CN205720122U - A kind of large volume sample injection system for gas chromatogram - Google Patents

A kind of large volume sample injection system for gas chromatogram Download PDF

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Publication number
CN205720122U
CN205720122U CN201620216612.9U CN201620216612U CN205720122U CN 205720122 U CN205720122 U CN 205720122U CN 201620216612 U CN201620216612 U CN 201620216612U CN 205720122 U CN205720122 U CN 205720122U
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column
gas chromatogram
large volume
chromatographic column
injection system
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CN201620216612.9U
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王嘉乐
罗辰
吴达
戚大伟
刘敏
林华清
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Shanghai Tobacco Group Co Ltd
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Shanghai Tobacco Group Co Ltd
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Abstract

This utility model relates to detecting instrument field, particularly relates to a kind of large volume sample injection system for gas chromatogram.This utility model provides a kind of large volume sample injection system for gas chromatogram, including gas chromatogram column oven, described gas chromatogram column oven is provided with chromatographic column pre-column and chromatographic column, described chromatographic column pre-column is connected with chromatographic column, also include that Agilent multi-mode injection port, described Agilent multi-mode injection port are connected with chromatographic column pre-column.The described large volume sample injection system for gas chromatogram, compared to tradition input mode, can significantly improve sampling volume, promote the sensitive of detection method.

Description

A kind of large volume sample injection system for gas chromatogram
Technical field
This utility model relates to detecting instrument field, particularly relates to a kind of large volume sample injection system for gas chromatogram.Described For the large volume sample injection system of gas chromatogram compared to tradition input mode, can significantly improve sampling volume, promote detection side Method sensitive.
Background technology
Traditional gas chromatographic sample introduction mode carrier with bushing pipe as solvent evaporation.Owing to when organic solvent vaporizes, expansion rate is big, boiling Point is relatively low, and the volume of bushing pipe cannot increase substantially, and therefore the sampling volume of gas chromatogram is generally limited by 5 below μ L. But, the increase of sampling volume can largely promote the sensitivity of detection method, improve the detection efficiency of machine.And For improving detector, adjusting the methods such as pre-treatment, the increase of sampling volume is more directly perceived, simple for promoting sensitivity Just.
Traditional large volume sample injection technology mainly has two classes, and one is based on convenient cold on-column injection, and two is based on temperature programming vaporisation techniques (PTV technology).Convenient cold on-column injection technology is applicable to analyze thermally labile sample, mainly by the color being connected with Cool-on-column inlet Spectrum post pre-column realizes solvent and focuses on, and increases sample size, and its shortcoming is that requirement sample substrate is clean, will not pollute chromatographic column and just can enter Row is analyzed.PTV input mode mainly realizes large volume sample injection by temperature programming-solvent air defense pattern, and i.e. sample is with liquid condition Enter cold bushing pipe, solvent and part low boiling component with carrier gas from shunting outlet air defense).After major part solvent volatilization is vented, Second time sample introduction can be carried out, repeat above solvent vent process, until completing required sample size.Bushing pipe have accumulated enough After determinand, raise vaporizer temperature and testing sample is transferred in chromatographic column, such that it is able to reach large volume sample injection effect.Its Advantage be sample be in bushing pipe vaporize, non-volatile matter be trapped in bushing pipe with protection chromatographic column be not contaminated, its shortcoming is to treat Survey target sample to be vented with carrier gas, cause analysis result on the low side.
Agilent gas chromatogram multi-mode injection port (MMI sample introduction) mouth compared with standard shunting/Splitless injecting samples mouth, take into Sample mouth temperature program(me) heating mode, thus cold Splitless injecting samples, i.e. liquid can also be realized and be sent to injection port bushing pipe by sample introduction needle In, to analyze sample and be temporarily stored into bushing pipe under injection port low temperature state, the rear vaporizer temperature that improves rapidly realizes test substance vaporization again Enter chromatographic column.Its advantage is that analyte vaporizes under minimum injector temperature rather than under constant high temperature, so that sample The probability of product thermal cracking is down to minimum, still allows for the vaporization of a large amount of analyte simultaneously.Its shortcoming is due to the position still office of vaporization Being limited to bushing pipe, therefore the volume of sample introduction still is limited to the volume of bushing pipe.Complete additionally, due to the vaporization of solvent remains moment , therefore the pressure increase of moment most likely results in sample partly and is spilled off bushing pipe.
Utility model content
The shortcoming of prior art in view of the above, the purpose of this utility model is to provide a kind of large volume for gas chromatogram Sampling system, is used for solving the problems of the prior art.
For achieving the above object and other relevant purposes, this utility model provides a kind of large volume sample injection system for gas chromatogram, It is characterized in that, including gas chromatogram column oven, described gas chromatogram column oven is provided with chromatographic column pre-column and chromatographic column, described Chromatographic column pre-column is connected with chromatographic column, also includes Agilent multi-mode injection port, is provided with in described Agilent multi-mode injection port Bushing pipe, described bushing pipe is connected with chromatographic column pre-column.
Preferably, described Agilent multi-mode injection port is the Agilent multi-mode injection port of cold Splitless injecting samples mode.
Preferably, described bushing pipe is not for shunt bushing pipe.
It is furthermore preferred that the described bushing pipe that do not shunts is not shunt bushing pipe with glass cotton.
It is furthermore preferred that the described internal diameter not shunting bushing pipe is 3.5-4.5mm, volume is 0.8-1.0mL.
Preferably, described chromatographic column pre-column is connected by two connectors with chromatographic column.
Preferably, described two connectors are Press Tight two connectors.
Preferably, described chromatographic column pre-column be deactivation without fixing phase capillary tube quartz glass cylinder, a length of 3-5 rice, internal diameter is 0.32-0.53 millimeter.
Preferably, described Agilent multi-mode injection port is positioned on gas chromatogram column oven.
As it has been described above, a kind of large volume sample injection system for gas chromatogram of the present utility model, have the advantages that this Utility model changes apparatus structure without complexity, i.e. may utilize Agilent multi-mode injection port (MMI injection port) and chromatographic column Pre-column realizes large volume sample injection, possesses traditional cold column head sampling and temperature programming vaporisation techniques (PTV technology) advantage.Use cold Splitless injecting samples, it is possible to achieve sample repeatedly sample introduction, improve further can sampling volume, promote sensitivity, at large volume sample injection Meanwhile, make non-volatile matter be trapped in bushing pipe reduction chromatographic column to pollute.Cold Splitless injecting samples can avoid the discrimination that solvent vent brings Depending on effect, it is ensured that the relatively accuracy of low boiling ingredient analysis.The vaporization of this utility model sample mainly completes in pre-column, therefore The volume of sample introduction is no longer limited by bushing pipe in theory, and the sample segment that the instant vaporization avoiding solvent causes dissipates out sample introduction Mouthful.
Accompanying drawing explanation
Fig. 1 is shown as this utility model structural representation.
Element numbers explanation
1 Agilent multi-mode injection port
2 bushing pipes
3 chromatographic column pre-columns
4 liang of connectors
5 chromatographic columns
6 gas chromatogram column ovens
Detailed description of the invention
By particular specific embodiment, embodiment of the present utility model being described below, those skilled in the art can be by this specification Disclosed content understands other advantages of the present utility model and effect easily.
Refer to Fig. 1.It should be clear that structure depicted in this specification institute accompanying drawings, ratio, size etc., the most only in order to coordinate Content disclosed in bright book, understands for those skilled in the art and reads, being not limited to this utility model enforceable Qualifications, therefore do not have technical essential meaning, the modification of any structure, the change of proportionate relationship or the adjustment of size, Do not affect under effect that this utility model can be generated by and the purpose that can reach, all should still fall in the skill disclosed in this utility model In the range of art content obtains and can contain.Meanwhile, in this specification cited as " on ", D score, "left", "right", " middle " And the term of " " etc., it being merely convenient to understanding of narration, and be not used to limit the enforceable scope of this utility model, it is relative Being altered or modified of relation, is changing under technology contents without essence, when being also considered as the enforceable category of this utility model.
As it is shown in figure 1, this utility model provides a kind of large volume sample injection system for gas chromatogram, including gas chromatogram column temperature Case 6, is provided with chromatographic column pre-column 3 and chromatographic column 5, described chromatographic column pre-column 3 and chromatographic column 5 in described gas chromatogram column oven 6 It is connected, also includes Agilent multi-mode injection port 1 (MMI injection port), in described Agilent multi-mode injection port 1, be provided with lining Pipe 2, described bushing pipe 2 is connected with chromatographic column pre-column 3.This utility model changes apparatus structure without complexity, i.e. may utilize Agilent Multi-mode injection port (MMI injection port) and chromatographic column pre-column realize large volume sample injection.Specifically, this utility model is using Time, sample is injected in Agilent multi-mode injection port 1 by sample introduction needle, and enters in the bushing pipe 2 of chromatographic column pre-column 3, described Agilent multi-mode injection port 1 and chromatographic column pre-column 3 all keep low temperature state, more preferably keep below solvent correction boiling point Temperature, the sample in bushing pipe 2 exists in liquid form.Along with the rising of Agilent multi-mode injection port 1 temperature and flow Increasing the solvent gasification brought, above fluid sample, pressure increases suddenly and solvent enters chromatographic column pre-column 3 and concentrates generation suction, Making sample be transferred in chromatographic column pre-column 3 with the form of solution band eventually, the sample entered in chromatographic column pre-column 3 is deposited with form of liquid film ?.Chromatographic column incubator 6 also keeps low temperature state in the starting stage, more preferably keeps below the temperature of solvent correction boiling point, After sample is transferred to pre-column 3 completely, chromatographic column incubator 6 start program heats up, and in pre-column 3, sample enters rear under carrier gas drives Chromatographic column 5.In utility model one embodiment, injector temperature arranges initial temperature and keeps below solvent correction boiling temperature, Being brought rapidly up after sample introduction completes, column oven temperature arranges initial temperature and is less than solvent correction boiling temperature, treats that sample is completely by entering Sample mouth is transferred to temperature programming after chromatographic column pre-column, and injection port flow set constant current mode, sample vaporization is transferred to chromatograph by bushing pipe Improve inlet pressure during post pre-column, prevent vaporescence sample from overflowing bushing pipe.
Provided by the utility model in the large volume sample injection system of gas chromatogram, vaporization is main in chromatographic column pre-column 3 Complete, so the volume of sample introduction is no longer limited by bushing pipe, and the sample segment that the instant vaporization avoiding solvent causes in theory Dissipate out injection port.Described chromatographic column pre-column 3 is preferably deactivation chromatographic column, in this utility model one embodiment, described deactivation Chromatographic column is Agilent 160-2535-30 deactivation Fused-silica capillary column, and internal diameter is 0.53mm.Those skilled in the art can root According to be actually needed (such as sampling volume) select chromatographic column pre-column 3 size, in this utility model one embodiment, described chromatograph The a length of 3-5 rice of post pre-column 3, internal diameter is 0.32-0.53 millimeter.
Provided by the utility model in the large volume sample injection system of gas chromatogram, described Agilent multi-mode injection port 1 It is preferably the Agilent multi-mode injection port of cold Splitless injecting samples mode, uses cold Splitless injecting samples, it is possible to achieve sample repeatedly enters Sample, improve further can sampling volume, promote sensitivity, at large volume sample injection simultaneously, make non-volatile matter be trapped in bushing pipe fall Low chromatographic column is polluted.Additionally, cold Splitless injecting samples can also avoid the discrimination effect that solvent vent brings, it is ensured that relatively low boiling becomes The accuracy of part detection.Further, in described Agilent multi-mode injection port 1, be provided with bushing pipe 2, described bushing pipe 2 be regardless of Stream bushing pipe, does not shunts bushing pipe preferably with glass cotton.The lining pipe that do not shunts with glass cotton is used to think that sample enters color The process of spectrum post pre-column 3 gasification provides sufficient cushion space.Those skilled in the art can adjust according to actual needs and not shunt lining The size of pipe, preferred internal diameter is 3.5-4.5mm, and volume is 0.8-1.0mL.In this utility model one embodiment, described not The internal diameter of shunting bushing pipe is 4mm, and volume is 0.9mL.
Provided by the utility model in the large volume sample injection system of gas chromatogram, those skilled in the art are optional suitable Mode connect chromatographic column pre-column 3 and chromatographic column 5, preferably by two connectors 4 by chromatographic column pre-column 3 and chromatographic column 5 phase Even, in this utility model one embodiment, described two connectors 4 are Press Tight two connectors.
Visible, the large volume sample injection system for gas chromatogram provided by the utility model possesses traditional cold column head sampling and program Intensification vaporisation techniques (PTV technology) advantage, compared to tradition input mode, can significantly improve sampling volume, promote detection Method sensitive.
In sum, this utility model effectively overcomes various shortcoming of the prior art and has high industrial utilization.
Above-described embodiment only illustrative principle of the present utility model and effect thereof, not for limiting this utility model.Any Above-described embodiment all can be modified under spirit and the scope of the present utility model or change by those skilled in the art. Therefore, such as art has usually intellectual without departing from the spirit disclosed in this utility model with under technological thought All equivalences completed are modified or change, and must be contained by claim of the present utility model.

Claims (9)

1. the large volume sample injection system for gas chromatogram, it is characterized in that, including gas chromatogram column oven (6), described gas chromatogram column oven (6) is provided with chromatographic column pre-column (3) and chromatographic column (5), described chromatographic column pre-column (3) is connected with chromatographic column (5), also include Agilent multi-mode injection port (1), being provided with bushing pipe (2) in described Agilent multi-mode injection port (1), described bushing pipe (2) is connected with chromatographic column pre-column (3).
A kind of large volume sample injection system for gas chromatogram, it is characterised in that described Agilent multi-mode injection port (1) is the Agilent multi-mode injection port of cold Splitless injecting samples mode.
A kind of large volume sample injection system for gas chromatogram, it is characterised in that described bushing pipe (2) is not for shunt bushing pipe.
A kind of large volume sample injection system for gas chromatogram, it is characterised in that the described bushing pipe that do not shunts is not shunt bushing pipe with glass cotton.
A kind of large volume sample injection system for gas chromatogram, it is characterised in that the described internal diameter not shunting bushing pipe is 3.5-4.5mm, and volume is 0.8-1.0mL.
A kind of large volume sample injection system for gas chromatogram, it is characterised in that described chromatographic column pre-column (3) is connected by two connectors (4) with chromatographic column (5).
A kind of large volume sample injection system for gas chromatogram, it is characterised in that described two connectors (4) are Press Tight two connectors.
A kind of large volume sample injection system for gas chromatogram, it is characterised in that described chromatographic column pre-column (3) be deactivation be 0.32-0.53 millimeter without fixing phase capillary tube quartz glass cylinder, a length of 3-5 rice, internal diameter.
A kind of large volume sample injection system for gas chromatogram, it is characterised in that described Agilent multi-mode injection port (1) is positioned on gas chromatogram column oven (6).
CN201620216612.9U 2016-03-21 2016-03-21 A kind of large volume sample injection system for gas chromatogram Active CN205720122U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113109483A (en) * 2021-05-07 2021-07-13 上海烟草集团有限责任公司 Analysis method for pyrolysis aroma components of potentially-fragrant raw material for cigarettes

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113109483A (en) * 2021-05-07 2021-07-13 上海烟草集团有限责任公司 Analysis method for pyrolysis aroma components of potentially-fragrant raw material for cigarettes

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