CN104407080B - portable gas chromatography capillary column module - Google Patents
portable gas chromatography capillary column module Download PDFInfo
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- CN104407080B CN104407080B CN201410740596.9A CN201410740596A CN104407080B CN 104407080 B CN104407080 B CN 104407080B CN 201410740596 A CN201410740596 A CN 201410740596A CN 104407080 B CN104407080 B CN 104407080B
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Abstract
Portable gas chromatography capillary column module of the invention possesses：Capillary column skeleton, circular hole has been axially formed from one end towards the other end；Block, is connected to described one end of the capillary column skeleton；Heater element, is inserted in the circular hole；Capillary column, is wound on the outer surface of the diaphragm；Barrel shrond, the inside configuration capillary column skeleton；Muff, covers on outside the finger-type cylinder being combined into by the barrel shrond and the block.
Description
Technical field
The present invention relates to gas chromatography analysis testing field, more particularly to a kind of Portable gas for gas chromatograph
Phase chromatography capillary string modules.
Background technology
Capillary column is in gas-chromatography（GC）In be responsible for separation function to compounding substances composition, be the crucial portion of GC
Part.Separation of the capillary column to material needs to carry out at a certain temperature, the lifting/lowering temperature speed and temperature homogeneity of chromatographic column
It is two important indicators of GC, determines the separating power and analyze speed of GC, it is therefore desirable to is heated to capillary column and temperature
Control design.
Traditional furnace box formula GC is that the wire turn that capillary column turns to 7~8 inches is suspended in a larger burner hearth,
It is thick with wrapping up（3~5cm）Heat-preservation cotton parcel furnace box, internal heater strip heats air, and applying power of enforcement using fan makes
Air flow heats/radiating to chromatographic column, and the desktop computer mode of heating of main flow belongs to such in the market.Due to by furnace box formula
The limitation of structure, the volume of this kind of device is big, weight weight, the big power consumption of thermal capacity are big, intensification cooling rate is slow.
The compact chromatogram column system of portable or modular construction is occurred in that in recent years, and the mode of heating of this kind of device is general
It is to be heated to chromatographic column by heat transfer.If United States Patent (USP) US8043565 and China CN02215114.1 are the generations of hot pillow formula heat transfer
Table, such device is that heater element is cast on a base for high heat conduction conductance, and submounts are furnished with cover plate, and chromatographic column is put
Put in the groove of base, base act as, to the heat pillow of chromatographic column conduction heat, opening the operable chromatographic column of upper cover plate.It is this kind of
Device reduces volume than stove chamber installation, reduces power consumption.However, the introducing of base and cover plate increased thermal capacity, base
Heater heating rate is far below with cover plate, therefore have impact on the programming rate of chromatographic column, on the other hand, heater element difference shadow
The uniformity of groove in base temperature is rung, post separation effect can have been influenceed.Low heat capacity（LTM）Technology overcomes heat pillow heating technique
Defect, LTM technologies are RVM companies patents of invention（Patents number：US5782964, US6209386, US6490852,
US6530260）, LTM technologies are that intertexture can be with coolant at one jointly by heater strip, capillary column, temperature sensor
On tubule, it is ensured that contacted with each other two-by-two between capillary column, heater strip, tubule three, realize chromatographic column super rapid heating and
Quick cooling, on the other hand, the tubule of winding chromatographic column can be coiled into 2~5 inches of annulars, substantially reduce chromatographic column coiling
Diameter.Agilent has merged RVM companies in 2008, and LTM patented technologies are converted into portable GC products, and in 2012
The patent distribution of LTM technologies has been done in China（Patent No. CN10268842A）.With Agilent 222-5532LTM modules（SN：
US12280712）As a example by, volume 150mm*153mm*53mm（* * wide long are high）, power consumption 300W, 1800 °C/min of programming rate, drop
Warm speed<1min, is that a performance peaks the GC post modules of rank.However, LTM technologies also have its defect：（1）Its capillary
The winding method of post and heater strip is complicated, it is necessary to realized with the coiling device of specialty, and user oneself cannot coiling, it is impossible to more moult
Capillary column, therefore it is limited to the selection of capillary column；（2）Its heater strip and chromatographic column are integrally fixed, and user cannot tear open
Open, once chromatographic column or heater strip have any one device to have the damage must to change whole module；（3）LTM Module Prices are expensive
（One U.S. dollar of module about 5000）, therefore selection of the restriction user to more chromatographic columns；（4）Its canoe cannot make chromatographic column
It is smaller that the diameter of disk contracts（2~5 inches）.
The content of the invention
The present invention is proposed to solve above-mentioned problems of the prior art, its object is to provide one kind just
Formula gas-phase chromatographic capillary column module is taken, be ensure that and realized that under the conditions of low-power consumption chromatographic column is rapidly heated, and can fast prompt drop
Temperature, on the other hand, the size of chromatographic column module is more compact, portable, and is easily changed the accessories such as chromatographic column, heater element, and
With a muff for easy attaching/detaching, facilitate the replacing of intraware, additionally, modular chromatogram column system is not only
Can be interconnected with various injectors and detector, and can in parallel or series, for the application function of expansion module between module.
To achieve these goals, the present invention provides a kind of portable gas chromatography capillary column module, it is characterised in that
Possess：
The capillary column skeleton of bobbin shape, from one end towards the other end along the capillary column skeleton axial shape
Into there is a circular hole, and the other end end face closing；
Block, is connected to described one end of the capillary column skeleton；
Heater element, is inserted in the circular hole of the capillary column skeleton；
Capillary column, is closely wound on the outer surface of the capillary column skeleton；And
Barrel shrond, its lower end closed and upper end open, and the capillary column skeleton is with coaxial with the barrel shrond
Mode is configured in the barrel shrond, and in the bottom face and the bottom face of the capillary column skeleton of the barrel shrond
Between remain with gap.
Additionally, in portable gas chromatography capillary column module of the invention, being also equipped with：Muff, covers on by described
Outside the finger-type cylinder that barrel shrond and the block are combined into.
Additionally, in portable gas chromatography capillary column module of the invention, the two ends band of the capillary column skeleton
There is protrusion eaves, also, the block is the disc with outer protrusion eaves.
Additionally, in portable gas chromatography capillary column module of the invention, also with being arranged on the capillary column
Temperature measuring device on skeleton.
Additionally, in portable gas chromatography capillary column module of the invention, also with for by the capillary column
The heat-conducting cream of the slot-coupled between skeleton and the heater element.
Additionally, in portable gas chromatography capillary column module of the invention, also with being arranged on the capillary column
Diaphragm between the protrusion eaves of protrusion eaves and the other end on the outer wall of skeleton and positioned at described one end, the capillary
Post is closely wound on the outer surface of the diaphragm.
Additionally, in portable gas chromatography capillary column module of the invention, in the outer eaves of the protrusion of the block and institute
Sealing ring is provided between the upper end for stating barrel shrond, thus, by the barrel shrond and the cap sealed, the circle is realized
Sealing between cylinder shell and the capillary column skeleton, forms bag between the barrel shrond and the capillary column skeleton
Enclose the circuferential spacing of the capillary column.
Additionally, in portable gas chromatography capillary column module of the invention, being wound with the institute of the capillary column
The circle diameter two ends of capillary column skeleton are stated, two thermal conductive silicon rubbers are respectively arranged with along the axial direction of the capillary column skeleton
Adhesive tape, thus, two parts is divided into by the circuferential spacing, the cooling gas circuit needed for being formed.
Additionally, in portable gas chromatography capillary column module of the invention, it is provided with for by institute in the block
State heater element extraction port, the temperature measuring device for the wire of the temperature measuring device to be drawn that the wire of heater element is drawn
The capillary column ingress port of one end connection and the other end of the capillary column for drawing port and the capillary column connect
The capillary column outlet port for connecing and the suction nozzle and outlet nozzle that are connected respectively with two parts of the circuferential spacing,
Hole corresponding with above-mentioned port respectively is provided with the muff.
Additionally, in portable gas chromatography capillary column module of the invention, the capillary column skeleton is by thermal conductivity
Light alloy material high is formed.
Additionally, in portable gas chromatography capillary column module of the invention, the winding section of the capillary column skeleton
A diameter of 20mm~the 80mm for dividing, is highly 20mm~200mm.
Additionally, in portable gas chromatography capillary column module of the invention, the heater element be heating rod or
Heating film.
Additionally, in portable gas chromatography capillary column module of the invention, the heat-conducting cream is heat-conducting silicone grease.
Additionally, in portable gas chromatography capillary column module of the invention, the heat-conducting cream is graphite film or indium
Paper tinsel.
Additionally, in portable gas chromatography capillary column module of the invention, the temperature measuring device is high-precision patch
Chip RTD, is attached on the wall of the winding portion of the capillary column skeleton.
Additionally, in portable gas chromatography capillary column module of the invention, the diaphragm is pellosil or pottery
Porcelain fiber cloth.
Additionally, in portable gas chromatography capillary column module of the invention, the capillary column is metal capillary
Post, MXT posts or vitreous silica post.
Additionally, in portable gas chromatography capillary column module of the invention, the capillary column is closely arranged with every circle
The mode of row winds.
Additionally, in portable gas chromatography capillary column module of the invention, the capillary column separates pre- with each circle
The mode at fixed interval winds.
Additionally, in portable gas chromatography capillary column module of the invention, the barrel shrond is low by thermal conductivity factor
Alloy material formed and inwall be minute surface.
Additionally, in portable gas chromatography capillary column module of the invention, the internal diameter of the barrel shrond is than described
The diameter of block is slightly smaller and more slightly larger than the diameter of the capillary column skeleton, and the block just covers the upper of the barrel shrond
End face, also, the barrel shrond is more slightly higher than the capillary column skeleton.
Additionally, in portable gas chromatography capillary column module of the invention, the sealing ring is led by high temperature resistant low-heat
Material is formed.
Additionally, in portable gas chromatography capillary column module of the invention, the set skin of the muff uses resistance to height
The polyimide fiber cloth of temperature cuts sewing and forms, described in the set intracutaneous portion filled with the excellent aeroge of heat-insulating property
The shape of muff is engaged with the profile of the finger-type chromatographic column module, including upper circular block and lower cylindrical sleeve, it is described on
Circular block and the lower cylindrical sleeve are closely connected by button loop.
Additionally, the present invention provides a kind of portable gas chromatography capillary column module, it is characterised in that
Possess portable gas chromatography capillary column module as described above,
The portable gas chromatography capillary column module is two i.e. the first portable gas chromatography capillary column module
The second portable gas chromatography capillary column mould different from the first portable gas chromatography capillary column module with attribute
Block,
The capillary column of the first portable gas chromatography capillary column module is gone out with a bilateral modulator
Mouth port is connected in series with the capillary column ingress port of the second portable gas chromatography capillary column module, described
The capillary column ingress port of the first portable gas chromatography capillary column module is connected to injector, and described second is portable
The capillary column outlet port of formula gas-phase chromatographic capillary column module is connected to detector.
Additionally, the present invention provides a kind of portable gas chromatography capillary column module, it is characterised in that
Possess multiple portable gas chromatography capillary column modules as described above, and multiple portable gas phase colors
The attribute for composing capillary column module is identical,
The capillary column outlet port of each of multiple portable gas chromatography capillary column modules with it is another
One capillary column ingress port of the portable gas chromatography capillary column module is connected by a bilateral modulator
Connect, first capillary column ingress port of the portable gas chromatography capillary column module and last described in just
The capillary column outlet port for taking formula gas-phase chromatographic capillary column module is hanging.
Additionally, the present invention provides a kind of portable gas chromatography capillary column module, it is characterised in that
Possess portable gas chromatography capillary column module as described above,
The portable gas chromatography capillary column module is two i.e. the first portable gas chromatography capillary column module
With the second portable gas chromatography capillary column module, and the first portable gas chromatography capillary column module and described
The attribute of the second portable gas chromatography capillary column module is identical,
The capillary column ingress port and described second of the first portable gas chromatography capillary column module is just
The capillary column ingress port for taking formula gas-phase chromatographic capillary column module is connected to same injector, also, described
The capillary column outlet port of one portable gas chromatography capillary column module and second portable gas chromatography hair
The capillary column outlet port of capillary column module is connected to different detectors.
As described above, the present invention considers reduction thermal capacity from every side and reducing energy consumption is designed：（1）It is high
The sealing space design that the cavity skeleton of thermal conductivity and the barrel shrond of low heat conductivity are formed reduces thermal capacity；（2）Heater
Part is capable of achieving to be rapidly heated by way of conducting and being heated directly to capillary column；（3）The mirror design of barrel shrond, can subtract
Few heat radiation loss；（4）Convection heat losses can be effectively prevented using aerogel insulation layers.Four aspects of summary, in drop
Supper-fast intensification is also achieved while low-power consumption.Have module additionally, the present invention takes cleverly cooling circulation canal to design
For quick temperature-reducing function.
Additionally, adiabatic system of the invention uses shell type：Set skin uses fire resistant polyimide fiber cloth, inside fills out airsetting
Glue, safety non-toxic, high insulating effect；Put with button loop, conveniently shirk；Put and leave metal core and facilitate internal components to draw
Line.Shell type design overcomes and passes adiabatic apparatus defect not easy to remove.
Additionally, design of the invention take into account each device convenient disassembly：Take off muff, you can change heater
Part；Skeleton is extracted out from barrel shrond, chromatographic column is that exposure is before eyes, is convenient for changing.Change device convenient, overcome existing
Module can not change the defect that entirely module is scrapped after chromatographic column, and indivedual accessory damages.
Additionally, small volume of the present invention, modularization, can pass through series/parallel expansion module application function.
Brief description of the drawings
Fig. 1 A are the longitudinal profile schematic diagrams of portable gas chromatography capillary column module of the invention.
Fig. 1 B are the horizontal section schematic diagrams of the module medium position in Figure 1A.
Fig. 1 C are the schematic diagrames of block.
Fig. 2A and Fig. 2 B are the schematic diagrames of the Application Example that module of the present invention is expanded to full two dimension or chromatography in series.
Fig. 3 A and Fig. 3 B are the schematic diagrames of the Application Example that module of the present invention is expanded to chromatogram in parallel.
Description of reference numerals：
1 capillary column skeleton
2 caps
3 heater elements
4 temperature measuring devices
5 heat-conducting creams
6 capillary columns
7 diaphragms
8 barrel shronds
9 sealing rings
10 heat-conducting silicon rubber bars
11 fan arc sealing areas
12 fan arc sealing areas
13 heater elements draw port
14 temperature measuring devices draw port
15 capillary column ingress ports
16 capillary column outlet ports
17 suction nozzles
18 outlet nozzles
19 heat abstractors
20 muffs
21 bilateral modulators
22 injectors
23 detectors
24 triple valves
25 another detectors.
Specific embodiment
Hereinafter, portable gas chromatography capillary column module of the invention is illustrated in detail referring to the drawings.
Figure 1A is portable gas chromatography capillary column module of the invention（Hereinafter, module otherwise referred to as of the present invention）'s
Longitudinal profile schematic diagram, Fig. 1 B are the horizontal section schematic diagrams of the module medium position in Figure 1A.
Specifically, as shown in FIG. 1A and 1B, portable gas chromatography capillary column module of the invention possesses：Two ends
The capillary column skeleton 1 of the bobbin shape with protrusion eaves, towards its other end along hair from one end of capillary column skeleton 1
Capillary column skeleton 1 has been axially formed circular hole, also, the other end end face closing；With the discoidal block for protruding outer eaves
2, one end of capillary column skeleton 1 is connected to, it is in figure ia the upper end for being connected to capillary column skeleton 1；Heater element 3, inserts
Enter in the circular hole of capillary column skeleton 1；Temperature measuring device 4, is arranged on capillary column skeleton 1 and positioned at capillary column skeleton 1
Between heater element 3；Heat-conducting cream 5, for by the slot-coupled between capillary column skeleton 1 and heater element 3；Diaphragm 7
It is arranged on the outer wall of capillary column skeleton 1, also, as shown in Figure 1A, diaphragm 7 is located at the two of capillary column skeleton 1
Between individual protrusion eaves；Capillary column 6, is closely wound on the outer surface of diaphragm 7；Barrel shrond 8, its lower end closed and upper end is opened
Put, capillary column skeleton 1 is configured in barrel shrond 8 in the mode coaxial with barrel shrond 8, also, as shown in Figure 1A,
Gap is remained between the bottom face of barrel shrond 8 and the bottom face of capillary column skeleton 1；Sealing ring 9, is arranged on block 2
Protrusion it is outer barrel shrond 8 and block 2 are sealed between eaves and the upper end of barrel shrond 8, realize barrel shrond 8 and capillary
Sealing between spinous process of the seventh cervical vertebra frame 1, forms the circuferential spacing for surrounding capillary column 1 between barrel shrond 8 and capillary column skeleton 1；
It is separately positioned on the circle diameter two ends of the capillary column skeleton 1 for being wound with capillary column 6 and along capillary column skeleton 1
Two axially extending heat-conducting silicon rubber bars 10, two parts are divided into by above-mentioned circuferential spacing, the cooling gas circuit needed for being formed；
Muff 20, covers on outside the finger-type cylinder being combined into by barrel shrond 8 and block 2.
Additionally, Fig. 1 C are the schematic diagrames of block.As shown in Figure 1 C, six holes are offered in block 2 as extraction pipeline
Port：Both end of which mouth draws heater element and thermal detector wire respectively, and two of which port is capillary styletable, is tapped into respectively
Sample device and detector, two other is breather port, a suction nozzle, an outlet nozzle.That is, six above-mentioned holes be not for
The heater element that the wire of heater element 3 is drawn draws port 13, the temperature measuring device for the wire of temperature measuring device 4 to be drawn
Draw the other end connection of the capillary column ingress port 15 and capillary column 6 of one end connection of port 14 and capillary column 6
Capillary column outlet port 16 and the suction nozzle 17 and outlet nozzle 18 that are connected respectively with two parts of circuferential spacing.This
Outward, six corresponding cores are reserved with muff 20 in case pipeline is drawn.
As shown in Figure 1A, in the present invention, capillary column skeleton 1 is for example traditional bobbin shape, and two ends carry
The eaves of protrusion, is prevented from capillary column slippage, and circle is axially provided with along skeleton at the upper surface center of capillary column skeleton 1
Hole, the lower end face closure of capillary column skeleton 1.Correspondingly, block 2 is the disc for example with the outer eaves of protrusion, in capillary
The upper surface of spinous process of the seventh cervical vertebra frame 1 is connected as a single entity with capillary column skeleton 1.Capillary column skeleton 1 is using thermal conductivity alloy in lightweight material high
Material, such as magnadure etc..It is formed with the protrusion eaves of capillary column skeleton 1 and is respectively communicated with suction nozzle 17 and outlet nozzle 18
Hole so that suction nozzle 17 and outlet nozzle 18 are connected with above-mentioned circuferential spacing.Additionally, capillary column skeleton and block are not limited
In structure as described above, as long as being that by being played a part of in the present invention, naturally it is also possible to be other structures.
Additionally, in the present invention, the winding portion of capillary column skeleton 1 is a diameter of of the part between two protrusion eaves
20mm~80mm, is highly 20mm~200mm.Additionally, the eaves requirement of tube wall and two ends protrusion is keeping the feelings of skeleton not deformation
It is as thin as possible under condition, to reduce thermal capacitance, it is easy to be rapidly heated/lower the temperature.
In the present invention, heater element 3 can use any heater element that can be profile-followed with the vestibule of capillary column skeleton 1,
For example, heating rod or heating film etc., and be not particularly restricted.Preferably, can be inserted directly into frame center hole using heating rod,
So it is convenient for changing.Heat-conducting cream 5 is provided between heater element 3 and capillary column skeleton 1, the effect of heat-conducting cream 5 is to make to add
Thermal device such as heating rod and the close-coupled of capillary column skeleton 1, realize giving the rapid and uniform heating of capillary column 6.Heat-conducting cream 5 can
To use heat-conducting silicone grease, operating temperature -50~480 DEG C are cheap, convenient to smear, and can also use graphite film or indium foil, two
The ductility and thermal conductivity of person are very well and operating temperature is higher, and the operating temperature of graphite is 0 ~ 3000 DEG C, the work temperature of indium foil
It is 0~2080 DEG C to spend, and simply both prices are all slightly higher.
Additionally, temperature measuring device 4 is high-precision SMD RTD, the winding portion of capillary column skeleton 1 is close to
On wall.But it is not limited to this, or other temperature measurement devices.
In the present invention, diaphragm 7 is enclosed within the periphery of capillary column skeleton 1, and diaphragm 7 can use for example resistant to elevated temperatures silicon
Glued membrane, or resistant to elevated temperatures ceramic fiber cloth, thickness is 0.5~1mm, plays friction and the elastic reaction of increase skeleton,
Both the light coiling of capillary column had been facilitated, and heating had been solved again and cooling situation lower skeleton expansion or shrinkage may caused capillary
Major gene is tight and be broken or slide problem because lax.
Additionally, in the present invention, it is preferred that capillary column 6 uses metal capillary post or MXT posts, such hair
Capillary column is different from the quartz column employed in patent document CN1877319A and CN10268842A, and metal column is stainless steel
Material, inside pipe wall is processed as inert layer, and chromatographic stationary phases are scribbled on inert layer, and the high temperature resistant that pipe outer wall scribbles micron order thickness is exhausted
Edge layer.Metal capillary post is than traditional quartz capillary column good toughness, and intensity is big, therefore can be with the smaller curvature of coiling half
Footpath, additionally, this capillary column is not broken under stress, temperature higher is resistant to than quartz column, and the life-span is longer.Additionally, at this
Capillary column 6 can also use vitreous silica post in invention.
Additionally, the coiling on capillary column, can be wound, it is also possible to separated with each circle in the compact arranged mode of every circle
The mode of predetermined space winds, and capillary column overall length is, for example, 5m ~ 30m.But the present invention can also use traditional quartzy capillary
Tubing string is, it is necessary to use the skeleton coiling of relatively large radius.
In the present invention, using the relatively low alloy material of thermal conductivity factor, cylinder inner wall is minute surface to barrel shrond 8, so that can
Reduce the radiation loss of internal heat.Additionally, the wall thickness on barrel shrond 8, can be made in the case of enough load-bearing it is relatively thin,
To reduce thermal capacity.
In the present invention, the internal diameter of barrel shrond 8 is omited than the diameter of the circular block 2 that the upper end of capillary column skeleton 1 is protruded
Small and more bigger than the diameter of capillary column skeleton 1, block 2 just covers the upper surface of barrel shrond 8, and barrel shrond 8 compares capillary
Tubing string skeleton 1 is slightly higher, i.e. remain with tiny seam between the bottom face of barrel shrond 8 and the bottom face of capillary column skeleton 1
Gap.
Additionally, sealing ring 9 is high-temperature resistant rubber or the low thermal conducting material of other high temperature resistants.The diameter and cylinder of sealing ring 9
The internal diameter of shell 8 is identical, is enclosed within the lower section of block 2, the sealing between barrel shrond 8 and capillary column skeleton 1 is realized, in cylinder
A narrow and small circumferential sealing space is formed between shell 8 and capillary column skeleton 1.
At the two ends of a certain bar diameter symmetry of circumference around the capillary column skeleton 1 for making capillary column 6 along skeleton axle
To one layer of high temperature resistant silicon adhesive tape 10 is pasted respectively, chromatographic column on the one hand can be compacted, on the other hand can be by barrel shrond 8 and capillary
Circumferential sealing space between tubing string skeleton 1 is divided into two fan arc sealing areas 11,12, two fan arc areas 11,12
By the gap area of the bottom face of capillary column skeleton 1, at each, the corresponding upper surface of fan arc area is each makes a call to a stomata,
Can be formed to the gas circuit of the cooling of capillary column 6.
Additionally, six ports in block, wherein the heater element drawn and temperature measuring device port connection high temperature resistant wire,
Two ports for drawing capillary column 6 are realized sealing with graphite pressure ring, and two capillary column joints can be transferred to by bilateral
The detector 23 of injector 22/, it is also possible to which serial or parallel connection to other modules realizes that functions of modules extends, suction nozzle 17, outlet nozzle
18 edges for being arranged on block 2, connect, with two fan arc areas 11,12 in barrel shrond 8 when capillary column 6 is needed respectively
When lowering the temperature, the fan arc area that cooling medium is entered between capillary column skeleton 1 and barrel shrond 8 by suction nozzle 17
And another fan arc area is flowed through from bottom, and finally flowed out from the outlet nozzle 18 at the edge of block 2, realize capillary column 6
Fast cooling.Cooling method can connect refrigerant by valve（Such as liquid CO 2 or liquid nitrogen）Mode realize, it is also possible to pass through
Air pump is connect at valve, is realized by the mode of rapid aeration.
Additionally, on muff 20, its set skin cuts sewing and forms using resistant to elevated temperatures polyimide fiber cloth, covers intracutaneous
Portion is to be capable of achieving good heat insulation effect filled with the excellent aeroge of heat-insulating property, the thickness aeroge of 10mm.Insulation is cut out a piece of cloth in a way with the minimum material to make two or more articles of clothing
The shape cut is engaged with the profile of finger-type chromatographic column module, including upper cap and following cylindrical sleeve, and two parts pass through button loop
Closely connection, unclamping button loop can lay down muff.
The existing portable chromatogram module size of Agilent is 150mm*153mm*53mm,（L*W*H）.And color of the invention
Spectrum module minimum dimension is 60mm*70mm（2R*H）, the size of chromatogram column system is further reduced, realize portable, mould
Block.
The operation principle of portable gas chromatography capillary column module of the invention：Can be by single finger-type module of the invention
As overall applicability, it is also possible to multiple finger-type modules are carried out into serial or parallel connection, identical or different chromatographic column, Neng Goutuo is taken
The application of color development spectrum.For example：（1）With bilateral by the block coupled in series of two or more identical capillary columns, increase capillary column
Length, realizes the separation to complicated ingredient；（2）The block coupled in series of two different capillary columns is formed complete two with a modulator
Dimension chromatographic system；（3）With leading to one the wired in parallel of multiple different type capillary columns is connect into obstructed detector more, be capable of achieving same
When to polytype composition parallel detection, improve analysis efficiency.With reference to serial or parallel connection, the finger-type capillary column module is only
Vertical heating, independent temperature conveniently realizes different measurements beneficial to different temperature settings.Each finger-type mould in serial or parallel connection
Block can be removed as entirety from whole machine, easy to loading and unloading.
Additionally, the present invention preferably elastomeric metal capillary post, the radius of curvature of coiling 5mm, therefore can without fracture
It is smaller with do chromatographic column module.Additionally, quartz capillary column is very crisp, its outer wall just has one after applying one layer of polyimide film
Fixed elasticity, this layer of polyimide film will occur aging under long term high temperature, cause capillary column to become fragile frangibility, and metal kernel
Will not be broken under capillary column long term high temperature, using metal capillary post, solve quartz column be under smaller radius of curvature it is long-term
The problem of easy fracture during hot operation, improves the life-span of chromatographic column module.
Embodiment 1
As shown in Figure 1A, Figure 1B, in the present embodiment 1, capillary column 6 is with 5m × 0.25mm i.d. × 0.25 μm specification
MXT posts as a example by be illustrated.It is elastic good due to capillary column 6, therefore thinner capillary column skeleton can be selected.Block 2
It is connected as a single entity with capillary column skeleton 1 in the upper surface of capillary column skeleton 1.Heater element 3 is inserted in the sky of capillary column skeleton 1
Coupled with capillary column skeleton 1 by heat-conducting cream 5 in chamber.Temperature measuring device 4 is close on the inwall of capillary skeleton 1, heater
Part 3 and temperature measuring device 4 heater element respectively from block 2 draw port 13 and temperature measuring device is drawn port 14 and draws and connect
In power supply and temperature controller, the accurate temperature controlling to capillary column 6 is realized with pid algorithm.The overall length 5m of capillary column 6, external diameter is about
0.4mm, with compact arranged form winding of single layer on capillary column skeleton 1, when coiling radius of curvature is 21, coiling wire turn
Height about 30mm, the joint of the reserved certain length in the two ends of capillary column 6 is respectively from capillary column ingress port 15 and capillary
Draw column outlet port 16.Diaphragm 7 is provided between capillary column skeleton 1 and capillary column 6, diaphragm 7 is close to hair
On capillary column skeleton 1, the friction and elasticity, the capillary column 6 that prevents thereon for playing increase capillary column skeleton 1 slip and because
The effect of the impact that capillary column skeleton 1 deforms and brought to capillary column 6.Two heat-conducting silicon rubber bars 10 are axially tight along skeleton
The both sides of capillary column skeleton 1 for being wound with capillary column 6 are attached to, fixation on the one hand is played to capillary column 6, on the other hand
The peripheral gap formed between barrel shrond 8 and capillary column skeleton 1 is divided into two fan arc sealing areas 11 and 12, two
The gap area that sector region 11 and 12 passes through the bottom face of capillary column skeleton 1, two sector regions 11 and 12 respectively with
Suction nozzle 17 in block 2 is connected with outlet nozzle 18, by the heat abstractor 19 for being connected with suction nozzle 17 and outlet nozzle 18 respectively
Formed to the gas circuit of the cooling of capillary column 6.The upper surface of barrel shrond 8 and the outer eaves of the protrusion of block 2 are sealed by sealing ring 9,
Barrel shrond 8 uses the alloy material of low heat conductivity, and inside is minute surface, prevents heat to external radiation.Capillary column 6 is suspended on close
Envelope space in, formed between barrel shrond 8 and capillary column skeleton 1 about 3~5mm peripheral gap and with capillary column skeleton
The space connection of 1 bottom.Muff 20 is closely linked as one by descending cylindrical sleeve and upper circular block to constitute accordingly by button loop
Body, the upper circular block of muff 20 reserves corresponding six metal cores and facilitates lead.The set skin of muff 20 is high temperature resistant
The sewing of polyimide fiber cloth is formed, inside filling aeroge, is covered on outside the finger-type cylinder that barrel shrond 8 and block 2 are combined into,
A complete gas-phase chromatographic capillary column module is formed, the module totality product of the present embodiment is about 60mm*70mm（2R*H）.This
Outward, in reverse order：Muff 20 is taken off, lower casing 8 is taken out, all exposure is before eyes for all devices, facilitates dismounting and change.
Embodiment 2
Similarly, the present embodiment is using the capillary column module as shown in Figure 1A and Figure 1B, the present embodiment and embodiment 1
Difference be, in the present embodiment, capillary column 6 using 30m × 0.25mm i.d. × 0.25 μm specification quartz
Post.The length of all capillary columns 6 is more long, and elasticity is poor, therefore the size of capillary column skeleton 1 is bigger than embodiment 1.Except this it
Outward, other all devices of the present embodiment and its assembling is not repeated completely with embodiment 1.The module totality product of the present embodiment is about
For：100mm*100mm（2R*H）.
Embodiment 3
In the present embodiment, it is Application Example that two modules of the present invention are expanded to comprehensive two dimensional gas chromatography module.
Fig. 2A and Fig. 2 B are the application implementations that module of the present invention is expanded to full two dimension or chromatography in series in the present embodiment
The schematic diagram of example.As shown in Figure 2 A and 2 B, the individual module in Fig. 2A is the module shown in Figure 1A and Figure 1B.Two module dresses
The capillary column attribute matched somebody with somebody is different.With a bilateral modulator 21 by first module（It is in fig. 2 the module in left side）Hair
Capillary column outlet port 16 and second module（It is in fig. 2 the module on right side）Capillary column ingress port 15 series connection connect
Connect, the capillary column ingress port 15 of first module is connected to injector 22, second capillary column outlet port of module
16 are connected to detector 23, and by adjusting intermediate dual-pass modulator 21, two modules form comprehensive two dimensional gas chromatography module.
Embodiment 4
It is in the present embodiment the Application Example of multimode series connection.
As shown in Figure 2 A and 2 B, individual module is the module shown in Figure 1A and Figure 1B in Fig. 2A.Configured in multiple modules
The identical capillary column of attribute, middle modulator 21 is simple bilateral modulator, by bilateral modulator 21 by two
Individual block coupled in series doubles capillary column length, but, the present invention is not limited to two series connection of module, can in this way by multiple
Block coupled in series, forms longer capillary column, strengthens the separating power of capillary column, can be used for the sample point to complicated ingredient
Analysis.
Embodiment 5
It is in the present embodiment two Application Examples of wired in parallel.
Fig. 3 A and Fig. 3 B are the schematic diagrames of the Application Example that module of the present invention expands to chromatogram in parallel.Such as Fig. 3 A and Fig. 3 B
Shown, the individual module in Fig. 3 A is the module shown in Figure 1A and Figure 1B, can the identical hair of mount attribute in two modules
Capillary column.Injector 22 connects two capillary column arrival ends 15 of module respectively by a triple valve 24, realizes two colors
Spectrum post wired in parallel.Two modules are connected to two different detectors of attribute 23,25, and single injected sampling can be realized to various
Separated component is detected simultaneously.Traditional single detector spectrometer, it is desirable to during to heterogeneity not missing inspection, generally requires to change detection
Device carries out repeating sample introduction test, and this mode by two wired in parallel overcomes current single detector and material composition is rung
Defect limited in one's ability is answered, the detectability of single measurement is substantially increased.
As described above, the present application is illustrated, but be not restricted to that this, it is understood that can be in the present invention
Various combinations and various changes are carried out in the range of objective to above-mentioned implementation method, for example, each part can come as needed
Its shape or structure are designed, additionally, for example, the part such as muff, temperature measuring device, heat-conducting cream or diaphragm can also basis
Need and remove from the structure of foregoing portable gas chromatography capillary column module.
Claims (26)
1. a kind of portable gas chromatography capillary column module, it is characterised in that possess：
The capillary column skeleton of bobbin shape, from one end towards the other end being axially formed along the capillary column skeleton
Circular hole, and the other end end face closing；
Block, is connected to described one end of the capillary column skeleton；
Heater element, is inserted in the circular hole of the capillary column skeleton；
Capillary column, is closely wound on the outer surface of the capillary column skeleton；And
Barrel shrond, its lower end closed and upper end open, and the capillary column skeleton is in the mode coaxial with the barrel shrond
Configure in the barrel shrond, and between the bottom face of the barrel shrond and the bottom face of the capillary column skeleton
Remain with gap.
2. portable gas chromatography capillary column module as claimed in claim 1, it is characterised in that
It is also equipped with：Muff, covers on outside the finger-type cylinder being combined into by the barrel shrond and the block.
3. portable gas chromatography capillary column module as claimed in claim 2, it is characterised in that
The two ends of the capillary column skeleton are with protrusion eaves, also, the block is the disc with outer protrusion eaves.
4. portable gas chromatography capillary column module as claimed in claim 3, it is characterised in that
Also there is the temperature measuring device being arranged on the capillary column skeleton.
5. portable gas chromatography capillary column module as claimed in claim 4, it is characterised in that
Also having is used for the heat-conducting cream of the slot-coupled between the capillary column skeleton and the heater element.
6. portable gas chromatography capillary column module as claimed in claim 5, it is characterised in that
Also with the protrusion eaves and the other end being arranged on the outer wall of the capillary column skeleton and positioned at described one end
Diaphragm between protrusion eaves,
The capillary column is closely wound on the outer surface of the diaphragm.
7. portable gas chromatography capillary column module as claimed in claim 6, it is characterised in that
Sealing ring is provided between eaves and the upper end of the barrel shrond outside the protrusion of the block, thus, by the cylinder
Shell and the cap sealed, realize the sealing between the barrel shrond and the capillary column skeleton, outside the cylinder
The circuferential spacing for surrounding the capillary column is formed between shell and the capillary column skeleton.
8. portable gas chromatography capillary column module as claimed in claim 7, it is characterised in that
At the circle diameter two ends of the capillary column skeleton for being wound with the capillary column, along the capillary column skeleton
Axial direction be respectively arranged with two heat-conducting silicon rubber bars, thus, the circuferential spacing is divided into two parts, the drop needed for being formed
Wet road.
9. portable gas chromatography capillary column module as claimed in claim 8, it is characterised in that
It is provided with for the heater element of the wire extraction of the heater element to be drawn into port, for by described in the block
The temperature measuring device that the wire of temperature measuring device is drawn draws the capillary column arrival end of one end connection of port and the capillary column
The capillary column outlet port of the other end connection of mouth and the capillary column and two parts with the circuferential spacing
The suction nozzle and outlet nozzle for connecting respectively,
Hole corresponding with above-mentioned port respectively is provided with the muff.
10. the portable gas chromatography capillary column module as described in any one of claim 1~9, it is characterised in that
The capillary column skeleton is formed by thermal conductivity light alloy material high.
The 11. portable gas chromatography capillary column module as described in any one of claim 1~9, it is characterised in that
A diameter of 20mm~80mm of the winding portion of the capillary column skeleton, is highly 20mm~200mm.
The 12. portable gas chromatography capillary column module as described in any one of claim 1~9, it is characterised in that
The heater element is heating rod or heating film.
The 13. portable gas chromatography capillary column module as described in any one of claim 5~9, it is characterised in that
The heat-conducting cream is heat-conducting silicone grease.
14. portable gas chromatography capillary column modules as claimed in claim 13, it is characterised in that
The heat-conducting cream is graphite film or indium foil.
The 15. portable gas chromatography capillary column module as described in any one of claim 4~9, it is characterised in that
The temperature measuring device is high-precision SMD RTD, is attached on the wall of the winding portion of the capillary column skeleton.
The 16. portable gas chromatography capillary column module as described in any one of claim 6~9, it is characterised in that
The diaphragm is pellosil or ceramic fiber cloth.
The 17. portable gas chromatography capillary column module as described in any one of claim 1~9, it is characterised in that
The capillary column is metal capillary post, MXT posts or vitreous silica post.
The 18. portable gas chromatography capillary column module as described in any one of claim 1~9, it is characterised in that
The capillary column is wound in the compact arranged mode of every circle.
The 19. portable gas chromatography capillary column module as described in any one of claim 1~9, it is characterised in that
The capillary column winds in the way of each circle separates predetermined space.
The 20. portable gas chromatography capillary column module as described in any one of claim 1~9, it is characterised in that
The barrel shrond is formed by the low alloy material of thermal conductivity factor and inwall is minute surface.
The 21. portable gas chromatography capillary column module as described in any one of claim 1~9, it is characterised in that
The internal diameter of the barrel shrond is more slightly smaller than the diameter of the block and more slightly larger than the diameter of the capillary column skeleton, described
Block just covers the upper surface of the barrel shrond, also, the barrel shrond is more slightly higher than the capillary column skeleton.
22. portable gas chromatography capillary column modules as claimed in claim 7, it is characterised in that
The sealing ring is formed by the low thermal conducting material of high temperature resistant.
The 23. portable gas chromatography capillary column module as described in any one of claim 2~9, it is characterised in that
The set skin of the muff cuts sewing and forms using resistant to elevated temperatures polyimide fiber cloth, in set intracutaneous portion filling
There is the aeroge that heat-insulating property is excellent,
The shape of the muff is engaged with the profile of the finger-type chromatographic column module, including upper circular block and lower cylinder
Set, the upper circular block and the lower cylindrical sleeve are closely connected by button loop.
A kind of 24. portable gas chromatography capillary column modules, it is characterised in that
Possess the portable gas chromatography capillary column module described in any one of claim 1~23,
The portable gas chromatography capillary column module is two i.e. the first portable gas chromatography capillary column module and category
The property second portable gas chromatography capillary column module different from the first portable gas chromatography capillary column module,
With a bilateral modulator by the capillary column port of export of the first portable gas chromatography capillary column module
Mouth is connected in series with the capillary column ingress port of the second portable gas chromatography capillary column module, and described first
The capillary column ingress port of portable gas chromatography capillary column module is connected to injector, second Portable gas
The capillary column outlet port of phase chromatography capillary string modules is connected to detector.
A kind of 25. portable gas chromatography capillary column modules, it is characterised in that
Possess the portable gas chromatography capillary column module described in any one of multiple claims 1~23, and it is multiple
The attribute of the portable gas chromatography capillary column module is identical,
The capillary column outlet port of each of multiple portable gas chromatography capillary column modules and another
The capillary column ingress port of the portable gas chromatography capillary column module is connected by a bilateral modulator, the
One capillary column ingress port of the portable gas chromatography capillary column module is described portable with last
The capillary column outlet port of gas-phase chromatographic capillary column module is hanging.
A kind of 26. portable gas chromatography capillary column modules, it is characterised in that
Possess the portable gas chromatography capillary column module described in any one of claim 1~23,
The portable gas chromatography capillary column module is two i.e. the first portable gas chromatography capillary column module and the
Two portable gas chromatography capillary column modules, and the first portable gas chromatography capillary column module and described second
The attribute of portable gas chromatography capillary column module is identical,
The capillary column ingress port of the first portable gas chromatography capillary column module and described second portable
The capillary column ingress port of gas-phase chromatographic capillary column module is connected to same injector, also, described first just
Take the capillary column outlet port and the second portable gas chromatography capillary of formula gas-phase chromatographic capillary column module
The capillary column outlet port of post module is connected to different detectors.
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| CN201410740596.9A CN104407080B (en) | 2014-12-08 | 2014-12-08 | portable gas chromatography capillary column module |
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| CN201410740596.9A CN104407080B (en) | 2014-12-08 | 2014-12-08 | portable gas chromatography capillary column module |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| EP3903100A4 (en) * | 2018-12-28 | 2022-08-31 | Bioneer Corporation | Heater integrated gas chromatography column device |
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