CN106324166A - Gas chromatography detector - Google Patents
Gas chromatography detector Download PDFInfo
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- CN106324166A CN106324166A CN201510388238.0A CN201510388238A CN106324166A CN 106324166 A CN106324166 A CN 106324166A CN 201510388238 A CN201510388238 A CN 201510388238A CN 106324166 A CN106324166 A CN 106324166A
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Abstract
The invention discloses a gas chromatography detector. The gas chromatography detector comprises a heating block, a gas pipe, a reference filling material, a temperature measurement part, a catalyst filling material, a thermal insulation layer, a cavity and a signal processing system. The gas chromatography detector utilizes air as carrying gas and make-up gas. A chromatogram system effluent carried by the carrying gas fast and orderly goes through a reference filler and a catalyst filler, the effluent burns under catalysis and releases heat so that the catalyst filler temperature is increased and temperature change is changed into electric signal output through a temperature measurement part. The detector can construct a common detector or a selective detector through change of catalyst filler chemical performances. The detector has the characteristics of high sensitivity and fast response and can be used for detection of volatile organic compounds and combustible inorganic gas.
Description
Technical field
The present invention relates to measure detection field, more particularly to a kind of based on principle of catalyst combustion
Gas chromatography detector, this detector can be used for volatile organic matter and incendivity inorganic gas
Detection.
Background technology
Gas chromatography detector is the Primary Component of gas chromatograph, and it directly determines gas phase color
The important analysis performances such as the sensitivity of analysis of spectrum, the range of linearity.At present, conventional gas chromatogram
Detector includes thermal conductivity cell detector (TCD), electron capture detector (ECD), flame ion
Change detector (FID), flame photometric detector (FPD) and flame thermionic detector (FTD)
Deng.
TCD generally use hydrogen, helium as carrier gas, FID, FPD except use hydrogen,
Outside nitrogen, argon or helium are as carrier gas, in addition it is also necessary to hydrogen as combustion gas, air or
Oxygen is as combustion-supporting gas.ECD generally uses nitrogen, hydrogen, argon or helium as load
Gas.Restriction due to gas cylinder so that above detector does not only exists potential safety hazard and is unfavorable for
Use as portable detector.Along with being continuously increased of field condition detection demand, compel to be essential
The portable detector of carrier gas is made with air.
Based on catalysis burning detection technique be utilize analyte under the effect of catalyst, with sky
Gas generation combustion reaction, reaction liberated heat is made catalyst temperature raise, is catalyzed by mensuration
The technology that analyte is detected by the variations in temperature of agent.This technology only needs air to participate in, and is
Build the desirable technique of portable detector.At present, sensor based on catalysis burning has been reported
Road, but generally there is the shortcoming that response time length, sensitivity are low.The high state of Nanjing University of Technology
By force, yellow rosy clouds have invented catalytic combustion-type carbon monoxide transducer (patent based on critesistor
Number: CN 102706923 A).Owing to sintering of catalyst is urged by it in thermistor surface formation
Changing pearl, tested gas reacts at catalyst coating, and temperature element is positioned at catalyst
Portion, causes temperature element can not reflect the temperature rise that catalysis burning causes truly, in time, and then
The response time making sensor is longer, and sensitivity is relatively low.Therefore, the catalysis combustion of this structure
Burn detection mode and still can not meet the needs of gas chromatographic detection.
Summary of the invention
In order to solve above-mentioned technical problem, it is an object of the invention to provide a kind of use air and make
For the gas chromatography detector of carrier gas, there is quickly response and highly sensitive feature simultaneously, with
Meet on-the-spot, portable demand.
For achieving the above object, the present invention uses the technical scheme to be:
The present invention provides a kind of gas chromatography detector: by heat block, gas circuit pipe, reference filler,
First temperature element, the second temperature element, catalyst filling, the first heat insulation layer, the second thermal insulation
Layer, cavity, signal processing system form;Described cavity is cylindrical structural, cylindrical structural
Sidewall have an interface being perpendicular to sidewall, connect make-up gas road, a cylindrical end closure is also
Have interface and connect gas chromatographic column, cylindrical other end opening, connect gas circuit pipe, gas
Phase chromatographic column is coaxial with gas circuit pipe and is connected, and described gas circuit pipe is sequentially filled from cavity one end
One heat insulation layer, reference filler, the second heat insulation layer, catalyst filling and the 3rd heat insulation layer;First
In the temperature measuring area embedment reference filler of temperature element, the temperature measuring area embedment catalysis of the second temperature element
In agent filler, the wire of the first temperature element and the second temperature element connects signal processing system;
Gas circuit pipe is placed in heating element heater.
The wire of described first temperature element and the second temperature element from gas circuit pipe away from cavity
One end is drawn and is connected with signal processing system, or at gas circuit tube side wall opening, above-mentioned wire from
Opening part is drawn, and opening part is with sealant sealing.
Described first temperature element and the second temperature element are thermocouple, thermal resistance wire or temperature-sensitive electricity
Resistance, preferred thermoelectric is even.Described heating element heater is resistance wire.
Described reference filler is close with the thermal capacitance of catalyst filling and heatproof is not less than 400 DEG C.
Described reference filler (6) is one or two or more kinds in kieselguhr or metal-oxide,
Be preferably kieselguhr, above-mentioned metal-oxide be aluminium oxide, calcium oxide or zirconic one or
Two kinds or three kinds.
Described first heat insulation layer (5), the second heat insulation layer (7), the 3rd heat insulation layer (9) are glass
One in glass cellucotton, quartz fibre sieve plate cotton, ceramic, quartz fibre sieve plate or two kinds with
On, preferably quartz fibre is cotton.
Described catalyst filling is the solid carrier filler of supported catalyst active component, is wherein catalyzed
Active component be one pack system noble metal, multicomponent noble metal, one pack system transition metal oxide,
Multicomponent transition metal oxide, perovskite composite oxide or spinelle type composite oxides
In any one;Solid carrier is porous inorganic material.Such as support the bimetallic oxidation of platinum-palladium
Alumina particles, the titanium dioxide granule of supported gold, chromium oxide load molecular sieve granule, copper manganese are compound
Oxide carried titanium dioxide granule;There is the LaCoO of Ca-Ti ore type3Or LaFeO3Load
SBA-15 granule;There is the CuFe of spinel-type2O4Load ZrO2Carrier etc..
Described catalyst filling is identical with the length filling bed of reference filler.
Described gas circuit pipe is the inert glass tubing of quartz ampoule, earthenware or inwall, preferably quartz ampoule.
Beneficial effect
The present invention is compared with other detectors, it is only necessary to air, as carrier gas and make-up gas, operates phase
To simply, it is simple to carry.Common detector and choosing can be realized by the kind of more catalyst changeout
The transformation of selecting property detector.
The present invention uses packed type structure, makes effluent quickly logical from inside under the drive of carrier gas
Crossing catalyst filling so that measured object contacts with catalyst filling fully, reaction completely, improves
Sensitivity;Temperature element is placed in inside catalytic filler, can reflect what catalysis burning caused in time
Variations in temperature, reduces response time.
The present invention uses heater to separate with temperature measuring equipment, makes noise be substantially reduced.
The addition of make-up gas reduces the effective volume of detector, improves peak shape.
Accompanying drawing explanation
Fig. 1 (a) is the detector arrangement schematic diagram described in the embodiment of the present invention 1;B () is this
Detector arrangement schematic diagram described in inventive embodiments 2
Wherein, 1-cavity;2-gas chromatographic column;3-make-up gas road;4-gas circuit pipe;5-first is exhausted
Thermosphere;6-reference filler;7-the second heat insulation layer;8-catalyst filling;9-the 3rd heat insulation layer;
10-the first temperature element;11-the second temperature element;12-heating element heater;13-fluid sealant.
Detailed description of the invention
Embodiment 1
Assemble a kind of gas chromatography detector, as shown in Fig. 1 (a), by heat block (12),
Gas circuit pipe (4), reference filler (6), the first temperature element (10), the second temperature element (11),
Catalyst filling (8), the first heat insulation layer (5), the second heat insulation layer (7), cavity (1), letter
Number processing system composition;Described cavity (1) is cylindrical structural, the sidewall of cylindrical structural
Having the interface being perpendicular to sidewall, connect make-up gas road (3), a cylindrical end closure is also opened
There is interface to connect gas chromatographic column (2), cylindrical other end opening, connect gas circuit pipe (4),
Gas chromatographic column (2) is coaxial with gas circuit pipe (4) and is connected, and described gas circuit pipe (4) is certainly
Cavity (1) one end is sequentially filled the first heat insulation layer (5), reference filler (6), the second thermal insulation
Layer (7), catalyst filling (8) and the 3rd heat insulation layer (9);First temperature element (10)
Temperature measuring area embedment reference filler (6) in, the temperature measuring area embedment of the second temperature element (11)
In catalyst filling (8), the first temperature element (10) and the second temperature element (11)
Wire from gas circuit pipe away from cavity one end draw connect signal processing system;Gas circuit pipe (4)
It is placed in heating element heater (12).
Above-mentioned heating element heater (12) is heat block;First temperature element and the second temperature element are equal
For K-type thermocouple;Reference filler is kieselguhr, and granularity is 60 mesh, loading 30mg;
It is cotton that first heat insulation layer, the second heat insulation layer, the 3rd heat insulation layer are quartz fibre;Catalytic filler is
Alumina load platinum catalyst, granularity is 60 mesh, loading 35mg;Gas circuit pipe is interior
Footpath 1mm quartz ampoule.This detector can be used for volatile organic matter, CO, H2Detection.
Embodiment 2
As shown in Fig. 1 (b), on the basis of the gas chromatography detector described in embodiment 1, gas
Road pipe 4 is respectively equipped with opening two packing areas, the first temperature element 10 and the second thermometric unit
The wire of part 11 is drawn from two opening parts respectively, and seals fixing with fluid sealant 13, seals
Inorganic glue selected by glue 13.
Embodiment 3
On the basis of the gas chromatography detector described in embodiment 1, catalyst filling 8 changes load into
Carrying the titanium dioxide granule of gold, loading 35mg, wherein the loading of gold is 10% (w/w),
This detector is used for 130 DEG C of selective enumeration method methanol.
Claims (10)
1. a gas chromatography detector, it is characterised in that: by heat block (12), gas circuit pipe
(4), reference filler (6), the first temperature element (10), the second temperature element (11), urge
Agent filler (8), the first heat insulation layer (5), the second heat insulation layer (7), cavity (1), signal
Processing system forms;Described cavity (1) is cylindrical structural, and the sidewall of cylindrical structural is opened
Having the interface being perpendicular to sidewall, connect make-up gas road (3), a cylindrical end closure also has
Interface connects gas chromatographic column (2), cylindrical other end opening, connects gas circuit pipe (4),
Gas chromatographic column (2) is coaxial with gas circuit pipe (4) and is connected, and described gas circuit pipe (4) is certainly
Cavity (1) one end is sequentially filled the first heat insulation layer (5), reference filler (6), the second thermal insulation
Layer (7), catalyst filling (8) and the 3rd heat insulation layer (9);First temperature element (10)
Temperature measuring area embedment reference filler (6) in, the temperature measuring area embedment of the second temperature element (11)
In catalytic filler (8), leading of the first temperature element (10) and the second temperature element (11)
Line connects signal processing system;Gas circuit pipe (4) is placed in heating element heater (12).
Detector the most according to claim 1, it is characterised in that: described first thermometric unit
The wire of part (10) and the second temperature element (11) from gas circuit pipe (4) away from cavity (1)
One end draw and be connected with signal processing system, or at gas circuit pipe (4) sidewall opening, on
Stating wire to draw from opening part, opening part seals with fluid sealant (13).
Detector the most according to claim 1, it is characterised in that: described first thermometric unit
Part (10) and the second temperature element (11) are in thermocouple, thermal resistance wire or critesistor
Planting or two kinds or three kinds, preferred thermoelectric is even;Described heating element heater (12) is resistance wire.
Detector the most according to claim 1, it is characterised in that: described reference filler (6)
And heatproof close with the thermal capacitance of catalyst filling (8) is not less than 400 DEG C.
5. according to the detector described in claim 1 or 4, it is characterised in that: described reference is filled out
Material (6) is one or two or more kinds in kieselguhr or metal-oxide, preferably kieselguhr,
Above-mentioned metal-oxide is the one in aluminium oxide, calcium oxide or zirconium oxide or two kinds or three kinds.
Detector the most according to claim 1, it is characterised in that: described first heat insulation layer
(5), the second heat insulation layer (7), the 3rd heat insulation layer (9) are porous high-temperature resistant thermal insulating material.
7. according to the detector described in claim 1 or 6, it is characterised in that: described first exhausted
Thermosphere (5), the second heat insulation layer (7), the 3rd heat insulation layer (9) are glass fibre cotton, quartz
One or two or more kinds in cellucotton, pottery sieve plate, quartz fibre sieve plate, is preferably quartz
Cellucotton.
Detector the most according to claim 1, it is characterised in that: described catalyst filling
(8) being the solid carrier filler of supported catalyst active component, wherein catalytic active component is single
Component noble metal, multicomponent noble metal, one pack system transition metal oxide, multicomponent transition gold
Belong to any one in oxide, perovskite composite oxide or spinelle type composite oxides;Gu
Body carrier is porous inorganic material.
Detector the most according to claim 1, it is characterised in that: described catalyst is filled out
Material (8) is identical with the filling bed length of reference filler (6).
Detector the most according to claim 1, it is characterised in that: described gas circuit pipe (4)
For the inert glass tubing of quartz ampoule, earthenware or inwall, preferably quartz ampoule.
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CN201096760Y (en) * | 2007-08-21 | 2008-08-06 | 北京吉天仪器有限公司 | Catalyzing and oxidation thermal resistance gas phase color spectrum detector |
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2015
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CN104101670A (en) * | 2013-04-02 | 2014-10-15 | 株式会社岛津制作所 | Column unit and gas chromatography device provided with the same |
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