CN106324166B - A kind of gas chromatography detector - Google Patents
A kind of gas chromatography detector Download PDFInfo
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- CN106324166B CN106324166B CN201510388238.0A CN201510388238A CN106324166B CN 106324166 B CN106324166 B CN 106324166B CN 201510388238 A CN201510388238 A CN 201510388238A CN 106324166 B CN106324166 B CN 106324166B
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- heat insulation
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- insulation layer
- temperature element
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Abstract
The invention discloses a kind of gas chromatography detector, including the component such as heat block, gas circuit pipe, reference filler, temperature element, catalyst filling, heat insulation layer, cavity, signal processing system.Use air as carrier gas and make-up gas, chromatographic system effluent passes sequentially through reference filler and catalyst filling rapidly under carrier gas drive, heat is released in effluent catalysis burning raises catalyst filling temperature, and temperature change is converted into electric signal output through temperature element.The detector can build common detector or selective detector by changing the chemical property of catalyst filling.The detector has the characteristics of sensitivity is high, response is fast, the detection available for volatile organic matter and incendivity inorganic gas.
Description
Technical field
The present invention relates to measurement detection field, more particularly to a kind of gas chromatographic detection based on principle of catalyst combustion
Device, the detector can be used for the detection of volatile organic matter and incendivity inorganic gas.
Background technology
Gas chromatography detector is the Primary Component of gas chromatograph, and it directly determines the sensitive of gas chromatographic analysis
The important analysis performance such as degree, range of linearity.At present, conventional gas chromatography detector includes thermal conductivity cell detector (TCD), electronics
Acquisition detector (ECD), flame ionization detector (FID), flame photometric detector (FPD) and flame thermionic detector
(FTD) etc..
TCD is usually using hydrogen, helium as carrier gas, and FID, FPD using hydrogen, nitrogen, argon gas or helium except being made
Outside for carrier gas, in addition it is also necessary to which hydrogen is used as combustion-supporting gas as combustion gas, air or oxygen.ECD is usually using nitrogen, hydrogen, argon
Gas or helium are used as carrier gas.Due to the limitation of gas cylinder so that above detector does not only exist potential safety hazard and is unfavorable for making
Used for portable detector.With being continuously increased for field condition detection demand, in the urgent need to making the portable of carrier gas with air
Formula detector.
Detection technique based on catalysis burning is that using analyte in the presence of catalyst, occur burning with air anti-
Should, reaction liberated heat raises catalyst temperature, and analyte is detected by determining the temperature change of catalyst
Technology.This technology only needs air to participate in, and is the desirable technique for building portable detector.At present, the biography based on catalysis burning
Sensor is it has been reported that but the low shortcoming of generally existing response time length, sensitivity.The high Guoqiang of Nanjing University of Technology, yellow rosy clouds
Catalytic combustion-type carbon monoxide transducer (the patent No. based on thermistor is invented：CN 102706923 A).Because it will
Sintering of catalyst is in thermistor surface formation catalysis beads, and tested gas reacts in catalyst coating, and temperature element
Positioned at catalytic inner, temperature element is caused to reflect temperature rise caused by catalysis burning truly, in time, and then cause sensing
The response time of device is longer, and sensitivity is relatively low.Therefore, the catalysis combustion supervision mode of this structure can not still meet gas-chromatography
The need for detection.
The content of the invention
In order to solve the above-mentioned technical problem, it is an object of the invention to provide a kind of gas phase color for using air as carrier gas
Detector is composed, while the characteristics of there is quick response and high sensitivity, to meet live, portable demand.
To achieve the above object, the present invention use technical scheme for：
The present invention provides a kind of gas chromatography detector：By heat block, gas circuit pipe, reference filler, the first temperature element,
Two temperature elements, catalyst filling, the first heat insulation layer, the second heat insulation layer, cavity, signal processing system composition；The cavity is
Cylindrical structural, the side wall of cylindrical structural is provided with the interface perpendicular to side wall, connection make-up gas road, a cylindrical end closure
And interface connection gas chromatographic column is provided with, cylindrical other end opening connects gas circuit pipe, gas chromatographic column and gas circuit pipe are same
Axle and it is connected, the gas circuit pipe is sequentially filled the first heat insulation layer, reference filler, the second heat insulation layer, catalyst from cavity one end
Filler and the 3rd heat insulation layer；In the temperature measuring area embedment reference filler of first temperature element, the temperature measuring area embedment of the second temperature element
In catalyst filling, the wire connection signal processing system of the first temperature element and the second temperature element；Gas circuit pipe is placed in heating
In element.
The wire of first temperature element and the second temperature element is drawn and signal from the one end of gas circuit pipe away from cavity
Processing system is connected, or in gas circuit pipe sidewall opening, above-mentioned wire is drawn at opening, and opening sentences sealant sealing.
First temperature element and the second temperature element are thermocouple, thermal resistance wire or thermistor, and preferred thermoelectric is even.Institute
Heating element heater is stated for resistance wire.
The reference filler is close with the thermal capacitance of catalyst filling and heatproof is not less than 400 DEG C.
The reference filler (6) is the one or two or more kinds in diatomite or metal oxide, preferably diatomite, on
It is aluminum oxide, one kind of calcium oxide or zirconium oxide or two kinds or three kinds to state metal oxide.
First heat insulation layer (5), the second heat insulation layer (7), the 3rd heat insulation layer (9) be glass fibre cotton, quartz fibre cotton,
One or two or more kinds in ceramic sieve plate, quartz fibre sieve plate, preferably quartz fibre cotton.
The catalyst filling is the solid carrier filler of supported catalyst active component, and wherein catalytic active component is single group
Noble metal, multicomponent noble metal, one pack system transition metal oxide, multicomponent transition metal oxide, Ca-Ti ore type is divided to be combined
It is any in oxide or spinelle type composite oxides；Solid carrier is porous inorganic material.For example support platinum-palladium bimetallic
Alumina particle, the titanium dioxide granule of supported gold, chromium oxide load molecular sieve particle, Cu-Mn complex oxide load dioxy
Change titanium particle；LaCoO with Ca-Ti ore type3Or LaFeO3Load SBA-15 particles；CuFe with spinel-type2O4Load
ZrO2Carrier etc..
The catalyst filling is identical with the length of the filling bed of reference filler.
The gas circuit pipe is quartz ampoule, earthenware or the inert glass tube of inwall, preferably quartz ampoule.
Beneficial effect
The present invention is compared with other detectors, it is only necessary to which air is as carrier gas and make-up gas, and operation is relatively easy, is easy to take
Band.The transformation of common detector and selective detector can be realized by the species of more catalyst changeout.
The present invention uses packed type structure, makes effluent under the drive of carrier gas quickly from inside by catalyst filling,
So that measured object is contacted fully with catalyst filling, reaction is complete, improves sensitivity；Temperature element is placed in catalytic filler
Portion, temperature change caused by catalysis burning can be reflected in time, the response time is reduced.
The present invention is separated using heater with temperature measuring equipment, substantially reduces noise.
The addition of make-up gas reduces the effective volume of detector, improves peak shape.
Brief description of the drawings
Fig. 1 (a) is the detector structural representation described in the embodiment of the present invention 1；(b) for described in the embodiment of the present invention 2
Detector structural representation
Wherein, 1- cavitys；2- gas chromatographic columns；3- make-up gas road；4- gas circuit pipes；The heat insulation layers of 5- first；6- reference fillers；
The heat insulation layers of 7- second；8- catalyst fillings；The heat insulation layers of 9- the 3rd；The temperature elements of 10- first；The temperature elements of 11- second；12- adds
Thermal element；13- fluid sealants.
Embodiment
Embodiment 1
A kind of gas chromatography detector is assembled, shown in such as 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), signal processing system composition；The cavity (1) is cylindrical structural, and the side wall of cylindrical structural is provided with vertically
In the interface of side wall, connect make-up gas road (3), a cylindrical end closure is simultaneously provided with interface connection gas chromatographic column (2), cylinder
The other end opening of shape, connection gas circuit pipe (4), gas chromatographic column (2) and gas circuit pipe (4) are coaxial and are connected, the gas circuit
Pipe (4) is sequentially filled the first heat insulation layer (5), reference filler (6), the second heat insulation layer (7), catalyst filling from cavity (1) one end
And the 3rd heat insulation layer (9) (8)；In the temperature measuring area embedment reference filler (6) of first temperature element (10), the second temperature element (11)
Temperature measuring area embedment catalyst filling (8) in, the wire of the first temperature element (10) and the second temperature element (11) is from gas circuit pipe
Draw connection signal processing system in one end away from cavity；Gas circuit pipe (4) 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 K-type thermocouple；Reference
Filler is diatomite, and granularity is 60 mesh, loading 30mg；First heat insulation layer, the second heat insulation layer, the 3rd heat insulation layer are quartz
Cellucotton；Catalytic filler is alumina load platinum catalyst, and granularity is 60 mesh, loading 35mg；Gas circuit pipe is internal diameter 1mm stones
Ying Guan.The 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 circuit pipe 4 is two packing areas
It is respectively equipped with opening, the wire of the first temperature element 10 and the second temperature element 11 is drawn at two openings respectively, and with close
The sealing of sealing 13 is fixed, and fluid sealant 13 selects inorganic glue.
Embodiment 3
On the basis of the gas chromatography detector described in embodiment 1, catalyst filling 8 is changed to the titanium dioxide of supported gold
Grain, loading 35mg, wherein the loading of gold is 10% (w/w), the detector is used for 130 DEG C of selective enumeration method methanol.
Claims (10)
1. a kind of gas chromatography detector, it is characterised in that：By heating element heater (12), gas circuit pipe (4), reference filler (6), 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), signal processing system is constituted；The cavity (1) is cylindrical structural, and the side wall of cylindrical structural is provided with perpendicular to side wall
Interface, is connected make-up gas road (3), and a cylindrical end closure is simultaneously provided with interface connection gas chromatographic column (2), it is cylindrical in addition
One end open, connection gas circuit pipe (4), gas chromatographic column (2) and gas circuit pipe (4) are coaxial and are connected, and the gas circuit pipe (4) is from chamber
Body (1) one end is sequentially filled the first heat insulation layer (5), reference filler (6), the second heat insulation layer (7), catalyst filling (8) and the 3rd
Heat insulation layer (9)；In the temperature measuring area embedment reference filler (6) of first temperature element (10), the temperature measuring area of the second temperature element (11)
It is embedded in catalytic filler (8), the wire connection signal processing system of the first temperature element (10) and the second temperature element (11)；Gas
Road pipe (4) is placed in heating element heater (12).
2. detector according to claim 1, it is characterised in that：First temperature element (10) and the second temperature element
(11) wire is drawn from the one end of gas circuit pipe (4) away from cavity (1) and is connected with signal processing system, or in gas circuit pipe (4)
Sidewall opening, above-mentioned wire is drawn at opening, and opening sentences fluid sealant (13) sealing.
3. detector according to claim 1, it is characterised in that：First temperature element (10) and the second temperature element
(11) it is one kind in thermocouple, thermal resistance wire or thermistor or two kinds or three kinds；The heating element heater (12) is resistance wire.
4. detector according to claim 1, it is characterised in that：The reference filler (6) and the heat of catalyst filling (8)
Hold close and heatproof and be not less than 400 DEG C.
5. the detector according to claim 1 or 4, it is characterised in that：The reference filler (6) is diatomite or metal oxygen
One kind in compound or two kinds, above-mentioned metal oxide are one kind or two kinds or three kinds in aluminum oxide, calcium oxide or zirconium oxide.
6. detector according to claim 1, it is characterised in that：First heat insulation layer (5), the second heat insulation layer (7),
Three heat insulation layers (9) are porous high-temperature resistant thermal insulating material.
7. the detector according to claim 1 or 6, it is characterised in that：First heat insulation layer (5), the second heat insulation layer
(7), the 3rd heat insulation layer (9) is glass fibre cotton, quartz fibre cotton, ceramic sieve plate, one kind in quartz fibre sieve plate or two kinds
More than.
8. detector according to claim 1, it is characterised in that：The catalyst filling (8) be supported catalyst activity into
The solid carrier filler divided, wherein catalytic active component are one pack system noble metal, multicomponent noble metal, one pack system oxo transition metal
It is any in compound, multicomponent transition metal oxide, perovskite composite oxide or spinelle type composite oxides；Solid
Carrier is porous inorganic material.
9. detector according to claim 1, it is characterised in that：The catalyst filling (8) and reference filler (6) are filled out
Fill bed length identical.
10. detector according to claim 1, it is characterised in that：The gas circuit pipe (4) is quartz ampoule, earthenware or interior
The inert glass tube of wall.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510388238.0A CN106324166B (en) | 2015-07-03 | 2015-07-03 | A kind of gas chromatography detector |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510388238.0A CN106324166B (en) | 2015-07-03 | 2015-07-03 | A kind of gas chromatography detector |
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| CN106324166A CN106324166A (en) | 2017-01-11 |
| CN106324166B true CN106324166B (en) | 2017-11-03 |
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Citations (8)
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|---|---|---|---|---|
| US3762878A (en) * | 1971-04-19 | 1973-10-02 | Beckman Instruments Inc | Apparatus for analyzing ambient air |
| CN2255615Y (en) * | 1995-07-24 | 1997-06-04 | 云南省分析测试研究所 | Gas chromatography catalytic tester |
| CN2826429Y (en) * | 2005-08-24 | 2006-10-11 | 安捷伦科技有限公司 | Novel gas chromatographic detector |
| CN200968949Y (en) * | 2006-07-10 | 2007-10-31 | 尹俊荣 | Impulsive discharge helium ionization gas chromatograph |
| CN101105485A (en) * | 2007-08-21 | 2008-01-16 | 昆明贵研金峰科技有限公司 | Catalytic oxidation heat resistance type gas chromatograph |
| 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 |
| CN201096761Y (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 instrument |
| 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 |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE427877B (en) * | 1981-10-23 | 1983-05-09 | Lars Folke Rittfeldt | PROCEDURE OF A GAS CHROMATOGRAPHY FOR CONTINUOUS, AUTOMATIC QUALITATIVE AND QUANTITATIVE AIR ANALYSIS AND DEVICE FOR IMPLEMENTATION OF THE PROCEDURE |
| JPH09184829A (en) * | 1995-12-28 | 1997-07-15 | Shimadzu Corp | Gas chromatograph |
| US7125821B2 (en) * | 2003-09-05 | 2006-10-24 | Exxonmobil Chemical Patents Inc. | Low metal content catalyst compositions and processes for making and using same |
| US8871149B2 (en) * | 2009-04-06 | 2014-10-28 | Thermo Fisher Scientific S.P.A. | Modular gas chromatograph |
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2015
- 2015-07-03 CN CN201510388238.0A patent/CN106324166B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3762878A (en) * | 1971-04-19 | 1973-10-02 | Beckman Instruments Inc | Apparatus for analyzing ambient air |
| CN2255615Y (en) * | 1995-07-24 | 1997-06-04 | 云南省分析测试研究所 | Gas chromatography catalytic tester |
| CN2826429Y (en) * | 2005-08-24 | 2006-10-11 | 安捷伦科技有限公司 | Novel gas chromatographic detector |
| CN200968949Y (en) * | 2006-07-10 | 2007-10-31 | 尹俊荣 | Impulsive discharge helium ionization gas chromatograph |
| CN101105485A (en) * | 2007-08-21 | 2008-01-16 | 昆明贵研金峰科技有限公司 | Catalytic oxidation heat resistance type gas chromatograph |
| 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 |
| CN201096761Y (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 instrument |
| 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 |
Non-Patent Citations (1)
| Title |
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| 便携气相色谱在现场检测中的应用;关亚风 等;《2013现场检测仪器及技术研讨会大会报告及论文》;20131231;第7页 * |
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| CN106324166A (en) | 2017-01-11 |
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