flow of impermeability; The 5A chromatogram pillar that the research and development of employing company are produced, technological innovation and product quality not only ensure but also reliable; Adopt two heartcut systems, purpose emptying main component guarantees that as much as possible baseline is steady; Adopt ten-way valve just blowing mode, characteristics are that the gas circuit flow of native system changes little after valve body switches; Adopt the stainless steel metering pin valve, not only may command emptying flow but also can suppress the reverse osmosis of air; Adopt outside detached column case, make different chromatogram pillars have independent temperature controlling function.
The gas-chromatography detection method that trace impurity is analyzed in ultra-pure gas, the sample introduction of employing sample gas secondary, main component is opened H2, O2 in the preparatory cutting of sample introduction for the first time of ten direction changeover valve V I; Ar, N2, CH4; The component of CO and sample introduction blowback second time CO2, C2+, H2O component; Separate the back again and switch the analysis of entering helium ion detector, concrete steps are following:
A, transfer valve V I adopt the forward sample introduction and the mode of blowback to change the gas circuit flow direction and link pipeline; Utilize the first pillar separation vessel to carrying component in the 1 gas circuit main body gas separately and behind the transfer valve: gas circuit changes stream goes other component blowbacks to separate to the first molecular sieve chromatography post, oppositely purges out residual air body composition and flow into the second pillar separation vessel by carrying 2 gas circuits;
B, transfer valve V II are made first heartcut to main component, the most main peak of emptying, and successively the impurity component is put into the second molecular sieve chromatography post and goes to separate; And control well repeatedly switching time of valve the impurity component to be dropped to and go out the peak on the baseline, to improve its detection sensitivity;
C, transfer valve V III mainly also are that the component that blowback is come is carried out all the other main peaks of secondary excision as the second cutting center, and the component that emptying is not wanted like trace water or sulfide, mainly obtains C02 or C2+ to separate on the second pillar separation vessel;
D, transfer valve V IV switch to the impurity component that separates on the second molecular sieve chromatography post and the second pillar separation vessel respectively and go to respond out the peak in the helium ion detector.
As preferably, sample introduction comprises the steps: for the first time
A, switch V I ten-way valve and carry high purity nitrogen sample gas in the 1 gas circuit series connection quantity tube and enter into the first pillar separation vessel and cut the pillar pre-separation in advance and go out H2, O2/Ar, contain N2 main body peak, CH4, CO and be put into the first molecular sieve chromatography post to go;
B, V I switching gas circuit then carry 1 gas circuit and enter into oppositely that the first pillar separation vessel blows out remaining nitrogen and the remaining component of the CO2/C2+ that comprises; At this moment carry 2 gas circuits and enter into H2, the O2/Ar that the first molecular sieve chromatography post removes to isolate earlier nitrogen; Put into and go in the second molecular sieve chromatography post (52) to continue to separate; In the time of just will having gone out the first molecular sieve chromatography post Deng N2, then switch V II valve emptying N2 peak, when waiting CH4 that is diffused among the N2 will go out the first molecular sieve chromatography post; Then switch V II valve, put into CH4 and get into the second molecular sieve chromatography post and go to separate;
C, likewise continue the surplus N2 of transfer valve emptying, then switch V II valve when waiting CO that is diffused among the N2 will go out the first molecular sieve chromatography post, put into CO and get into the second molecular sieve chromatography post and go to separate;
D, adjust to well under the emptying N2 time each time and can the CH4, the CO that analyzed among the N2 be gone out the peak by the helium diluted of carrying in 3 to baseline;
E, the isolated H2 of the second molecular sieve chromatography post pillar, O2/Ar, CH4, CO component are got in the helium ion detector by the switching of V IV valve and respond; In this process the first pillar separation vessel blow out remaining nitrogen and comprise in the remaining component of CO2/C2+ all switch emptying and fall by V II valve.
As preferably; Sample introduction switches ten direction changeover valve V I once more by the external event clock control for the second time; Carry high purity nitrogen sample gas in the 1 gas circuit series connection quantity tube and enter into the first pillar separation vessel and cut the pillar pre-separation in advance and go out H2, O2/Ar, contain N2 main body peak, CH4, CO and be put into the one the first molecular sieve chromatography column molecular sieve chromatographic columns to go, and switch whole emptying by transfer valve V II and fall; Control transfer valve V I switching gas circuit then, carry 1 gas circuit and enter into oppositely that the first pillar separation vessel blows out remaining nitrogen and the remaining component of the CO2/C2+ that comprises; Blow out remaining nitrogen by the emptying of transfer valve V III; Switching transfer valve V III (3) is put into and is removed separation of C O2 or C2+ component in the second pillar separation vessel pillar when isolating the first pillar separation vessel (61) Deng CO2, and at this moment transfer valve V IV performs in advance to switch in CO2 or the C2+ entering helium ion detector and responds.
As preferably, needle-valve can be used to regulate and carries 1 with to carry 2 flow velocity balances consistent in the transfer valve V I valve in the gas circuit after the sub-sampling blowback, and make transfer valve V IV switch laggard in the helium ion detector flow identical, its base flow variation is not quite.
The present invention is switched through just blowing with blowback of ten direction changeover valves and six direction changeover valves; The change action of heartcut is all accomplished by system's countercharge chromatographic work station; The corresponding external event of each valve is controlled, and the order of its action also by incident executions that program, control by holistic approach process automation like this; Action is fast consistent reliable, the data repeatability of system and accuracy by the stable flow rate gas circuit and accurately valve switch and guarantee.
Description of drawings
Fig. 1 is gas-chromatography detection system of the present invention and method flow synoptic diagram.
Fig. 2 waits until the first pillar separation vessel synoptic diagram for the ten-way valve sampling with blowback CO2, C2+, H2O.
Fig. 3 is for the ten-way valve sample introduction and cut H2, N2, CH4 to the first molecular sieve chromatography post synoptic diagram in advance.
Fig. 4 enters into the second molecular sieve chromatography post synoptic diagram for the transfer valve V II first cutting center emptying first molecular sieve chromatography post main peak and purging peak to be detected.
Fig. 5 puts into peak to be detected in the second molecular sieve chromatography post for the transfer valve V II first cutting center and removes to separate synoptic diagram.
Fig. 6 is surplus main peak and H2O in the transfer valve V III second cutting center emptying first pillar separation vessel, C2+ etc.
Fig. 7 cuts CO2 for the transfer valve V III second cutting center or C2+ separates in the second pillar separation vessel.
Fig. 8 enters into the helium ion detector for H2, O2, N2, CH4, CO in the transfer valve V IV switch.
Fig. 9 enters into the helium ion detector for CO2 in the transfer valve V IV or C2+ switch.
Wherein 1-transfer valve V I, 2-transfer valve V II, 3-transfer valve V III, 4-transfer valve V IV, 8-helium ion detector, 9-needle-valve, 11-damper tube, 21-damper tube, 31-damper tube, 41-damper tube, 51-the first molecular sieve chromatography post, 52-the second molecular sieve chromatography post, 61-the first pillar separation vessel, 62-the second pillar separation vessel, 71-variable valve A, 72-variable valve B, 73-variable valve C.
Embodiment
Below in conjunction with accompanying drawing 1 to accompanying drawing 9 and embodiment the present invention is described in further detail:
Embodiment 1
The gas-chromatography detection system that trace impurity is analyzed in ultra-pure gas; Comprise and carry 1, carry 2, carry 3, carry 4 gas circuits; Transfer valve V I 1 and transfer valve V II 2, transfer valve V III 3 and transfer valve V IV 4, ten logical purgings between pneumatic transfer valve V I 1 and the pneumatic transfer valve V II 2 of six logical purgings are provided with the first molecular sieve chromatography post 51; Be provided with the second molecular sieve chromatography post 52 between transfer valve V II 2 and the transfer valve V IV 4; Be provided with needle-valve 9 between transfer valve V I 1 and the transfer valve V III 3, be provided with the second pillar separation vessel 62 between transfer valve V III 3 and the transfer valve V IV 4.The computer tube line length was come constant flow practice control after carrier gas 1, carrier gas 2, carrier gas 3, carrier gas 4 were all done damping with microporous pipe, and this mode gas circuit stability of flow is accurate; Can measure the subtle change of 2-3ml/min flow through the adjustment of every 5-10cm length.See accompanying drawing 1 for details.
Carry that 1 gas circuit is connected with the 4. number interface of transfer valve V I 1, year 2 gas circuits are connected with the 7. number interface of transfer valve V I 1; Sample inlet is connected with the 1. number interface of transfer valve V I 1, and sample export is connected with the 2. number interface of transfer valve V I 1, and the 10. number interface of transfer valve V I 1 is connected through pipeline with 3. number interface, also is provided with quantity tube 12 on this pipeline; Carry 1 gas circuit and be connected with the 4. number interface of transfer valve V I 1, the pipeline that the 5. number interface of transfer valve V I 1 is connected with 9. number interface is provided with the first pillar separation vessel 61; The upper end of needle-valve 9 is connected with the 8. number interface of transfer valve V I 1, and the lower end is connected with the 1. number interface of transfer valve V III 4; Carrying 2 gas circuits is connected with the 7. number interface of transfer valve V I 1; One end of the first molecular sieve chromatography post 51 is connected with the 6. number interface of transfer valve V I 1, and the other end is connected with the 1. number interface of transfer valve V II 2.
Carrying 3 gas circuits is connected with the 3. number interface of transfer valve V II 2; One end of the second molecular sieve chromatography post 52 is connected with the 2. number interface of transfer valve V II 2, and the other end is connected with the 3. number interface of transfer valve V IV 4; 4. number interface of transfer valve V II 2 is connected through pipeline with 5. number interface, and No. six interfaces of transfer valve V II 2 are connected with variable valve A71.
Carrying 4 gas circuits is connected with the 3. number interface of transfer valve V III 3; 4. number interface of transfer valve V III 3 is connected through pipeline with 5. number interface, and the 6. number interface of transfer valve V III 3 is connected with variable valve B72; One end of the second pillar separation vessel 62 is connected with the 2. number interface of transfer valve V III 3, and the other end is connected with the 1. number interface of transfer valve V IV 4.
2. number interface of transfer valve V IV 4 is connected with helium ion detector 8, and the 4. number interface of transfer valve V IV 4 is connected through pipeline with 5. number interface, and the 6. number interface of transfer valve V IV 4 is connected with variable valve C73.
Transfer valve V I 1 is ten logical to purge pneumatic transfer valves, and transfer valve V II, V III, V IV 2,3,4 are six logically to purge pneumatic transfer valves, carries 1, carries 2, carries 3, carries on 4 gas circuits and be respectively equipped with damper tube 11,21,31,41.Stainless steel metering pin valve 9 is adopted in each gas circuit emptying and control among the present invention, and the airshed size can regulated and control out to characteristics one effectively; Characteristics two can make gas circuit form forward towards external pressure, guarantee that air can't reverse osmosis.Gas circuit web member, pipeline and joint etc. all adopt the Valco standard component of VICI company; To guarantee ultra high purity gas analysis gas-path leakage ratings＜1*10-8atm cc/sec.
Trace impurity is analyzed in ultra-pure gas gas-chromatography detection system and method, the sample introduction of employing sample gas secondary, main component is opened H2, O2 in the ten direction changeover valve V I 1 preparatory cuttings of sample introduction for the first time; Ar, N2, CH4; The component of CO and sample introduction blowback second time CO2, C2+, H2O component; Separate the back again and switch 8 analyses of entering helium ion detector, concrete steps are following:
A, transfer valve V I 1 adopt the forward sample introduction and the mode of blowback to change the gas circuit flow direction and link pipeline; Utilize 61 pairs of the first pillar separation vessels to carry component in the 1 gas circuit main body gas separately and behind the transfer valve: gas circuit changes stream goes other component blowbacks to separate to the first molecular sieve chromatography post 51, oppositely purges out residual air body composition and flow into the second pillar separation vessel 62 by carrying 2 gas circuits;
Transfer valve V I 1 adopts the forward sample introduction and the gas circuit that changes of blowback mode to flow to and link pipeline; Main component is by carrying behind the 1 gas circuit forward sample introduction at the first pillar separation vessel, 61 pre-separation H2, O2/Ar, N2; CH4, the component of CO put into the first molecular sieve chromatography post 51 and separate; Then, oppositely purge out residual air body composition by year 2 gas circuits and flow into the second pillar separation vessel, 62 separation of C O2 components, like Fig. 2, shown in 3.
B, 2 pairs of main components of transfer valve V II are made first heartcut, the most main peak of emptying, and successively the impurity component is put into the second molecular sieve chromatography post 52 and goes to separate; And control well repeatedly switching time of valve the impurity component to be dropped to and go out the peak on the baseline, to improve its detection sensitivity;
Transfer valve V II 2 is as the first cutting center; The 5A molecular sieve chromatography pillar of respectively connecting before and after the valve is the first molecular sieve chromatography post 51 and the second molecular sieve chromatography post 52; The first molecular sieve chromatography post 51 is used for the most of main body of pre-separation and emptying peak; Remaining a small amount of main body peak the impurity peaks that comprises by emptying several times relatively with put into the second molecular sieve chromatography post 52 and come the removing impurities peak, the impurity peaks of analysis is got back on the horizontal base line, improve the detection sensitivity of impurity peaks.Like accompanying drawing 4, shown in 5.
C, transfer valve V III 3 mainly also are that the component that blowback is come is carried out surplus its main peak of secondary excision as the second cutting center, and the component that emptying is not wanted like trace water or sulfide, mainly obtains CO2 or C2+ to separate on the second pillar separation vessel 62;
Adopted V III six-way valve as the second cutting center, characteristics are accurate stainless steel metering pin valves that damping is used of series connection before the valve, are equal to the resistance of chromatographic column, and one second pillar separation vessel 62 special uses of series connection come separation of C O2 behind the V III valve, also can be used to separation of C 2+; The valve action of V III be emptying do not want be spread in the first pillar separation vessel 61 and surplus main body and component such as trace water or sulfide etc. that blowback goes out.See accompanying drawing 6,7 valves for details and switch synoptic diagram.
D, transfer valve V IV 4 switch to the impurity component that separates on the second molecular sieve chromatography post 52 and the second pillar separation vessel 62 respectively and go to respond out the peak in the helium ion detector.
Adopted V IV six-way valve to switch the isolated H2 of the first molecular sieve chromatography post, 51 pillars; O2/Ar, N2, CH4; CO component and the isolated CO2 of the second pillar separation vessel, 62 pillars or C2+ component get into 8 responses of helium ion detector, thereby measure the signal value of each impurity composition.See accompanying drawing 8,9 valves for details and switch synoptic diagram.Described ten logical all adopt the modular, pneumatically powered valve of the blowing and sweeping type Valco of VICI company with six direction changeover valves; Its principal character is the sweep gas protection gas circuit of design positive-pressure type in cavity; Guarantee that the air that the valve body rotor gap that mechanical seal causes when switching gas circuit has can't diffuse into by reverse osmosis, the malleation of protection gas is cut from carrier gas and the possible contact of air fully; Guarantee that the switching in valve body hole and hole just carries out between carrier gas.
Sample introduction comprises the steps: for the first time
A, switch V I ten-way valve and carry high purity nitrogen sample gas in the 1 gas circuit series connection quantity tube 12 and enter into the first pillar separation vessel 61 and cut the pillar pre-separation in advance and go out H2, O2/Ar, contain N2 main body peak, CH4, CO and be put into the first molecular sieve chromatography post 51 to go; As shown in Figure 3.
B, V I switching gas circuit then carry 1 gas circuit and enter into oppositely that the first pillar separation vessel 61 blows out remaining nitrogen and the remaining component of the CO2/C2+ that comprises; At this moment carry 2 gas circuits and enter into H2, the O2/Ar that the first molecular sieve chromatography post 51 removes to isolate earlier nitrogen; Put into and go in the second molecular sieve chromatography post 52 to continue to separate; In the time of just will having gone out the first molecular sieve chromatography post 51 Deng N2, then switch V II valve emptying N2 peak, when waiting CH4 that is diffused among the N2 will go out the first molecular sieve chromatography post 51; Then switch V II valve, put into CH4 and get into the second molecular sieve chromatography post 52 and go to separate;
C, likewise continue the surplus N2 of transfer valve emptying, then switch V II valve when waiting CO that is diffused among the N2 will go out the first molecular sieve chromatography post 51, put into CO and get into the second molecular sieve chromatography post 52 and go to separate;
D, adjust to well under the emptying N2 time each time and can the CH4, the CO that analyzed among the N2 be gone out the peak by the helium diluted of carrying in 3 to baseline;
E, the isolated H2 of the second molecular sieve chromatography post, 52 pillars, O2/Ar, CH4, CO component are switched response in the entering helium ion detector 8 by V IV valve; In this process the first pillar separation vessel 61 blow out remaining nitrogen and comprise in the remaining component of CO2/C2+ all switch emptying and fall by V II valve.
Sample introduction switches ten direction changeover valve V I 1 once more by the external event clock control for the second time; Carry high purity nitrogen sample gas in the 1 gas circuit series connection quantity tube 12 and enter into the first pillar separation vessel 61 and cut the pillar pre-separation in advance and go out H2, O2/Ar, contain N2 main body peak, CH4, CO and be put into the one the first molecular sieve chromatography post 51 molecular sieve chromatography posts 51 to go, and switch whole emptying by transfer valve V II 2 and fall; Control transfer valve V I 1 switching gas circuit then, carry 1 gas circuit and enter into oppositely that the first pillar separation vessel 61 blows out remaining nitrogen and the remaining component of the CO2/C2+ that comprises; Blow out remaining nitrogen by 3 emptying of transfer valve V III; Switching transfer valve V III 3 is put in the second pillar separation vessel, 62 pillars and is removed separation of C O2 or C2+ component when isolating the first pillar separation vessel 61 Deng CO2, and at this moment transfer valve V IV 4 performs in advance and switches response in CO2 or the C2+ entering helium ion detector 8.
Needle-valve 9 can be used to regulate and carries 1 with to carry 2 flow velocity balances consistent in transfer valve V I 1 valve in the gas circuit after the sub-sampling blowback, and make transfer valve V IV 4 switch laggard in the helium ion detector flow identical, its base flow variation is not quite.
Below we through this method is implemented in the impurity proximate analysis of ultra-pure nitrogen (99.9999%), reach the purpose that ultra-pure nitrogen is detected; Its implementation process is following: instrument sampling is for the first time automatically switched V I ten-way valve and is carried high purity nitrogen sample gas in the 1 gas circuit series connection 1ml quantity tube and enter into the first pillar separation vessel 61 and cut the pillar pre-separation in advance and go out H2, O2/Ar, contain N2 main body peak, CH4, CO and be put into first first molecular sieve chromatography post 51 to go; V I switching gas circuit carries 1 gas circuit and enters into oppositely that the first pillar separation vessel 61 blows out remaining nitrogen and the remaining component of the CO2/C2+ that comprises then, and C2+ is mainly alkane and alkene; At this moment carry 2 gas circuits and enter into H2, the O2/Ar that the first molecular sieve chromatography post 51 removes to isolate earlier nitrogen; Put into and go in second the second molecular sieve chromatography post 52 to continue to separate; Just to go out 51 switchings of first molecular sieve chromatography post V II valve emptying N2 peak Deng N2; Then switch V II valve when CH4 among the N2 will go out the first molecular sieve chromatography post 51 Deng being diffused in, put into CH4 and get into the second molecular sieve chromatography post 52 and go to separate; Likewise continue the surplus N2 of transfer valve emptying, then switch V II valve when waiting CO that is diffused among the N2 will go out the first molecular sieve chromatography post 51, put into CO and get into the second molecular sieve chromatography post 52 and go to separate; Adjust to well under the emptying N2 time each time and can the CH4, the CO that analyzed among the N2 be gone out the peak by the helium diluted of carrying in 3 to baseline; The isolated H2 of the second molecular sieve chromatography post, 52 pillars, O2/Ar, CH4, CO component are got in the PDHID helium ion detector by the switching of V IV valve and respond; In this process the first pillar separation vessel 61 blow out remaining nitrogen and comprise in the remaining component of CO2/C2+ all switch emptying and fall by V II valve.
In a word, the above is merely preferred embodiment of the present invention, and all equalizations of doing according to claim of the present invention change and modify, and all should belong to the covering scope of patent of the present invention.
Claims (10)
1. the gas-chromatography detection system that trace impurity is analyzed in ultra-pure gas; Comprise and carry 1, carry 2, carry 3, carry 4 gas circuits; Transfer valve V I (1) and transfer valve V II (2), transfer valve V III (3) and transfer valve V IV (4) is characterized in that: be provided with the first molecular sieve chromatography post (51) between transfer valve V I (1) and the transfer valve V II (2); Be provided with the second molecular sieve chromatography post (52) between transfer valve V II (2) and the transfer valve V IV (4); Be provided with needle-valve (9) between transfer valve V I (1) and the transfer valve V III (3), be provided with the second pillar separation vessel (62) between transfer valve V III (3) and the transfer valve V IV (4).
2. the gas-chromatography detection system that trace impurity is analyzed in ultra-pure gas according to claim 1 is characterized in that: year 1 gas circuit is connected, carries 2 gas circuits and is connected with the 7. number interface of transfer valve V I (1) with the 4. number interface of transfer valve V I (1); Sample inlet is connected with the 1. number interface of transfer valve V I (1), and sample export is connected with the 2. number interface of transfer valve V I (1), and the 10. number interface of transfer valve V I (1) is connected through pipeline with 3. number interface, also is provided with quantity tube (12) on this pipeline; Carry 1 gas circuit and be connected with the 4. number interface of transfer valve V I (1), the pipeline that the 5. number interface of transfer valve V I (1) is connected with 9. number interface is provided with the first pillar separation vessel (61); The upper end of needle-valve (9) is connected with the 8. number interface of transfer valve V I (1), and the lower end is connected with the 1. number interface of transfer valve V III (4); Carrying 2 gas circuits is connected with the 7. number interface of transfer valve V I (1); One end of the first molecular sieve chromatography post (51) is connected with the 6. number interface of transfer valve V I (1), and the other end is connected with the 1. number interface of transfer valve V II (2).
3. the gas-chromatography detection system that trace impurity is analyzed in ultra-pure gas according to claim 1 is characterized in that: carry 3 gas circuits and be connected with the 3. number interface of transfer valve V II (2); One end of the second molecular sieve chromatography post (52) is connected with the 2. number interface of transfer valve V II (2), and the other end is connected with the 3. number interface of transfer valve V IV (4); 4. number interface of transfer valve V II (2) is connected through pipeline with 5. number interface, and No. six interfaces of transfer valve V II (2) are connected with variable valve A (71).
4. the gas-chromatography detection system that trace impurity is analyzed in ultra-pure gas according to claim 1 is characterized in that: carry 4 gas circuits and be connected with the 3. number interface of transfer valve V III (3); 4. number interface of transfer valve V III (3) is connected through pipeline with 5. number interface, and the 6. number interface of transfer valve V III (3) is connected with variable valve B (72); One end of the second pillar separation vessel (62) is connected with the 2. number interface of transfer valve V III (3), and the other end is connected with the 1. number interface of transfer valve V IV (4).
5. the gas-chromatography detection system that trace impurity is analyzed in ultra-pure gas according to claim 1; It is characterized in that: the 2. number interface of transfer valve V IV (4) is connected with helium ion detector (8); 4. number interface of transfer valve V IV (4) is connected through pipeline with 5. number interface, and the 6. number interface of transfer valve V IV (4) is connected with variable valve C (73).
6. the gas-chromatography detection system that trace impurity is analyzed in ultra-pure gas according to claim 1; It is characterized in that: described transfer valve V I (1) is the pneumatic transfer valves of ten logical purgings; Transfer valve V II, V III, V IV (2,3,4) are six logical to purge pneumatic transfer valves, carry 1, carry 2, carry 3, carry on 4 gas circuits and be respectively equipped with damper tube (11,21,31,41).
7. the gas-chromatography detection method that trace impurity is analyzed in ultra-pure gas is characterized in that, adopts the sample introduction of sample gas secondary; Main component is opened H2, O2, Ar in the preparatory cutting of sample introduction for the first time of ten direction changeover valve V I (1); N2, CH4, the component of CO and sample introduction blowback second time CO2; C2+, the H2O component; Separate the back again and switch entering helium ion detector (8) analysis, concrete steps are following:
A, transfer valve V I (1) adopt the forward sample introduction and the mode of blowback to change the gas circuit flow direction and link pipeline; Utilize the first pillar separation vessel (61) to carrying component in the 1 gas circuit main body gas separately and behind the transfer valve: gas circuit changes stream goes other component blowbacks to separate to the first molecular sieve chromatography post (51), oppositely purges out residual air body composition and flow into the second pillar separation vessel (62) by carrying 2 gas circuits;
B, transfer valve V II (2) are made first heartcut to main component, the most main peak of emptying, and successively the impurity component is put into the second molecular sieve chromatography post (52) and goes to separate; And control well repeatedly switching time of valve the impurity component to be dropped to and go out the peak on the baseline, to improve its detection sensitivity;
C, transfer valve V III (3) are as the second cutting center; Main also is that the component that blowback is come is carried out all the other main peaks of secondary excision; The component that emptying is not wanted like trace water or sulfide, mainly obtains C02 or C2+ to separate on the second pillar separation vessel (62);
D, transfer valve V IV (4) switch to the impurity component that separates on the second molecular sieve chromatography post (52) and the second pillar separation vessel (62) respectively and go to respond out the peak in the helium ion detector.
8. the gas-chromatography detection method that trace impurity is analyzed in ultra-pure gas according to claim 7 is characterized in that, sample introduction comprises the steps: for the first time
A, switch V I ten-way valve and carry high purity nitrogen sample gas in the 1 gas circuit series connection quantity tube (12) and enter into the first pillar separation vessel (61) and cut the pillar pre-separation in advance and go out H2, O2/Ar, contain N2 main body peak, CH4, CO and be put into the first molecular sieve chromatography post (51) to go;
B, V I switching gas circuit then carry 1 gas circuit and enter into oppositely that the first pillar separation vessel (61) blows out remaining nitrogen and the remaining component of the CO2/C2+ that comprises; At this moment carry 2 gas circuits and enter into H2, the O2/Ar that the first molecular sieve chromatography post (51) removes to isolate earlier nitrogen; Put into and go in the second molecular sieve chromatography post (52) to continue to separate; In the time of just will having gone out the first molecular sieve chromatography post (51) Deng N2, then switch V II valve emptying N2 peak, when waiting CH4 that is diffused among the N2 will go out the first molecular sieve chromatography post (51); Then switch V II valve, put into CH4 and get into the second molecular sieve chromatography post (52) and go to separate;
C, likewise continue the surplus N2 of transfer valve emptying, then switch V II valve when waiting CO that is diffused among the N2 will go out the first molecular sieve chromatography post (51), put into CO and get into the second molecular sieve chromatography post (52) and go to separate;
D, adjust to well under the emptying N2 time each time and can the CH4, the CO that analyzed among the N2 be gone out the peak by the helium diluted of carrying in 3 to baseline;
E, the isolated H2 of second molecular sieve chromatography post (52) pillar, O2/Ar, CH4, CO component are switched response in the entering helium ion detector (8) by V IV valve; In this process the first pillar separation vessel (61) blow out remaining nitrogen and comprise in the remaining component of CO2/C2+ all switch emptying and fall by V II valve.
9. the gas-chromatography detection method that trace impurity is analyzed in ultra-pure gas according to claim 7; It is characterized in that: sample introduction switches ten direction changeover valve V I (1) once more by the external event clock control for the second time; Carry high purity nitrogen sample gas in the 1 gas circuit series connection quantity tube (12) and enter into the first pillar separation vessel (61) and cut the pillar pre-separation in advance and go out H2, O2/Ar, contain N2 main body peak, CH4, CO and be put into a 5A1 molecular sieve chromatography post (51) to go, and switch whole emptying by transfer valve V II (2) and fall; Control transfer valve V I (1) switching gas circuit then, carry 1 gas circuit and enter into oppositely that the first pillar separation vessel (61) blows out remaining nitrogen and the remaining component of the CO2/C2+ that comprises; Blow out remaining nitrogen by transfer valve V III (3) emptying; Switching transfer valve V III (3) is put in second pillar separation vessel (62) pillar and is removed separation of C O2 or C2+ component when isolating the first pillar separation vessel (61) Deng CO2, and at this moment transfer valve V IV (4) performs in advance and switches response in CO2 or the C2+ entering helium ion detector (8).
10. the gas-chromatography detection method that trace impurity is analyzed in ultra-pure gas according to claim 7; It is characterized in that: needle-valve in the gas circuit after the sub-sampling blowback (9) can be used to regulate in transfer valve V I (1) valve carry 1 consistent with year 2 flow velocity balances; And make transfer valve V IV (4) switch laggard in the helium ion detector flow identical, its base flow changes little.
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