CN1877320A - Minisize chromatographic column box with high precision temperature control system - Google Patents

Minisize chromatographic column box with high precision temperature control system Download PDF

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Publication number
CN1877320A
CN1877320A CN 200510074928 CN200510074928A CN1877320A CN 1877320 A CN1877320 A CN 1877320A CN 200510074928 CN200510074928 CN 200510074928 CN 200510074928 A CN200510074928 A CN 200510074928A CN 1877320 A CN1877320 A CN 1877320A
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temperature control
control system
minisize
heating
chromatographic column
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CN 200510074928
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CN100374859C (en
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张西咸
方向
张颿
陈莲
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Abstract

The invention discloses a micro chromatographic column tank which comprises a tank body, capillary column heating frame set in the tank, capillary column bound around the frame, a heating device set on the inner or outer wall of the cylinder frame, a precise thermo resistor and a temperature control system set out of the tank. The capillary column heating frame employs metal alloy material; the capillary column employs quartz material; the heating device is flexible electrical heating membrane coated on the inner wall of the frame; the temperature control system includes a temperature control module, the precise thermo resistor connects with the signal input terminal of the temperature control module, the output terminal of the temperature control module connects with the insulating single-phase alternative current modulator module of which one end of the output terminal connects with the heating device, and the other end of the output terminal connects with the input power.

Description

A kind of Minisize chromatographic column box with high precision temperature control system
Technical field
The present invention relates to a kind of parts of analytical instrument, specifically, relate to a kind of portable minisize, modular capillary pipe chromatograph box with high-precision temperature control system.
Background technology
The portable minisize chromatograph box is a kind of detecting instrument of working at normal temperatures and pressures, and the heating skeleton of chromatograph box inside adopts metal material to make the capillary column cylinder frame, and capillary column is wrapped on the cylinder frame, by electric heating material capillary column is heated.The temperature sensing that will heat hoop by thermal resistance reaches the purpose of adjusting temperature to temperature-control circuit by its control SSR (solid-state relay) again.
But, because the technical matters of heating material and heater, at present, the maximum operating temperature of traditional portable minisize chromatograph box can only reach 180 ℃~200 ℃, the control circuit of simultaneously traditional portable minisize chromatograph box directly is connected with solid-state relay, temperature-control circuit utilizes the break-make of SSR to reach the purpose (temperature control precision of traditional chromatograph box is at 1 ℃ usually) of adjustment temperature, and this makes and all can't satisfy intimate harsh index request aspect versatility and to many modern analytical techniques application scenario that reappearance is had relatively high expectations.
Summary of the invention
The technical issues that need to address of the present invention just are to overcome in existing traditional miniature chromatograph box application technology temperature and control inexact defective, a kind of novel portable minisize chromatograph box is provided, it has integrated, microminiaturized, general and modularization, the heat-insulating property excellence, lifting/lowering temperature speed is fast, characteristics such as temperature control precision height.
For addressing the above problem, the present invention adopts following technical scheme:
Minisize chromatographic column box with high precision temperature control system of the present invention, comprise casing, be arranged on capillary column heating skeleton and the capillary column that is wrapped on the skeleton in the casing, be arranged in the skeleton or the heating arrangement and the accurate thermal resistance of outer wall, be arranged on the outer temperature control system of casing, described capillary column heating skeleton all adopts the high-temperature insulation material of identical material or synthetic insulating material to make with capillary column, described heating arrangement is to be coated in the skeleton or the electrical-heating film on the outer wall, described temperature control system comprises temperature control modules, the signal input part of accurate thermal resistance and temperature control modules is connected, the temperature control modules output terminal is connected with isolated form single phase ac regulation module, one end of isolated form single phase ac regulation module output terminal is connected with heating arrangement, and the other end of isolated form single phase ac regulation module output terminal connects the input power supply.
High-temperature insulation material of the present invention is any one in quartz glass, glass, enamel, pottery or other high temperature insulating material, is preferably quartz glass.
Heating skeleton of the present invention is cylinder, cylinder or sphere shape, is preferably cylindrical shape, and drum diameter is that 60mm~120mm, cylinder heights are 40mm~100mm, and wall thickness is 0.2mm~6mm.
It is that 1 meter~60 meters, arrangement mode are for closely arranging or being spaced that the utility model capillary column twines total length.
Electrical-heating film of the present invention is the electrical-heating film that semiconductor nano Electric radiant Heating Film, infrared ray electric heating film or flexible electrical heating film maybe can be coated on other type on the skeleton.
Electrical-heating film applied thickness of the present invention is 0.01mm~4mm, and coating method is whole stickup, spraying or evaporation.
Accurate thermal resistance of the present invention adopts platinum resistance temperature measurement element, with vacuum-deposited thin film technique platinum is splashed on the ceramic substrate, fixing with the glass sintering material lead-in wire, make thin-film component through laser resistor trimming again, miniature platinum thermal resistance sensing probe directly is fixed on the quartz glass heating skeleton top layer by the surface-welding technology.
Temperature control modules of the present invention has PID adjusting control, fuzzy control and the self-adaptation adjusting control function of regulating.
Isolated form single phase ac regulation module of the present invention serves as synchronous with the electrical network phase place, when the size that changes Control current is 4~20mA, the inner trigger pulse that just produces 0 °~180 ° of relative line voltages is isolated by photoelectricity, output terminal just triggers corresponding controllable silicon conducting, realizes pressure regulation.
Be provided with a pair of axial control fan and heat-insulation system in the casing of the present invention.Described heat-insulation system adopts the ceramic fiber cotton material, and the high temperature inorganic glue by can be anti-500 ℃ sticks on inwall around the casing with it.
Casing external dimensions of the present invention is high in 80mm~160mm*80mm~160mm*80mm~160mm for the wide * of long *.
Principle of work of the present invention is:
The capillary column cylinder heating skeleton drum diameter 60mm~120mm of chromatograph box of the present invention inside, cylinder heights are 40mm~100mm, wall thickness 0.2mm~6mm, adopting quartz glass is made the capillary column cylinder frame, capillary column is wrapped on the cylinder frame, by being coated in the nano electroheating film on the quartz glass making capillary column cylinder frame, with strong far infrared, accurate heat, magnetic oscillation stack energy, being converted into efficiently, heat energy directly heats the capillary cylinder.To heat the signal input part of the temperature sensing of skeleton by thermal resistance again, adjust control by temperature control modules to temperature control modules.Then, the temperature control modules output terminal changes Control current, makes isolated form single phase ac regulation module trigger corresponding controllable silicon conducting, thereby reaches the purpose of phase-shift voltage regulating, adjustment temperature.Adopt a pair of axial control fan to auxiliary lifting/lowering temperature control technology of pneumatic blending and cabinet insulation material technology simultaneously, thereby realize fast, non-overshoot and precise dose control.
Pedestal of the present invention is a silica glass material, quartz glass is an a kind of special glass that contains the single composition of silicon dioxide, has extremely low thermal expansivity, high temperature tolerance (1100 ℃), fabulous chemical stability, excellent electric insulation, low and stable ultrasonic delay performance, best saturating ultraviolet spectrum performance, saturating visible light and near infrared spectrum performance are higher than the mechanical property of simple glass far away.Its thermal expansivity is little, microminaturization easily.In addition, capillary column also adopts quartz material, so the thermal expansivity of both integral structures is very little, solved problem fully and effectively such as multiple factors such as thermal expansion, the rate of heat addition, thermal uniformity and wide temperature ranges (room temperature~400 ℃).Heating process is capillary chromatographic column to be realized accurately and fast and even the heating by the direct precision of nano electroheating film that is coated on the quartz glass.
Nano electroheating film of the present invention superposes and can be converted into the materializing procedure of heat energy with strong far infrared, accurate heat, magnetic oscillation.So the electric heating conversion efficiency height is than traditional type of heating energy-conservation 30%.Long service life, rationally the serviceability temperature life-span is that resistance wire is more than 5 times.Voltage adaptation wide ranges: 6V~380V (AC/DC) is by adjusting power density, heating-up temperature is set arbitrarily between room temperature~1100 ℃, its thermal efficiency is up to more than 96%, and the working temperature that can make capillary chromatographic column is carried out multistage arbitrarily and set between room temperature~400 ℃.System's serviceability temperature height, geometric configuration are unrestricted.Owing to combine closely in rete and base material (quartz glass) surface, microminaturization and modularization that can implementation structure, characteristics such as have simultaneously that heat radiation is abundant, programming rate is fast, electric heating conversion efficiency is high, homogeneous heating and overall thermal expansion coefficient are little.
Accurate thermal resistance of the present invention adopts platinum resistance temperature measurement element, with vacuum-deposited thin film technique platinum is splashed on the ceramic substrate, fixing with the glass sintering material lead-in wire, make thin-film component through laser resistor trimming again, by the surface-welding technology miniature platinum thermal resistance sensing probe directly is fixed on the heating skeleton top layer, to obtain high measuring accuracy and fast response time.
Temperature controller of the present invention has various control function: PID control, fuzzy control, and self-adaptation is regulated control etc.The present invention controls temperature range room temperature~400 ℃, control accuracy ± 0.1 ℃ (annotate: the control accuracy of traditional miniature chromatograph box only is ± 1 ℃).
Isolated form single phase ac regulation module of the present invention, (4~20mA), the inner trigger pulse that just produces 0 °~180 ° of relative line voltages is isolated by photoelectricity when the size that changes Control current, output terminal just triggers corresponding controllable silicon conducting, thereby reaches the purpose of pressure regulation.
The present invention assists lifting/lowering temperature control fan system, at the problem that often produces toning in multistage falls the temperature programme process fast, utilizes a pair of axial control fan that pneumatic blending is realized the accurate control that temperature is auxiliary.
The heat-insulation system of capillary column case of the present invention adopts the ceramic fiber cotton material, high temperature inorganic glue by can be anti-500 ℃ sticks on inwall around the post case with it, a good temperature environment and insulating power are provided, and this improvement and control effect to integral post oven temperature, degree characteristic is very favourable.
Conventional chromatogram post case external physical dimensions is about 300mm*300mm*300mm (the wide * height of long *), casing external physical dimensions of the present invention is about 80mm~160mm*80mm~160mm*80mm~160mm (the wide * height of long *), reduce box sizes greatly, reached microminiaturized purpose.
The invention has the beneficial effects as follows:
The temperature control model that the present invention adopts reaches 5 rank temperature programmes, utilize temperature control modules control isolated form single phase ac regulation module and auxiliary lifting/lowering temperature control fan part, have that heating is fast with radiating rate, control accuracy is high, temperature overshot is less, especially heating material environmental protection good characteristics such as (environmental protection characteristic of heating material require more and more higher in the world).At the Gneral analysis instrument, especially in Modern Small, field instrumentation and hand-held analyzer device, have purposes and application prospect quite widely, have remarkable economical and social benefit.
Description of drawings
Fig. 1 is the outer heating arrangement synoptic diagram of the embodiment of the invention 1 described skeleton.
Fig. 2 is a heating arrangement synoptic diagram in the embodiment of the invention 2 and the 3 described skeletons.
Among the figure:
1, casing 2, heating arrangement
3, be wrapped in capillary column on the skeleton
4, capillary column heating skeleton 5, accurate thermal resistance
6, temperature control modules 7, isolated form single phase ac regulation module
8, a pair of axial control fan 9, heat-insulation system
Embodiment
Embodiment 1
As shown in Figure 1, Minisize chromatographic column box with high precision temperature control system of the present invention, comprise casing 1, the casing external dimensions is high in 80mm*80mm*80mm for the wide * of long *, be arranged on capillary column cylinder heating skeleton 4 and the capillary column 3 that is wrapped on the cylinder skeleton in the casing, be arranged on heating arrangement 2 and the accurate thermal resistance 5 and the temperature control modules 6 of cylinder skeleton outer wall.Described capillary column cylinder heating skeleton and the equal adopting quartz glass of capillary column are made, and described heating skeleton body diameter is 60mm, and it is that 1 meter, arrangement mode are for closely arranging that capillary column twines total length.Described heating arrangement is the semiconductor nano Electric radiant Heating Film that is coated on the cylinder skeleton outer wall, and described electrical-heating film applied thickness is 0.01mm, and coating method is an evaporation.Described accurate thermal resistance adopts platinum resistance temperature measurement element, with vacuum-deposited thin film technique platinum is splashed on the ceramic substrate, fixing with the glass sintering material lead-in wire, make thin-film component through laser resistor trimming again, miniature platinum thermal resistance sensing probe directly is fixed on the quartz glass heating skeleton top layer by the surface-welding technology.The signal input part of accurate thermal resistance and temperature control modules is connected, the temperature control modules output terminal is connected with isolated form single phase ac regulation module 7, one end of isolated form single phase ac regulation module output terminal is connected with heating arrangement, and the other end of isolated form single phase ac regulation module output terminal connects the input power supply.
Temperature control modules of the present invention has PID and regulates control, fuzzy control and self-adaptation adjusting control function.
Isolated form single phase ac regulation module of the present invention serves as synchronous with the electrical network phase place, (4~20mA), the inner trigger pulse that just produces 0 °~180 ° of relative line voltages is isolated by photoelectricity when the size that changes Control current, output terminal just triggers corresponding controllable silicon conducting, realizes pressure regulation.
Be provided with a pair of axial control fan 8 and heat-insulation system 9 in the casing of the present invention.Described heat-insulation system adopts the ceramic fiber cotton material, and the high temperature inorganic glue by can be anti-500 ℃ sticks on inwall around the casing with it.
Embodiment 2
As shown in Figure 2, Minisize chromatographic column box with high precision temperature control system of the present invention, comprise casing 1, the casing external dimensions is high in 160mm*160mm*160mm for the wide * of long *, be arranged on capillary column cylindrical shape heating skeleton 2 and the capillary column 3 that is wrapped on the skeleton in the casing, be arranged on heating arrangement 4 and the accurate thermal resistance 5 and the temperature control modules 6 of inboard wall of skeleton.Described capillary column heating skeleton and capillary column all adopt glass to make, and the drum diameter of described heating skeleton is that 120mm, cylinder heights are 100mm, and it is that 60 meters, arrangement mode are for being spaced that wall thickness 4mm, capillary column twine total length.Described heating arrangement is the infrared ray electric heating film that is coated on the cylinder frame inwall, and described electrical-heating film applied thickness is 0.1mm, and coating method is spraying.Described accurate thermal resistance adopts platinum resistance temperature measurement element, with vacuum-deposited thin film technique platinum is splashed on the ceramic substrate, fixing with the glass sintering material lead-in wire, make thin-film component through laser resistor trimming again, miniature platinum thermal resistance sensing probe directly is fixed on the heating skeleton top layer by the surface-welding technology.The signal input part of accurate thermal resistance and temperature control modules is connected, the temperature control modules output terminal is connected with isolated form single phase ac regulation module 7, one end of isolated form single phase ac regulation module output terminal is connected with heating arrangement, and the other end of isolated form single phase ac regulation module output terminal connects the input power supply.
Temperature control modules of the present invention has PID and regulates control, fuzzy control and self-adaptation adjusting control function.
Isolated form single phase ac regulation module of the present invention serves as synchronous with the electrical network phase place, (4~20mA), the inner trigger pulse that just produces 0 °~180 ° of relative line voltages is isolated by photoelectricity when the size that changes Control current, output terminal just triggers corresponding controllable silicon conducting, realizes pressure regulation.
Be provided with a pair of axial control fan 8 and heat-insulation system 9 in the casing of the present invention.Described heat-insulation system adopts the ceramic fiber cotton material, and the high temperature inorganic glue by can be anti-500 ℃ sticks on inwall around the casing with it.
Embodiment 3
As shown in Figure 2, Minisize chromatographic column box with high precision temperature control system of the present invention, comprise casing 1, the casing external dimensions is high in 120mm*120mm*120mm for the wide * of long *, be arranged on capillary column cylindrical shape heating skeleton 2 and the capillary column 3 that is wrapped on the skeleton in the casing, be arranged on heating arrangement 4 and the accurate thermal resistance 5 and the temperature control modules 6 of inboard wall of skeleton.Described capillary column heating skeleton and capillary column all adopt enamel to make, and the drum diameter of described heating skeleton is that 100mm, cylinder heights are 60mm, and it is that 10 meters, arrangement mode are for being spaced that wall thickness 6mm, capillary column twine total length.Described heating arrangement is the flexible electrical heating film that is coated on the inboard wall of skeleton, and described electrical-heating film applied thickness is 4mm, and coating method is whole the stickup.Described accurate thermal resistance adopts platinum resistance temperature measurement element, with vacuum-deposited thin film technique platinum is splashed on the ceramic substrate, fixing with the glass sintering material lead-in wire, make thin-film component through laser resistor trimming again, miniature platinum thermal resistance sensing probe directly is fixed on the heating skeleton top layer by the surface-welding technology.The signal input part of accurate thermal resistance and temperature control modules is connected, the temperature control modules output terminal is connected with isolated form single phase ac regulation module 7, one end of isolated form single phase ac regulation module output terminal is connected with heating arrangement, and the other end of isolated form single phase ac regulation module output terminal connects the input power supply.
Temperature control modules of the present invention has PID and regulates control, fuzzy control and self-adaptation adjusting control function.
Isolated form single phase ac regulation module of the present invention serves as synchronous with the electrical network phase place, (4~20mA), the inner trigger pulse that just produces 0 °~180 ° of relative line voltages is isolated by photoelectricity when the size that changes Control current, output terminal just triggers corresponding controllable silicon conducting, realizes pressure regulation.
Be provided with a pair of axial control fan 8 and heat-insulation system 9 in the casing of the present invention.Described heat-insulation system adopts the ceramic fiber cotton material, and the high temperature inorganic glue by can be anti-500 ℃ sticks on inwall around the casing with it.

Claims (14)

1, a kind of Minisize chromatographic column box with high precision temperature control system, comprise casing, be arranged on capillary column heating skeleton and the capillary column that is wrapped on the skeleton in the casing, be arranged in the skeleton or the heating arrangement and the accurate thermal resistance of outer wall, be arranged on the outer temperature control system of casing, it is characterized in that described capillary column heating skeleton all adopts the high-temperature insulation material of identical material or synthetic insulating material to make with capillary column, described heating arrangement is to be coated in the skeleton or the electrical-heating film on the outer wall, described temperature control system comprises temperature control modules, the signal input part of accurate thermal resistance and temperature control modules is connected, the temperature control modules output terminal is connected with isolated form single phase ac regulation module, one end of isolated form single phase ac regulation module output terminal is connected with heating arrangement, and the other end of isolated form single phase ac regulation module output terminal connects the input power supply.
2, Minisize chromatographic column box with high precision temperature control system as claimed in claim 1 is characterized in that: described high-temperature insulation material is any one in quartz glass, glass, enamel, pottery or other high temperature insulating material.
3, Minisize chromatographic column box with high precision temperature control system as claimed in claim 2 is characterized in that: described high-temperature insulation material is a quartz glass.
4, as the arbitrary described Minisize chromatographic column box with high precision temperature control system of claim 1-3, it is characterized in that: described heating skeleton is cylinder, cylinder or sphere shape.
5, Minisize chromatographic column box with high precision temperature control system as claimed in claim 4 is characterized in that: described heating skeleton is a cylindrical shape, and drum diameter 60mm~120mm, cylinder heights are 40mm~100mm, wall thickness 0.2mm~6mm.
6, as the arbitrary described Minisize chromatographic column box with high precision temperature control system of claim 1-5, it is characterized in that: it is that 1 meter~60 meters, arrangement mode are for closely arranging or being spaced that capillary column twines total length.
7, Minisize chromatographic column box with high precision temperature control system as claimed in claim 1 is characterized in that: described electrical-heating film is the electrical-heating film that semiconductor nano Electric radiant Heating Film, infrared ray electric heating film or flexible electrical heating film maybe can be coated on other type on the skeleton.
8, Minisize chromatographic column box with high precision temperature control system as claimed in claim 7 is characterized in that: described electrical-heating film applied thickness is 0.01mm~4mm, and coating method is whole stickup, spraying or evaporation.
9, Minisize chromatographic column box with high precision temperature control system as claimed in claim 1, it is characterized in that: described accurate thermal resistance adopts platinum resistance temperature measurement element, with vacuum-deposited thin film technique platinum is splashed on the ceramic substrate, fixing with the glass sintering material lead-in wire, make thin-film component through laser resistor trimming again, miniature platinum thermal resistance sensing probe directly is fixed on the heating skeleton top layer by the surface-welding technology.
10, Minisize chromatographic column box with high precision temperature control system as claimed in claim 1 is characterized in that: described temperature control modules has PID adjusting control, fuzzy control and the self-adaptation adjusting control function of regulating.
11, as the arbitrary described Minisize chromatographic column box with high precision temperature control system of claim 1-10, it is characterized in that: described isolated form single phase ac regulation module serves as synchronous with the electrical network phase place, when the size that changes Control current is 4~20mA, the inner trigger pulse that just produces 0 °~180 ° of relative line voltages, isolate by photoelectricity, output terminal just triggers corresponding controllable silicon conducting, realizes pressure regulation.
12, as the arbitrary described Minisize chromatographic column box with high precision temperature control system of claim 1-11, it is characterized in that: be provided with a pair of axial control fan and heat-insulation system in the described casing.
13, Minisize chromatographic column box with high precision temperature control system as claimed in claim 12 is characterized in that: described heat-insulation system adopts the ceramic fiber cotton material, and the high temperature inorganic glue by can be anti-500 ℃ sticks on inwall around the casing with it.
14, as the arbitrary described Minisize chromatographic column box with high precision temperature control system of claim 1-13, it is characterized in that: described casing external dimensions is high in 80mm~160mm*80mm~160mm*80mm~160mm for the wide * of long *.
CNB2005100749285A 2005-06-06 2005-06-06 Minisize chromatographic column box with high precision temperature control system Expired - Fee Related CN100374859C (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104034831A (en) * 2014-06-08 2014-09-10 华东理工大学 Super-long protein and polypeptide separation capillary liquid chromatography column system with automatic temperature control
CN104407080A (en) * 2014-12-08 2015-03-11 同方威视技术股份有限公司 Portable gas chromatographic capillary column module
CN106706817A (en) * 2017-03-15 2017-05-24 厦门宜柱科技有限公司 Capillary liquid chromatographic column temperature control device

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2116215U (en) * 1992-03-24 1992-09-16 上海市徐汇区中心医院 Liquid phase chromatograph column constant temperature cabinet
JP2000111536A (en) * 1998-09-30 2000-04-21 Shimadzu Corp Column oven for liquid chromatograph
US6093921A (en) * 1999-03-04 2000-07-25 Mt Systems, Llc Microwave heating apparatus for gas chromatographic columns
CN2515675Y (en) * 2001-03-22 2002-10-09 海城市石油化工仪器厂 Ring chromatographic column box
JP4188206B2 (en) * 2003-11-04 2008-11-26 株式会社日立ハイテクノロジーズ Column oven for liquid chromatography

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104034831A (en) * 2014-06-08 2014-09-10 华东理工大学 Super-long protein and polypeptide separation capillary liquid chromatography column system with automatic temperature control
CN104034831B (en) * 2014-06-08 2016-03-30 华东理工大学 Overlength protein with temp auto-controlled, peptide separation capillary liquid chromatographic column system
CN104407080A (en) * 2014-12-08 2015-03-11 同方威视技术股份有限公司 Portable gas chromatographic capillary column module
CN104407080B (en) * 2014-12-08 2017-06-27 同方威视技术股份有限公司 portable gas chromatography capillary column module
CN106706817A (en) * 2017-03-15 2017-05-24 厦门宜柱科技有限公司 Capillary liquid chromatographic column temperature control device

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