CN203772879U - Universal sample injector, gas chromatograph and combined spectrometer - Google Patents
Universal sample injector, gas chromatograph and combined spectrometer Download PDFInfo
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- CN203772879U CN203772879U CN201320880833.2U CN201320880833U CN203772879U CN 203772879 U CN203772879 U CN 203772879U CN 201320880833 U CN201320880833 U CN 201320880833U CN 203772879 U CN203772879 U CN 203772879U
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- vaporizer
- injector
- injector housing
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- sample
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Abstract
The utility model discloses a universal sample injector, comprising a sample injection opening mechanism, a sample injector shell, a vaporizing chamber, a heater, a temperature control unit, a carrier gas channel, an isolation pad purging channel, a shunting channel, a coolant channel and a multi-channel airflow control valve. The universal sample injector can be taken as a temperature programmed sample injector combining a shunting/non-shunting mode with a cold column head sample injection manner, is capable of bringing the advantages of various sample injection manners into full play and overcoming many defects and is high in practicability and flexibility.
Description
Technical field
The utility model belongs to analyzing and testing field, relates to a kind of gas chromatography or gas chromatography-ion mobility spectrometry coupling spectrometer sampling device, relates in particular to a kind of shunting for capillary column/not branch program intensification injector.
Background technology
Adopt gas chromatography (GC), GC and ion mobility spectrometry (IMS)/mass spectrum (MS) coupling spectrometer to carry out in analytic process sample, first sample will pass through injector.Injector is for being added to fast, accurately, quantitatively GC column cap in primary importance by interested sample composition gasification and after mixing with carrier gas.Since Perkin Elmer produces first capillary column, because its post effect is high, the advantage that separating property is good, had today exceed 90% GC analyze all realize (" Basic Gas Chromatography " by capillary column, Second Edition, by Harold M. McNair and James M. Miller. Copyright 2009 John Wiley & Sons, Inc.).Due to the long-pending little characteristic of capacity of capillary column itself, make shunting/Splitless injecting samples device become GC, GC-IMS or the most general injector of GC-MS.
At present existing ripe shunting/Splitless injecting samples device.But due to the actual split ratio difference of different sample component, separate under ratio in certain setting, this will cause the composition that enters chromatographic column (capillary column) to be different from original sample composition, bring shunting to discriminate against (shunting for the sample of wide boiling range is discriminated against particularly serious), thereby impact analysis accuracy, causes quantitative and repeatability is poor.
Cause shunting to discriminate against and mainly contain three aspects:
The one, the heating-up temperature branch of vaporizer is inhomogeneous, and the temperature difference at vaporizer center and two ends is very large in some cases, while causing like this position arriving after the gasification of the different component of the inhomogeneous gasification of sample or boiling point lower than gasification point, produces and condenses.
The 2nd, carrier gas is without preheating, and carrier gas enters vaporizer and have the variation of a thermograde, can cause like this sample different component gasification rate difference.Gasify to the time that enters chromatographic column very short (in second) from vaporizer.Like this, because bypass flow is greater than flow in post farthest, therefore component just may be than many points of the components being gasified totally some samples that pour off not too completely in gasification.
The 3rd, the rate of propagation difference of different sample component in carrier gas, and rate of propagation is directly proportional to temperature, is to eliminate the important measures that shunting is discriminated against so make sample Quick-gasifying as far as possible.Therefore injector temperature must strictly be controlled as slightly higher than post case temperature, like this, has improved on the one hand the cost of manufacture of injector, is also unfavorable on the one hand the analysis to determination system of thermal unstable material.
Patent CN1352390A discloses a kind of injector, solve the Preheating of carrier gas, this injector is derived between passage and vaporizer and is provided with carrier gas preheating chamber in shunting, and carrier gas inlet communicates with carrier gas preheating chamber bottom, and the top of carrier gas preheating chamber is communicated with vaporizer.Carrier gas moves upward from entrance enters the preheating of carrier gas preheating chamber, then enters vaporizer from top and contacts with sample and make it moment gasification.Although this injection port has solved the problem of carrier gas Preheating and shunting discrimination, but because its preheating chamber is connected with vaporizer, this has been equivalent to increase the volume of vaporizer, increase the front dead volume of post.Like this, the sample mix gas after gasification can antidiffusion arrive preheating chamber, will cause retention time to increase and peak broadening.
In order to overcome some problems that exist in patent CN1352390A, patent CN203216933U discloses a kind of injector for difficult volatile matter, comprise the anemostat of shell and described enclosure, shell end covers and is provided with the carrier passage being connected with anemostat, it is inner and apart from anemostat bottom certain distance that carrier gas passage extends to anemostat, the benefit of design is like this, because sample is placed on the bottom of anemostat, the volatilization concentration on sample its surface in the time of volatilization is the highest, carrier gas passage is extended to sample surfaces top, carrier gas can all be taken away the Volatile Gas of sample surfaces like this.In order to make injector top and the bottom homogeneous heating, be evenly arranged in the shell surrounding of this injector the electrical bar that extends to end cap from outer casing bottom, realize injector top and the bottom homogeneous heating.This patent has reduced the inhomogeneous gasification problem of sample, but this injector only has not shunt mode.Due to comparatively complexity of Splitless injecting samples pattern operating conditions, high to operative technique requirement, in real work, apply the split sampling that is far from general, just in the time that can not meeting analysis requirement (being mainly sensitivity requirement), split sampling just considers Splitless injecting samples.
In addition, in the time that Detection task is various, need continuous sample introduction, and the boiling range of adjacent twice sample has in notable difference situation, need to reset the temperature of injector, although dissimilar shunting/Splitless injecting samples device kind is more, and the universal sample injector of fast cooling few.In order to realize quick test, therefore need to increase fast cooling design and temperature control design at universal sample injector.
Utility model content
In order to solve above-mentioned problems of the prior art, the purpose of this utility model is to provide a kind of simple in structure, quick continuous sample introduction, to the effective universal injector of wide boiling range sample detection.Inventor recognizes, the preheating of the uniform temperature of vaporizer, carrier gas and the abundant mixing of sample can be eliminated shunting and discriminate against.
In order to achieve the above object, according to an aspect of the present utility model, provide a kind of universal injector.Described universal injector comprises sample introduction port mechanism, injector housing, vaporizer, well heater, temperature conditioning unit, carrier gas passage, dottle pin purge passage, split channel, coolant channel, hyperchannel control damper and temperature conditioning unit; Described sample introduction port mechanism is positioned at the top of described injector housing, and described sample introduction port mechanism comprises end cap and is positioned at the dottle pin of described end cap below; Described vaporizer is positioned at the center of described injector housing, has open top at described vaporizer top, is provided with capillary column at the center position of described vaporizer bottom; Between described end cap and vaporizer, there is O-ring seal; Described O-ring seal is arranged on the inwall of described vaporizer, is positioned near described open top, for bushing pipe or sample hose being supported on to the inside of described vaporizer; Described injector housing is metal material, and described end cap center is coaxial with described vaporizer center; In described injector housing, be provided with the carrier gas passage, dottle pin purge passage, split channel and the coolant channel that extend along the length direction of described injector housing; Described multiple passage is evenly distributed on described vaporizer around; The length direction of described carrier gas passage from described injector housing bottom along described injector housing extends, and communicates with the open top of described vaporizer; Described dottle pin purge passage goes out vaporizer and outwards derives gas from the bottom of described injector housing in the lower opening of described dottle pin; Described split channel is from the wall upper shed of described vaporizer, and outwards derives gas from the bottom of described injector housing; Described coolant channel is evenly distributed on described vaporizer around, and outwards derives cooling medium from the bottom of described injector housing; The duty of described multiple passages is regulated and is realized by hyperchannel control damper; Described well heater is heated to realize single-point heating or temperature programme by described temperature conditioning unit control.
Described coolant channel plays the effect into vaporizer refrigeration cool-down, when cooling, can adopt the cold-producing medium that thermal capacity is large, comprises liquid nitrogen, liquid CO
2or water, also can directly dispel the heat with nitrogen or the air purge of air flow.In the time using liquid nitrogen or nitrogen cooling, coolant channel and vaporizer are set to communicate, cooling medium enters vaporizer by cooling duct, and flow out along split channel dottle pin purge passage and refrigerant outlet passage, play on the one hand the effect cooling, also play on the one hand the function that purges purification gasification chamber.In the time using the cold-producing medium cooling of non-inertia, coolant channel refluxes on described injector housing, and discord vaporizer communicates.Described well heater is evenly distributed on described injector housing outer wall, ensures that injector is heated evenly up and down.
This universal injector is equivalent to one and has given full play to the strong point of various input modes shunt/not shunting the programmed temperature sampling device combining with convenient cold on-column injection, has overcome above-mentioned shortcoming, and practicality is stronger, and dirigibility is better.
The beneficial effect of this universal injector is:
1, be provided with some passages along the length direction of described vaporizer, one of them is as carrier gas passage, can make carrier gas enter vaporizer preheating before, there is enough thermal capacity, ensure after sample enters vaporizer and gasified by Quick uniform, then enter capillary column, discriminate against thereby reduce shunting, thereby obtain preferably testing result.
2, other multiple passages respectively as the also design of coolant channel, dottle pin purge passage, split channel on injector housing, the benefit of this design is to reduce metal shell thermal capacity by getting through road on the one hand more, on described injector housing, mobile cooling medium and carrier gas can be taken away the heat of vaporizer on the other hand, vaporizer is played to the effect of cooling, this design can ensure to be rapidly heated and also can realize fast cooling, is of value to the quick continuous sample introduction while processing a large amount of Detection task.
3, the even branch of the well heater of the utility model injector is on injector housing, and the benefit of design is to realize to described injector housing homogeneous heating like this, and realizing is again rapidly heated ensures sample gasification evenly, reduces shunting and discriminates against.
4, the cooperation control of cooling duct, hyperchannel control damper and temperature controller makes injector have temperature programme function.Because the volatility of different samples is different, volatile for some, or at high temperature easily the material of cracking will set low temperature it is first volatilized, will be heated to high temperature to it for the sample of difficulty volatilization and promote volatilization, obtain best volatile quantity to each sample composition.Can service routine intensification sample introduction for the detection of wide boiling range sample, this can effectively protect the material of easy thermal cracking or coking.The benefit of design is injector to be used as universal injector like this, can effectively tackle wide boiling range sample analysis, eliminates shunting and discriminates against.
Preferably, described O-ring seal is high-temperature resistant rubber material or graphite material.
Preferably, described well heater is resistance wire or mica sheet.
According on the other hand of the present utility model, a kind of gas chromatograph is also disclosed, described gas chromatograph comprises the universal injector described in any one in above embodiment.
According to another aspect of the present utility model, a kind of gas chromatography-ion mobility spectrometry coupling spectrometer is also disclosed, described coupling spectrometer comprises the universal injector described in any one in above embodiment.
Also disclose a kind of gas chromatography-mass spectrography spectrometer more on the one hand according to of the present utility model, described coupling spectrometer comprises the universal injector described in any one in above embodiment.
Brief description of the drawings
For content of the present utility model is more easily understood, below in conjunction with accompanying drawing and specific implementation method, the utility model is described further.
Fig. 1 is according to the structural representation of the universal injector of the utility model one embodiment;
The symbol table of Fig. 1 Reference numeral is shown: 1-end cap, 2-dottle pin, 3-injector housing, 4-O-ring seal, 5-vaporizer, 6-bushing pipe, hole, 7-carrier gas road, 8-dottle pin sweep gas passage, 9-split channel, 10-coolant channel, 11-coolant entrance, 12-air source inlet, 13-hyperchannel control damper, 14-carrier gas inlet, 15-shunts outlet, the outlet of 16-dottle pin sweep gas, 17-coolant outlet, the total gas outlet of 18-, 19-capillary column, 20-well heater, 21-temperature controller, 22-injector housing xsect.
Embodiment
Referring to Fig. 1, according to an embodiment of the present utility model, the sample introduction port mechanism of injector is positioned at the top of injector, is made up of end cap 1 and dottle pin 2.End cap 1 is enclosed within on injector housing 3 by screw buckle, and convenient disassembly is inserted disposable sample hose while being convenient to solid sampling.
Described vaporizer 5 is positioned at the inside of described injector housing, has sealing dottle pin 2 by vaporizer and sample introduction port sealing between described vaporizer 5 and end cap 1, and described end cap center is coaxial with vaporizer center.When gas or liquid sample sample introduction, in vaporizer, can place quartz or glass bushing pipe, when solid sample sample introduction, can place absorption has the disposable sample hose of solid constituent.
Described bushing pipe or disposable sample hose 6 are overlapped tightening seal and are supported the centre that is placed in vaporizer 5 by O RunddichtringO 4.
Center position in vaporizer 5 bottoms is provided with capillary column 19.Described capillary column 19 is fixed on vaporizer bottom by the nut of sealing gasket and conveniently assemble and disassemble.
Evenly be provided with some passages in described injector housing 3 inside along vaporizer excircle, the position of passage can see in conjunction with injector housing square section 22, and all entry and exit of passage are all designed in the bottom of injector housing and all along the upper end of vaporizer length direction arrival injector.Described some passages can be divided into carrier gas passage 7, dottle pin purge passage 8, split channel 9, coolant channel 10 by function.Wherein, carrier gas inlet 14 is connected by valve with air source inlet 12, and the carrier gas inlet 14 of described carrier gas along carrier gas passage 8 from described injector housing bottom upwards enters vaporizer by the entrance of vaporizer 5 mobile being preheated along carrier passage; Described dottle pin purge passage 8 purges outlet 16 derivation in the lower opening of dottle pin 2 and along the length direction of described injector housing by the dottle pin of described injector housing bottom; Described split channel 9 enter by bushing pipe bottom that gap between vaporizer 5 and bushing pipe 6 enters into the top of vaporizer and below O-ring seal 4 near go out vaporizer 5 and along the split channel on described injector housing from bottom tapping outlet 15 derive.Described coolant channel 10 is evenly distributed on described vaporizer 5 around.Cooling medium can enter described coolant channel 10 from coolant entrance 11.In the time using the inert substance refrigeration cool-downs such as liquid nitrogen or nitrogen, coolant channel 10 can be communicated with vaporizer and above-mentioned cooling medium and carrier gas enter vaporizer cool gasification chamber simultaneously, cooling medium Ke Yan road dottle pin purge passage 8, split channel 9 and coolant channel 10 flow out from coolant outlet 17, one puts in the face of vaporizer plays the effect cooling, and plays on the one hand and purges the function purifying; In the time using other non-inertia cooling materials, coolant channel 10 is independent return flow line, is not communicated with vaporizer 5, only plays cooling.The duty of each passage and work schedule regulate realization by hyperchannel control damper 13.Total gas outlet 18 is connected with the outlet of above-mentioned multiple passages by hyperchannel control damper 13, for Exhaust Gas.
Described well heater 20 is evenly distributed on described injector housing around, ensures that described injector housing is heated evenly up and down.Well heater 20 realizes single-point by described temperature conditioning unit 21 controls or temperature programme is heated.Temperature conditioning unit 21 and hyperchannel control damper 13 synergies realize the cooling of injector.Detect when wide boiling range sample can opening program intensification function sample introduction, can effectively avoid cracking or the coking of low boiling position, can overcome again shunting and discriminate against, ensure the accuracy of testing result.
Preferably, described O-ring seal is high-temperature resistant rubber material or graphite material; Described well heater is resistance wire or mica sheet.
According on the other hand of the present utility model, a kind of gas chromatograph is also disclosed, described gas chromatograph comprises the universal injector described in any one in above embodiment.
According to another aspect of the present utility model, a kind of gas chromatography-ion mobility spectrometry coupling spectrometer is also disclosed, described coupling spectrometer comprises the universal injector described in any one in above embodiment.
Also disclose a kind of gas chromatography-mass spectrography spectrometer more on the one hand according to of the present utility model, described coupling spectrometer comprises the universal injector described in any one in above embodiment.
Above-mentioned embodiment is the explanation to technical solutions of the utility model just; the utility model is not limited only to above-described embodiment, and every and above-mentioned principle and the improvement on the utility model basis replace all should be within protection domain of the present utility model.
Claims (6)
1. a universal injector, comprising: sample introduction port mechanism, injector housing, vaporizer, well heater, temperature conditioning unit, carrier gas passage, dottle pin purge passage, split channel, coolant channel, hyperchannel control damper and temperature conditioning unit; Wherein
Described sample introduction port mechanism is positioned at the top of described injector housing, and described sample introduction port mechanism comprises end cap and is positioned at the dottle pin of described end cap below;
Described vaporizer is positioned at the center of described injector housing, has open top at described vaporizer top, is provided with capillary column at the center position of described vaporizer bottom;
Between described end cap and vaporizer, there is O-ring seal; Described O-ring seal is arranged on the inwall of described vaporizer, is positioned near described open top, for bushing pipe or sample hose being supported on to the inside of described vaporizer;
Described injector housing is metal material, and described end cap center is coaxial with described vaporizer center;
In described injector housing, be provided with the carrier gas passage, dottle pin purge passage, split channel and the coolant channel that extend along the length direction of described injector housing; Described multiple passage is evenly distributed on described vaporizer around;
The length direction of described carrier gas passage from described injector housing bottom along described injector housing extends, and communicates with the open top of described vaporizer;
Described dottle pin purge passage outwards derives gas in the lower opening of described dottle pin and from the bottom of described injector housing; Described split channel is from the wall upper shed of described vaporizer, and outwards derives gas from the bottom of described injector housing; Described coolant channel is evenly distributed on described vaporizer around, and outwards derives cooling medium from the bottom of described injector housing; The duty of described multiple passages is regulated and is realized by hyperchannel control damper;
Described well heater is heated to realize single-point heating or temperature programme by described temperature conditioning unit control.
2. universal injector according to claim 1, wherein said O-ring seal is high-temperature resistant rubber material or graphite material.
3. universal injector according to claim 1, wherein said well heater is resistance wire or mica sheet.
4. a gas chromatograph, described gas chromatograph comprises according to the universal injector described in any one in claim 1-3.
5. a coupling spectrometer, described coupling spectrometer is gas chromatography-ion mobility spectrometry coupling spectrometer, and described coupling spectrometer comprises according to the universal injector described in any one in claim 1-3.
6. a coupling spectrometer, described coupling spectrometer is gas chromatography-mass spectrography spectrometer, and described coupling spectrometer comprises according to the universal injector described in any one in claim 1-3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320880833.2U CN203772879U (en) | 2013-12-30 | 2013-12-30 | Universal sample injector, gas chromatograph and combined spectrometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320880833.2U CN203772879U (en) | 2013-12-30 | 2013-12-30 | Universal sample injector, gas chromatograph and combined spectrometer |
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| CN203772879U true CN203772879U (en) | 2014-08-13 |
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| CN201320880833.2U Withdrawn - After Issue CN203772879U (en) | 2013-12-30 | 2013-12-30 | Universal sample injector, gas chromatograph and combined spectrometer |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104407080A (en) * | 2014-12-08 | 2015-03-11 | 同方威视技术股份有限公司 | Portable gas chromatographic capillary column module |
| CN104749389A (en) * | 2013-12-30 | 2015-07-01 | 同方威视技术股份有限公司 | Universal type sample injector, gas chromatograph and combined spectrum instrument |
| CN109507135A (en) * | 2019-01-17 | 2019-03-22 | 中国科学院合肥物质科学研究院 | A kind of organic nitrate multichannel heating device based on Research on Cavity Ring Down Spectroscopy |
-
2013
- 2013-12-30 CN CN201320880833.2U patent/CN203772879U/en not_active Withdrawn - After Issue
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104749389A (en) * | 2013-12-30 | 2015-07-01 | 同方威视技术股份有限公司 | Universal type sample injector, gas chromatograph and combined spectrum instrument |
| WO2015101170A1 (en) * | 2013-12-30 | 2015-07-09 | 同方威视技术股份有限公司 | Universal sample injector, gas chromatograph, and spectrometer used in combination therewith |
| 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 |
| CN104407080A (en) * | 2014-12-08 | 2015-03-11 | 同方威视技术股份有限公司 | Portable gas chromatographic capillary column module |
| CN104407080B (en) * | 2014-12-08 | 2017-06-27 | 同方威视技术股份有限公司 | portable gas chromatography capillary column module |
| CN109507135A (en) * | 2019-01-17 | 2019-03-22 | 中国科学院合肥物质科学研究院 | A kind of organic nitrate multichannel heating device based on Research on Cavity Ring Down Spectroscopy |
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| GR01 | Patent grant | ||
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| AV01 | Patent right actively abandoned |
Granted publication date: 20140813 Effective date of abandoning: 20170714 |