CN1139807C - Chromatic spectrum sample feeder - Google Patents
Chromatic spectrum sample feeder Download PDFInfo
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- CN1139807C CN1139807C CNB001274422A CN00127442A CN1139807C CN 1139807 C CN1139807 C CN 1139807C CN B001274422 A CNB001274422 A CN B001274422A CN 00127442 A CN00127442 A CN 00127442A CN 1139807 C CN1139807 C CN 1139807C
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- carrier gas
- vaporizer
- sample
- shunting
- preheating chamber
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Abstract
The present invention relates to a chromatogram sample injector mainly solving the problems that in the prior art, samples and supporting gas can not be fully mixed causing the distortion of analytical data distortion; otherwise, samples and supporting gas are ensured that samples and supporting gas are fully mixed, and simultaneously, the service life of chromatographic columns and the stability of analysis signals are influenced. The present invention perfectly solves the problems by a technical scheme that supporting gas enters preheating chambers for preheating before entering vaporizing chambers for ensuring the uniform temperature distribution of the vaporizing chambers with sufficient heat capacity; gas control valves and by-pass channels are additionally arranged between guide pipes of the vaporizing chambers and chromatographic columns. The chromatogram sample injector can be applied to the industrial production of chromatographic analysis devices.
Description
The present invention relates to chromatic spectrum sample feeder, especially relate to shunting or be regardless of the flow chromatography injector.
Along with the increasingly extensive use of capillary column, follow the problem that runs in the capillary column use also to become increasingly conspicuous.As everyone knows and since kapillary itself intrinsic characteristic, little as volumetric flow rate, sample capacity is little etc., makes split sampling become the method for main employing at present.But split sampling regular meeting bring sample " distortion ", and then cause quantitative precision poor, influence the correct judgement of data.Therefore develop a kind of " linearity " split sampling system, be not only the target that lot of domestic and foreign chromatographic apparatus producer is pursued, also vast chromatogram user presses for.
All there are in various degree distortion phenomenon in domestic and international existing shunting at present or split stream injector, not for the analysis of wide boiling range sample.Existing split stream injector, causes the main cause of sample " distortion " to be: wide boiling range sample fails fully to be mixed after entering vaporizer, just pass through split stream injector,, make and do not have a sample of adequate representation and enter chromatographic column, cause errors of analytical results bigger, particularly serious for wide boiling range sample.
Introduced a kind of multi-usage gas chromatography or look-mass spectrum injector among the document CN2080673U.This injector comprises heating arrangement, temperature sensing device, temperature control equipment, sample introduction mechanism, heating vaporizer, carrier gas conduit and wireway, between wireway and vaporizer, set up a valve in addition, valve is positioned at vaporizer, by this valve the time of sample dissociation in the vaporizer or evaporation process is controlled.In the document,, when carrier gas contacts with sample introduction sample, be difficult to make sample to reach rapid vaporization, thereby can make analysis result cause distortion because carrier gas directly enters vaporizer.In the document, though set up a valve in vaporizer, work as valve closing in addition, when guaranteeing that vaporizer sample and carrier are fully mixed, can cause in the external chromatographic column does not have flow, thereby can influence the life-span of chromatographic column and the stability of analytic signal.
The objective of the invention is to exist sample and the carrier gas can not be fully mixed in the document in order to overcome in the past, cause and analyze data distortion or when guaranteeing that sample and carrier gas fully mix, can influence the life-span of chromatographic column and the shortcoming of analytic signal stability, a kind of new chromatic spectrum sample feeder is provided.This injector has when guaranteeing that carrier gas and sample are fully mixed rapidly, can not influence the characteristics of chromatographic column operate as normal.
The objective of the invention is to realize: a kind of chromatic spectrum sample feeder by following technical scheme, comprise sample introduction mechanism, carrier gas inlet, well heater, carrier gas preheating chamber, shunting derivation passage and vaporizer, wherein sample introduction mechanism is on the top of vaporizer, the outside that passage is positioned at vaporizer is derived in shunting, the inside of carrier gas preheating chamber, carrier gas preheating chamber outside is a well heater; The bottom that passage is derived in shunting communicates with vaporizer, is closed state with the carrier gas preheating chamber, and the top seal of passage is derived in shunting; Shunting is derived the inter-agency space of channel roof and sample introduction and is communicated with carrier gas preheating chamber and vaporizer respectively; The bottom of vaporizer links to each other with extraneous chromatogram by conduit, and carrier gas inlet communicates with carrier gas preheating chamber bottom, is connected with the gas transfer valve between vaporizer and extraneous chromatogram, has extraneous bypass channel to link to each other in addition between carrier gas inlet and the gas transfer valve.
In the technique scheme, the preferred version of gas transfer valve is three-way switch valve or four-way switching valve.
Among the present invention, owing to set up the carrier gas preheating chamber, and allow carrier gas enter from carrier gas preheating chamber bottom, make fully preheating of carrier gas, sample moment is fully vaporized, thereby reach carrier gas and sample can fully mix evenly, can guarantee that vaporizer has that even temperature distributes simultaneously, enough thermal capacity and ensure that sample and carrier gas have enough vaporization incorporation times, and can avoid sample to produce antidiffusion, cause the problem of the inhomogeneous loss of short circuit.Between vaporizer and extraneous chromatogram, be connected the gas transfer valve in addition, the scheme that has extraneous bypass channel to link to each other in addition between carrier gas inlet and the gas transfer valve, when the gas transfer valve switches to extraneous bypass channel when linking to each other with extraneous chromatogram with vaporizer and extraneous chromatogram pipeline, avoided not having in the external chromatographic column problem of flow, thereby can guarantee the operate as normal of external chromatogram, reach the purpose that does not influence chromatographic column life-span and analytic signal stability, obtained better technical effect.
Accompanying drawing 1 is a vertical structure diagrammatic cross-section of the present invention.
1 is sample introduction mechanism in the accompanying drawing 1, and 2 is vaporizer, and 3 are the carrier gas preheating chamber, 4 is well heater, and 5 are shunting derivation passage, and 6 is the gas transfer valve, 7 is chromatographic column, 8 is bypass channel, and 9 is the diverting switch valve, and 10 is the dottle pin blow down valve, 11 is valve control, 12 is temperature controller, and 13 is carrier gas inlet, and 14 is conduit.
The technology of the present invention workflow be: carrier gas passes into carrier gas inlet 13 and enters carrier gas preheating chamber 3, under the heating of heater 4, carrier gas is by flowing from bottom to top, gradually by abundant preheating, then enter vaporizer 2, avoided vaporizer 2 epimeres to have temperature " cold-zone ", like this when hot carrier gas when sample introduction sample in the sample introduction mechanism 1 contacts, sample introduction sample moment is fully vaporized, then guarantee the fully mixed of carrier gas and sample introduction sample. Shunting is set in addition derives passage 5, the shunting gas of heat is flowed from bottom to top, further strengthened the uniform temperature distribution of vaporizer 2 and for vaporizer 2 provides enough thermal capacity, avoided vaporizer 2 to have thermograde. The temperature of heater 4 is accurately controlled by temperature controller 12.
Set up gas transfer valve 6 (being generally three-way switch valve or four-way switching valve) between vaporizer 2 and chromatographic column 7, diverting switch valve 9 is set up in the shunting outlet. Shunting switch valve 9 cuts out during sample introduction, and depot siding was through shunting outlet emptying before unnecessary carrier gas " short circuit " was directly purged by dottle pin by vaporizer 2 tops. Simultaneously four-way or threeway gas transfer valve 6 start, and chromatographic column 7 contains cyclostrophic and turns to bypass channel 8 and provide. At this moment, vaporizer 2 becomes vaporization hybird environment static, that do not have carrier gas to flow. The switching time of four-way or threeway gas transfer valve 6, diverting switch valve 9 is by 11 controls of valve switch controller. Can ensure the vaporization incorporation time that sample is enough, also can avoid the inhomogeneous loss of sample short circuit, all there is preferably effect in capillary column effect and the extended column life-span for protection chromatographic column 7 simultaneously.
The invention will be further described below by embodiment.[embodiment]
Adopt injector of the present invention and general split stream injector, to be used for the comparison of quantitative analysis results.
Instrument: HP-5890 II type gas chromatograph.
Detecting device: flame ionization ditector (FID) and thermal conductivity detector (TCD) (TCD)
Integraph: HP-3396
Injector: (1) general split stream injector,, split ratio 180: 1
(2) injector split ratio of the present invention is 180: 1
Temperature of vaporization chamber: 250 ℃, detector temperature: 280 ℃, column temperature: 140 ℃ 8 minutes, be warmed up to 200 ℃ with 30 ℃/minute then, stopped 10 minutes.Chromatographic column: 0.1 micron of HP-20M:50 rice * 0.2* millimeter *
Carrier gas: hydrogen
Sample: propylene, water, methyl alcohol, propylene glycol monomethyl ether potpourri
The different injector quantitative analysis results of same sample see Table 1
Two kinds of injector quantitative results of table 1 relatively
| Component | Propylene | Epoxypropane | Methyl alcohol | Water | Propylene glycol monomethyl ether | |
| Allocate sample size (weight %) into | 0.96 | 6.65 | 41.79 | 47.73 | 2.86 | |
| General injector | Mean value | 0.80 | 6.12 | 40.84 | 49.14 | 3.1 |
| Relative error (%) | 16.67 | 7.97 | 2.27 | -2.95 | -8.39 | |
| Injector of the present invention | Mean value | 0.94 | 6.62 | 41.66 | 47.9 | 2.88 |
| Relative error (%) | 2.08 | 0.45 | 0.31 | -0.35 | -0.70 | |
From table 1 data as can be seen, adopt general split stream injector,, the sample analysis result precision is relatively poor, especially with sample mixture in main component group depart from component far away, its " distortion " is even more serious, and the propylene relative error is up to 16.67%, and the propylene glycol monomethyl ether relative error is also bigger.Adopt split stream injector, of the present invention, quantitative error is less, data accuracy height.
Can illustrate that by top embodiment the present invention is a kind of quantitatively chromatic spectrum sample feeder accurately, is applicable to the split sampling analysis of various samples.
Claims (2)
1, a kind of chromatic spectrum sample feeder, comprise sample introduction mechanism, carrier gas inlet, well heater, carrier gas preheating chamber, shunting derivation passage and vaporizer, wherein sample introduction mechanism is on the top of vaporizer, the outside that passage is positioned at vaporizer is derived in shunting, the inside of carrier gas preheating chamber, carrier gas preheating chamber outside is a well heater; The bottom that passage is derived in shunting communicates with vaporizer, is closed state with the carrier gas preheating chamber, and the top seal of passage is derived in shunting; Shunting is derived the inter-agency space of channel roof and sample introduction and is communicated with carrier gas preheating chamber and vaporizer respectively; The bottom of vaporizer links to each other with extraneous chromatogram by conduit, and carrier gas inlet communicates with carrier gas preheating chamber bottom, is connected with the gas transfer valve between vaporizer and extraneous chromatogram, has extraneous bypass channel to link to each other in addition between carrier gas inlet and the gas transfer valve.
2,, it is characterized in that the gas transfer valve is three-way switch valve or four-way switching valve according to the described chromatic spectrum sample feeder of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001274422A CN1139807C (en) | 2000-11-15 | 2000-11-15 | Chromatic spectrum sample feeder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001274422A CN1139807C (en) | 2000-11-15 | 2000-11-15 | Chromatic spectrum sample feeder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1352390A CN1352390A (en) | 2002-06-05 |
| CN1139807C true CN1139807C (en) | 2004-02-25 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB001274422A Expired - Fee Related CN1139807C (en) | 2000-11-15 | 2000-11-15 | Chromatic spectrum sample feeder |
Country Status (1)
| Country | Link |
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| CN (1) | CN1139807C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104749389B (en) | 2013-12-30 | 2017-07-14 | 同方威视技术股份有限公司 | Universal injector, gas chromatograph and combination spectrometer |
| CN106525523B (en) * | 2017-01-03 | 2023-09-08 | 公安部第一研究所 | Thermal analysis sample injector for ion mobility spectrometer |
| CN114878731B (en) * | 2022-06-06 | 2024-04-26 | 翊新诊断技术(苏州)有限公司 | Volume-selectable ultra-microscale sample injection valve for liquid chromatography |
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2000
- 2000-11-15 CN CNB001274422A patent/CN1139807C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1352390A (en) | 2002-06-05 |
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Granted publication date: 20040225 Termination date: 20111115 |