CN204855466U - Dull and stereotyped directly -heated type chromatographic column temperature modulating device - Google Patents
Dull and stereotyped directly -heated type chromatographic column temperature modulating device Download PDFInfo
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- CN204855466U CN204855466U CN201520617247.8U CN201520617247U CN204855466U CN 204855466 U CN204855466 U CN 204855466U CN 201520617247 U CN201520617247 U CN 201520617247U CN 204855466 U CN204855466 U CN 204855466U
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Abstract
The utility model discloses a dull and stereotyped directly -heated type chromatographic column temperature modulating device one includes that disc preforming no. 1, disc preforming no. 2, chromatographic column no. 1, chromatographic column no. 2, gasket no. 1, gasket no. 2, rigidity heat conduction are dull and stereotyped one, rigidity heat conduction is dull and stereotyped one, dull and stereotyped heating plate and fixed screw, dull and stereotyped heating plate is by the dull and stereotyped centre gripping of rigidity heat conduction dull and stereotyped one and rigidity heat conduction, and the surface of snail line structure and accurate laminating, rigidity heat conduction dull and stereotyped one dull and stereotyped one in rigidity heat conduction is respectively coiled into to chromatographic column no. 1, chromatographic column no. 2, and surface dull and stereotyped in rigidity heat conduction, rigidity heat conduction dull and stereotyped one is pressed respectively with chromatographic column no. 1, chromatographic column no. 2 to disc preforming no. 1, disc preforming no. 2, the utility model discloses guarantee the temperature modularity can the circumstances under, can effectively improve the production efficiency of chromatographic column module, improved the maintainability of module greatly, small, caloic is hanged down, low cost, do not restrict the maximum operation (service) temperature of chromatographic column, ability used repeatedly reduces the wasting of resources, and production efficiency is high.
Description
Technical field
This patent relates to gas chromatograph chromatogram column temperature modulating device, particularly relate to a kind of low thermal mass, heating rate fast, be suitable for automated production, detachable reusable gas chromatographic column temperature modulation device, be specially a kind of dull and stereotyped Direct-heating column temperature modulation device.
Background technology
Gas chromatography is a kind of for separating of, the component of detection of complex organic compound and the measurement means of content thereof, has separating power strong, highly sensitive, the feature that reproducible reliability is high.Especially for character and similar organic compound thereof, as isomers etc., vapor-phase chromatography can be utilized its effective Isolation and Identification.Vapor-phase chromatography may be used for analytical gas, or boiling point within the specific limits, and has the liquid or solid sample of certain thermal stability.In view of the versatility of vapor-phase chromatography, gas chromatograph is widely used in petrochemical complex in recent years, environmental protection, the fields such as forensic identification food security and occupational health.
Gas chromatograph is generally made up of injection port, chromatographic column and detecting device.In analytic process, the blend sample first will analyzed is imported by injection port.Sample, after injection port heating and gasifying, is promoted to enter in gas chromatographic column by the continuous flow (being called carrier gas) that flow is controlled.Gas chromatographic column is normally by hollow pipelines of making of inert material such as stainless steel or quartz and form by being filled in channel interior (being called chromatography column) or being deposited on the chemisorbed material that tube wall (is called capillary chromatograph).Research finds, be mixed with the carrier gas (being called mobile phase) of gasification sample when flowing in chromatographic column, there is fine distinction in sorbing material (being called Stationary liquid) the interactional molecular force in different organic compound and chromatographic column, result in different organic compound flowing velocity in the chromatography column different, finally cause different organic compound component to flow out the time difference of chromatographic column end.The discriminating to its composition just can be realized according to the time of component outflow.Suction-operated between Stationary liquid and mobile phase, except the chemical property of the molecular structure and Stationary liquid that depend on organic compound, is more subject to the flow velocity of mobile phase, especially the temperature impact of chromatographic column.
In fact, theoretical research and the practice of gas chromatography all show, in detachment process, the temperature control precision of chromatographic column not only directly can affect gas chromatograph accuracy qualitatively and repeatability, and can affect the separating power of chromatographic column.Based on this discovery, a kind of method based on modulating chromatogram column temperature in analytic process is widely used in gas chromatography exploitation and optimizing process.Researchist, for different application, utilizes constant temperature, linear temperature increase, multi order linear to heat up, the various temperature modulator approaches such as non-linear intensification, can greatly improve chromatographic resolution efficiency, and effectively can shorten analysis time.Especially adopting is the modulator approach adopting temperature programme, and can make analysis speed lifting at double, and programming rate is faster, analytical cycle is shorter.These advantages all make chromatogram column temperature modulator approach be called one of main trend that current gas chromatographic technique develops.And the core realizing these chromatogram column temperature modulator approaches is exactly temperature is adjusted to the design of device.
In traditional gas chromatograph, the temperature of chromatographic column controls to rely on air bath chromatographic column incubator to realize.As RobertL describes in United States Patent (USP) 4420679, air bath chromatographic column incubator is casing chromatographic column being put into surrounding parcel insulation material, also secures the electric fan for stirring air and the heater strip around flabellum in casing.In analytic process, it is inner to whole chromatograph box that the air heated by heater strip is stirred fan forced convection, realizes the homogeneous heating to chromatographic column.Although be the comparatively uniform chromatographic column type of heating of one, the efficiency of heating surface of the design of air bath column oven is lower.Common air bath column oven is heated to the power consumption of 350 ~ 400 DEG C between 1500W ~ 2000W, and its highest heating rate is less than 90 DEG C/min usually.And for chromatographic column itself heating useful power less than 1/10.Because a large amount of power is wasted, in order to prevent the excessive instrument internal temperature that causes of column oven heat radiation too high, a large amount of insulation materials must be used to completely cut off high temperature.This makes again the chromatographic volume and weight of conventional gas-phase greatly increase.The restriction of power consumption and volume not only improves traditional chromatographic use cost, the more important thing is and limits the application of gas chromatography in traverse measurement and industrial on-line monitoring.Because no matter be for the battery powered portable instrument of employing, being arranged on the vehicle-mounted instrument measured in car still needs to install in the wild, and the on-line monitoring equipment of work in 7X24 hour, huge power consumption and volume all limit traditional chromatographic applicability.
Engineers starts the chromatogram column temperature modulator approach of seeking other.1989, US Patent No. 5006399 proposes increased the conductive resistance coating of one deck at chromatographic column outside surface, realized the temperature modulation to chromatogram column temperature by the electric current of controlled loading on resistance coating.Although such structure makes the power consumption needed for heating chromatographic column greatly reduce, its Problems existing is also apparent.First, the difficulty of resistive layer is evenly plated at the chromatographic column skin of the long 5 ~ 30m of external diameter 0.5mm higher.Secondly because coating is comparatively fragile, in winding, install and in seal process, be easy to local failure resistive layer.Uneven along the power density in chromatogram column length direction when the unevenness of coating and local damage can make to heat, thus make non-uniform temperature, local temperature can be caused when even more serious too high, burn chromatographic column.Complicated plating process, high cost of manufacture and low robustness limit the application of this technology.
The people such as Mustacich in 1998 propose a kind of by heater strip in US Patent No. 6209386, sensor sleeve together penetrate the chromatographic column heating arrangement in a contractile sleeve pipe after insulating sleeve with chromatographic column.This structure directly contacts conduction by heater strip and chromatographic column and realizes heat trnasfer, but in order to ensure heating uniformity, must the strict gap controlling heater strip sensor and insulating sleeve, and and chromatographic column between gap.And too small gap causes this structure to be difficult to penetrate longer chromatographic column, the application scenario of the chromatographic column using below 5m length usually can only be used for.And this structure cannot be used for more general 30m chromatographic column.In order to improve this defect, calendar year 2001, the people such as Mustacich are in US Patent No. 6682699, propose a kind of by after heater strip ceramic fiber line winding insulation, direct and chromatographic column, thermometric platinum resistance silk are closely wound in wire harness, again wire harness is coiled into toroid winding, and with aluminium foil or tinfoil parcel, improves temperature homogeneity.Although this invention power consumption compared with the design of resistance coating slightly increases, there is significant decline compared with traditional colour chromatographic column box.Its heating rate can reach >600 DEG C/min, can effectively shorten the chromatographic resolution time, and greatly reduces the length restriction of chromatographic column.But this structure also proposes higher requirement to manufacture craft, first when being wound around non-conductive fibre line, must ensure that all heater strip surfaces are all covered by single, otherwise can short circuit be produced; Secondly, in order to insulate, chromatographic column itself can only adopt quartz material, and the fragility of quartz wool buttress shaft makes easily fracture when being wound around with heater strip or produce higher stress.When chromatographic column heats, stress aggravation can cause chromatographic column to rupture.This defect is particularly outstanding when using length to be greater than the chromatographic column of more than 20m.These strict processing technologys require to cause producing this chromatogram column temperature modulation module needs the production equipment of complex and expensive and the higher personnel of professional ability.In addition, from its usage economy, this integrated design also makes customer using cost high, because when the importing of chromatographic column or the careless fracture of outflow end, or Sample introduction end is subject to (these situations are more common when chromatograph uses) when pollution needs to amputate, current chromatographic column module can only be scrapped, use new chromatographic column.Because integral structure cannot support the chromatographic column wound to extract again.Complicated manufacture craft and high use cost make the chromatogram temperature modulation module of this structure can only be applicable to limited application scenario.
2006, Roques proposed a kind of new flat heater structure in US Patent No. 75l3936.Its principle is side chromatographic column being arranged in flat heater sheet according to the mode individual layer of snail line, then chromatographic column, heating plate to be forced together maintenance close contact with compressing tablet.Owing to adopting the conduction pattern heating of close contact, the heat that flat heater sheet produces directly effectively is delivered in chromatographic column.And the main feature of this structure larger simplifies Direct-heating column heating arrangement, makes processing and manufacturing cost decrease, the larger lifting of robustness.Due to heating surface (area) (HS Relatively centralized, caloic is relatively little, the power of about 90W can realize 300 DEG C/min heating rate in like fashion.But when practical application, this design still also exists certain defect.First, in order to the quartzy chromatographic column of fragility is arranged in snail line mode, need to use resistant to elevated temperatures silicon-based adhesive to be coated in the surface of heating plate or rigidity conducting strip, then arrange chromatographic column to manually.Such technique makes chromatographic column production efficiency lower, especially concerning long chromatographic column, coils inefficiency by hand.Be example with the chromatographic column of the most frequently used long 30m, external diameter 0.5mm, calculate with minimum bending radius 30mm, chromatographic column needs around about 90 circles, and the diameter of heating plate need reach 150mm.And make the maximum heating temperature of chromatographic column be subject to the restriction of the use maximum temperature of bonding agent owing to have employed silicon-based adhesive.And from the angle of operation and maintenance, this structure still belongs to single use design, after namely chromatographic column assembles, cannot continue use because reason amputation port local such as fracture or pollutions.And after arriving chromatographic column serviceable life, chromatographic column also cannot disassemble, and can only abandon whole heating arrangement.
Scan existing chromatogram column temperature modulation system, directly to chromatographic column heating, to have efficiency high, low in energy consumption to adopt heat exchange pattern, response rapidly and volume and weight also can significantly reduce, be the development trend of chromatogram column temperature modulation technique.But just current direct heating technique and structure all exist, complex manufacturing technology, need manual operations, one definite limitation is existed to chromatogram column length, heating arrangement integrated design, defects such as can not adjusting and reuse, therefore, need a kind of keep the prerequisite of existing performance under, more applicable produce, safeguard and use structural design.
Utility model content
The purpose of this utility model is to solve the direct heating technique of existing spectrum column temperature modulating device and structure all exists, complex manufacturing technology, needs manual operations, there is a definite limitation to chromatogram column length, heating arrangement integrated design, defect defects such as can not adjusting and reuse.Mainly solve following problem:
First, current flat heater structure, need to be bonded in chromatographic column to keep snail wire shaped on heated plate with silicon-based adhesive, but be less than 260 DEG C because of existing silicon-based adhesive maximum operation (service) temperature, too high temperature can cause adhesive failure and can send poisonous and harmful substance.Thus the maximum operation (service) temperature of chromatographic column is limited.
Secondly, when reality uses, user is often amputated the chromatographic column of certain length because portion of chromatographic column importing end office (EO) pollutes from port, then continue to use remaining chromatographic column, this can extend chromatographic column serviceable life and after current flat panel formula directly-heated chromatographic column adhesives chromatographic column, again chromatographic column cannot be taken off from heated plate, so after the exit of chromatographic column accidentally ruptures or polluted, whole chromatographic column heating arrangement can only be replaced.Cause shorten serviceable life.Even and if after chromatographic column normally uses the life-span, although the life-span of heating arrangement much larger than the life-span of chromatographic column, still need chromatographic column to abandon together with heating module, cannot reuse, cause the wasting of resources, use cost significantly increases.
Again, existing dull and stereotyped directly-heated chromatographic column module, in manufacturing process, for ensureing that chromatographic column can the mode of single flat surface helix line arrange, needs to adopt manual alignment chromatographic column.If to typical 30m chromatographic column, coiling 90 is needed to enclose.Adopt manual arrangement significantly will increase the production cycle, have a strong impact on production efficiency, and be difficult to effective Mass Control, finally cause cost of goods manifactured high.
Finally, the heat dissipation of heating arrangement, for flat heating arrangement, the surface area positive correlation of the dissipation of its evenly heat and heating region.With current design, for after the chromatographic column coiling that 30m is long, the diameter of required heating region is greater than 150mm, and the long chromatographic column of 60m is needed for some particular application, the diameter of heating region is needed to be greater than 250mm, although 60% of diameter increase, can cooling surface area increases by 3 times, average power dissipation is caused why to add 3 times.Therefore current design ap-plication is when long chromatographic column and speciality chromatographic column, and the feature of its low-power consumption will be no longer outstanding.
The utility model adopts following technical scheme:
A kind of dull and stereotyped Direct-heating column temperature modulation device, comprises plate-like compressing tablet one, plate-like compressing tablet two, chromatographic column one, chromatographic column two, pad one, pad two, rigidity heat conduction flat board one, rigidity heat conduction flat board one, flat heater sheet and fixed screw, plate-like compressing tablet one is identical with plate-like compressing tablet two, chromatographic column one is identical with chromatographic column two, pad one is identical with pad two, rigidity heat conduction dull and stereotyped one is identical with rigidity heat conduction flat board one, described flat heater sheet is clamped by rigidity heat conduction dull and stereotyped one and rigidity heat conduction dull and stereotyped one, chromatographic column one, chromatographic column two is coiled into snail line structure and precision is fitted in rigidity heat conduction flat board one respectively, the surface of rigidity heat conduction flat board one, plate-like compressing tablet one, plate-like compressing tablet two is by chromatographic column one, chromatographic column two is pressed in rigidity heat conduction flat board one respectively, the surface of rigidity heat conduction flat board one, inserts pad one between plate-like compressing tablet one and rigidity heat conduction flat board one, inserts pad two, plate-like compressing tablet one between plate-like compressing tablet two and rigidity heat conduction flat board one, plate-like compressing tablet two is fixedly connected with up and down by fixed screw, described plate-like compressing tablet one, plate-like compressing tablet two axially connects elastic card claw with elastic connection way.
Described rigidity heat conduction flat board one, rigidity heat conduction flat board one by metal material, as copper, aluminium, stainless steel etc. are made, both can ensure its rigidity and flatness, simultaneously also can the temperature of the homogenize area of heating surface, promote the homogeneity of heating.Described flat heater sheet can be the flexible heater sheet adopting printed circuit technique to make, the mica heating plate produced as polyimide flex heating plate, silicon rubber flexible heater sheet or employing rigid plane heating technique or ceramic heating flake, it is thin that flexible heater sheet has thickness, adapt to arbitrary surfaces, and the features such as simple installation, but by the restriction of encapsulating material, serviceability temperature can not more than 250 DEG C.And rigidity heating plate has high temperature resistant, that output power is high feature, but regular surfaces can only be applied to.Mica heating plate can long-term work below 400 DEG C, and output power density can reach 17W/cm
2.
When rigidity heat conduction flat board one, rigidity heat conduction flat board one are by heating, heat is transferred in chromatographic column one, chromatographic column two by the mode of conduction.Because when rigidity heat conduction flat board one, the dull and stereotyped heating of rigidity heat conduction, two surperficial power densities and coefficient of heat conductivity are identical, although so chromatographic column one, chromatographic column two are fitted in respectively the both sides up and down of flat heater sheet, heat transfer condition and heating power are identical substantially.Chromatographic column one, chromatographic column two can be two independently chromatographic columns, the analytical applications that two root chromatogram columns of can satisfying the demand heat simultaneously, such as binary channels parallel parsing, the analytical column that mariages TCD detecting device needs and reference column heating etc.; Also can be a root chromatogram column, its center partially passes through rigidity heat conduction flat board one, the fluting at rigidity heat conduction dull and stereotyped one and dull and stereotyped heating plate center links together, the analytical applications of longer (30m-60m) chromatographic column of can satisfying the demand like this.
In order to keep chromatographic column to be fitted on rigidity heat conduction flat board one, rigidity heat conduction flat board one with the mode precision of snail line when being wound around chromatographic column and using, plate-like compressing tablet one, plate-like compressing tablet two is adopted chromatographic column one, chromatographic column two to be pressed in respectively the surface of rigidity heat conduction flat board one, rigidity heat conduction flat board one.But because mostly chromatographic column is to be made up of quartz material, thickness of column 0.1mm-0.2mm, pressure is crossed conference and is caused chromatographic column cracked.Thus plate-like compressing tablet one, plate-like compressing tablet two have annular projection, such plate-like compressing tablet plate-like compressing tablet constitutes the space of a ring-type between, plate-like compressing tablet two and rigidity heat conduction flat board one, rigidity heat conduction flat board one, its height is consistent with chromatographic column external diameter, thus avoids and cause chromatographic column to be out of shape cracked situation because coupling mechanism force is excessive.And in order to adapt to the chromatographic column of different-diameter, between plate-like compressing tablet one and rigidity heat conduction flat board one, insert pad one, between plate-like compressing tablet two and rigidity heat conduction flat board one, insert pad two.This device can be made by adjustment pad to be applicable to the chromatographic column of various outer diameter once the thickness of, pad two.Plate-like compressing tablet one, plate-like compressing tablet two can be symmetrical the both sides being arranged on flat heater sheet, so just can realize double-deck chromatographic column and be wound with.
Described elastic card claw comprises shell fragment, spacing claw and guiding bead, described shell fragment, by stamped metal sheets between spacing claw and guiding bead, mold injection integral type connects, also by riveted joint, screw welding, glued joint and interference fit connection, spacing claw and rigidity heat conduction flat board one, gap between rigidity heat conduction flat board one is less than chromatographic column one respectively, the diameter of chromatographic column two, and the displacement of the maximum flexibility that elastic card claw can realize is less than chromatographic column one, the diameter of chromatographic column two, the guiding bead of circular conical surface or arc-shaped surface is adopted to be used for chromatographic column one, lead when chromatographic column two is wound around and prevent chromatographic column one, chromatographic column two is composed post and is scratched.
Plate-like compressing tablet one, plate-like compressing tablet two limit chromatographic column one, chromatographic column two in the motion of axis direction, and the motion of chromatographic column radial direction is limited by elastic card claw.Described plate-like compressing tablet one, plate-like compressing tablet two axially connect elastic card claw with elastic connection way, can move in axis direction certain limit.Elastic card claw and plate-like compressing tablet one, plate-like compressing tablet two integrally process, and the shape of adjustment junction can reduce the rigidity of elastic card claw, realizes the regime of elastic deformation met the demands.Under normal installed condition, gap between spacing claw and rigidity heat conduction flat board one, rigidity heat conduction flat board one is less than the diameter of chromatographic column one, chromatographic column two respectively, and the displacement of the maximum flexibility that elastic card claw can realize is greater than the diameter being less than chromatographic column one, chromatographic column two, when needs are wound around chromatographic column, the power needed for winding can make chromatographic column jack-up elastic card claw.After chromatographic column is passed through, elastic card claw can set back.Now, the radial displacement of chromatographic column has limited with regard to limited claw.Different with quantity according to the distribution of elastic card claw, chromatographic column often around a circle, at least will pass through an elastic card claw.Because the gap of elastic card claw and rigidity heat conduction flat board should be substantially suitable with column diameter, so need guide piece when being wound around, when not damaging chromatographic column face coat, auxiliary chromatographic column slips in annular gap smoothly.The utility model adopts the guiding bead of circular conical surface or arc-shaped surface when being wound around chromatographic column, can being that chromatographic column effectively avoids sharp edge, preventing chromatographic column from scratching.
Use plate-like compressing tablet one, plate-like compressing tablet two and elastic card claw stationary chromatographic post, not only achieve chromatographic column dull and stereotyped with the rigidity heat conduction of fitting of snail line mode, this canoe of what is more important is reversible, and namely user can locally amputate according to actual needs or all replace chromatographic column.The column oven that the Direct-heating column heating arrangement that this advantage makes this utility model provide adopts with traditional experiment room equipment has identical dirigibility in chromatographic column use.
Described chromatographic column one, chromatographic column two can adopt individual layer to twine the mode of mode or Double wound.The utility model is applied to the canoe of the chromatographic column of different length.When the chromatographic column of required winding is shorter, individual layer can be adopted to twine mode, winding of single layer mode is side chromatographic column one being coiled in flat heater sheet, and make chromatographic column be fitted on rigidity heat conduction flat board one with a plate-like compressing tablet one, and at the opposite side of flat heater sheet, in order to reduce power dissipation and environmental temperature fluctuation to the impact of temperature control, adopting heat-insulation layer compressing tablet, insulation material being covered on rigidity heat conduction flat board one.When the longer chromatographic column of use one or two independently chromatographic column time, then need the mode adopting Double wound.Now, plate-like compressing tablet one, plate-like compressing tablet two is needed to use chromatographic column one, chromatographic column two to be fixed on the both sides of flat heater sheet.When the chromatographic column that winding one is longer, pass, then respectively from center to edge coiling chromatographic column in the circular hole needing just chromatographic column one, chromatographic column two to process in advance from rigidity heat conduction flat board one, rigidity heat conduction dull and stereotyped one and dull and stereotyped heating plate or annular groove.And when coiling two independently chromatographic column time, the chromatographic column of both sides can independent coiling.Experiment shows, the chromatographic column of heating equal length, adopts bilayer arrangement mode lower than the average power consumption of individual layer arrangement mode by more than 40%.
The manufacturing process of the apparatus structure of automatic winding chromatographic column is: with round orifices orientation, and chromatographic column heating arrangement is fixed on rotating driving device, the axis of circular hole and rotation axis coincident.Alignment device is placed in helix tangential direction, is in same plane with helix.First chromatographic column is wrapped on chromatographic column heating arrangement through alignment device.That chromatographic column by alignment device, through the guiding of the bead that leads, will touch elastic card claw when rotating driving device rotates.Regulating guiding bead can produce certain tensile force, making chromatographic column successfully by elastic card claw jack-up, can finally slip into the gap between plate-like compressing tablet and rigidity heat-conducting plate flat board when being wound around.The pre-tensioning regulating guiding bead to produce can also tighten up chromatographic column when being wound around, and makes it tight coiling, very close to each other.
The beneficial effects of the utility model:
The utility model (1), when ensureing temperature modulation performance, effectively can improve the production efficiency of chromatographic column module, substantially increase the maintainability of module; (2) volume is little, caloic is low, with low cost; (3) maximum operation (service) temperature of chromatographic column is not limited; (4) can reuse, reduce the wasting of resources, use cost significantly reduces, and production efficiency is high.
Accompanying drawing explanation
Fig. 1 is the wiring layout of described dull and stereotyped Direct-heating column temperature modulation device;
Fig. 2 is the explosive view of described dull and stereotyped Direct-heating column temperature modulation device;
Fig. 3 is described plate-like compressing tablet and elastic card claw connection layout
Fig. 4 is described elastic card claw structural drawing;
The fundamental diagram of elastic card claw when Fig. 5 is described winding chromatographic column;
Fig. 6 is the single flat surface helix line arrangement architecture figure of described chromatographic column;
Fig. 7 is the double layer planar helical row structural drawing of described chromatographic column;
Fig. 8 is the structure of automatic winding chromatographic column;
Fig. 9 is long to 30m with the speed of 100 DEG C/min, and the interior chromatographic column through 0.25mm carries out the chromatogram that temperature modulation obtains;
Figure 10 is long to 30m with the speed of 400 DEG C/min, and the interior chromatographic column through 0.25mm carries out the chromatogram that temperature modulation obtains.
Description of reference numerals
1 plate-like compressing tablet one; 2 plate-like compressing tablets two; 3 chromatographic columns one; 4 chromatographic columns two; 5 pads one; 6 pads two; 7 rigidity heat conduction flat boards one; 8 rigidity heat conduction flat boards one; 9 flat heater sheets; 10 fixed screws; 11 elastic card claws; 12 shell fragments; 13; Spacing claw; 14 guiding beads; 15 heat-insulation layer compressing tablets; 16 insulation materials; 17 circular holes; 18 alignment devices
Embodiment
The utility model is further illustrated below in conjunction with accompanying drawing and preferred embodiment of the present utility model.
As shown in Figure 1-2, a kind of dull and stereotyped Direct-heating column temperature modulation device, comprises plate-like compressing tablet 1, plate-like compressing tablet 22, chromatographic column 1, chromatographic column 24, pad 1, pad 26, rigidity heat conduction dull and stereotyped 1, rigidity heat conduction dull and stereotyped 1, flat heater sheet 9 and fixed screw 10, plate-like compressing tablet 1 is identical with plate-like compressing tablet 22, chromatographic column 1 is identical with chromatographic column 24, pad 1 is identical with pad 26, rigidity heat conduction dull and stereotyped 1 is identical with rigidity heat conduction flat board 1, described flat heater sheet 9 is clamped by rigidity heat conduction dull and stereotyped 1 and rigidity heat conduction dull and stereotyped 1, chromatographic column 1, chromatographic column 24 is coiled into snail line structure and precision is fitted in rigidity heat conduction dull and stereotyped 1 respectively, the surface of rigidity heat conduction dull and stereotyped 1, plate-like compressing tablet 1, plate-like compressing tablet 22 is by chromatographic column 1, chromatographic column 24 is pressed in rigidity heat conduction dull and stereotyped 1 respectively, the surface of rigidity heat conduction dull and stereotyped 1, inserts pad 1 between plate-like compressing tablet 1 and rigidity heat conduction dull and stereotyped 1, between plate-like compressing tablet 22 and rigidity heat conduction dull and stereotyped 1, insert pad 26, plate-like compressing tablet 1, plate-like compressing tablet 22 is fixedly connected with by fixed screw about 10, described plate-like compressing tablet 1, plate-like compressing tablet 22 axially connects elastic card claw 11 with elastic connection way.
Described rigidity heat conduction is dull and stereotyped 1, rigidity heat conduction dull and stereotyped 1 by metal material, as copper, aluminium, stainless steel etc. are made, both can ensure its rigidity and flatness, simultaneously also can the temperature of the homogenize area of heating surface, promotes the homogeneity of heating.Described flat heater sheet 9 can be the flexible heater sheet adopting printed circuit technique to make, the mica heating plate produced as polyimide flex heating plate, silicon rubber flexible heater sheet or employing rigid plane heating technique or ceramic heating flake, it is thin that flexible heater sheet has thickness, adapt to arbitrary surfaces, and the features such as simple installation, but by the restriction of encapsulating material, serviceability temperature can not more than 250 DEG C.And rigidity heating plate has high temperature resistant, that output power is high feature, but regular surfaces can only be applied to.Mica heating plate can long-term work below 400 DEG C, and output power density can reach 17W/cm
2.
When rigidity heat conduction flat board 1, rigidity heat conduction dull and stereotyped 1 are by heating, heat is transferred in chromatographic column 1, chromatographic column 24 by the mode of conduction.Because rigidity heat conduction is dull and stereotyped 1, rigidity heat conduction dull and stereotyped one 8 heating time two surperficial power densities and coefficient of heat conductivity be identical, although so chromatographic column 1, chromatographic column 24 are fitted in respectively the both sides up and down of flat heater sheet 9, heat transfer condition and heating power are identical substantially.Chromatographic column 1, chromatographic column 24 can be two independently chromatographic columns, the analytical applications that two root chromatogram columns of can satisfying the demand heat simultaneously, such as binary channels parallel parsing, the analytical column that mariages TCD detecting device needs and reference column heating etc.; Also can be a root chromatogram column, its center partially passes through that rigidity heat conduction is dull and stereotyped 1, the fluting at rigidity heat conduction dull and stereotyped 1 and dull and stereotyped heating plate 9 center links together, the analytical applications of longer (30m-60m) chromatographic column of can satisfying the demand like this.
To be fitted in the mode precision of snail line to keep chromatographic column when being wound around chromatographic column and using that rigidity heat conduction is dull and stereotyped 1, in rigidity heat conduction dull and stereotyped 1, rigidity heat conduction is dull and stereotyped 1, the surface of rigidity heat conduction dull and stereotyped 1 to adopt plate-like compressing tablet 1, plate-like compressing tablet 22 chromatographic column 1, chromatographic column 24 to be pressed in respectively.But because mostly chromatographic column is to be made up of quartz material, thickness of column 0.1mm-0.2mm, pressure is crossed conference and is caused chromatographic column cracked.Thus plate-like compressing tablet 1, plate-like compressing tablet 22 have annular projection, the space of a ring-type is just constituted between such plate-like compressing tablet plate-like compressing tablet 1, plate-like compressing tablet 22 and rigidity heat conduction flat board 1, rigidity heat conduction dull and stereotyped 1, its height is consistent with chromatographic column external diameter, thus avoids and cause chromatographic column to be out of shape cracked situation because coupling mechanism force is excessive.And in order to adapt to the chromatographic column of different-diameter, between plate-like compressing tablet 1 and rigidity heat conduction dull and stereotyped 1, insert pad 1, between plate-like compressing tablet 22 and rigidity heat conduction dull and stereotyped 1, insert pad 26.This device just can be made to be applicable to the chromatographic column of various outer diameter by the thickness of adjustment pad 1, pad 26.Plate-like compressing tablet 1, plate-like compressing tablet 22 can be symmetrical the both sides being arranged on flat heater sheet 9, so just can realize double-deck chromatographic column and be wound with.
As in Figure 3-5, described elastic card claw 11 comprises shell fragment 12, spacing claw 13 and guiding bead 14, described shell fragment 12, by stamped metal sheets between spacing claw 13 and guiding bead 14, mold injection integral type connects, also by riveted joint, screw welding, glued joint and interference fit connection, spacing claw 13 and rigidity heat conduction dull and stereotyped 1, gap between rigidity heat conduction dull and stereotyped 1 is less than chromatographic column 1 respectively, the diameter of chromatographic column 24, and the displacement of the maximum flexibility that elastic card claw 11 can realize is less than chromatographic column 1, the diameter of chromatographic column 24, adopt the guiding bead 14 of circular conical surface or arc-shaped surface for chromatographic column 1, lead when chromatographic column 24 is wound around and prevent chromatographic column 1, chromatographic column 24 is composed post and is scratched.
Plate-like compressing tablet 1, plate-like compressing tablet 22 limit chromatographic column 1, chromatographic column 24 in the motion of axis direction, and the motion of chromatographic column radial direction is limited by elastic card claw 11.Described plate-like compressing tablet 1, plate-like compressing tablet 22 axially connect elastic card claw 11 with elastic connection way, can move in axis direction certain limit.Elastic card claw 11 and plate-like compressing tablet 1, plate-like compressing tablet 22 integrally process, and the shape of adjustment junction can reduce the rigidity of elastic card claw 11, realizes the regime of elastic deformation met the demands.Under normal installed condition, the diameter that spacing claw 13 and rigidity heat conduction are dull and stereotyped 1, gap between rigidity heat conduction dull and stereotyped 1 is less than chromatographic column 1, chromatographic column 24 respectively, and the displacement of the maximum flexibility that elastic card claw 11 can realize is greater than the diameter being less than chromatographic column 1, chromatographic column 24, when needs are wound around chromatographic column, the power needed for winding can make chromatographic column jack-up elastic card claw 11.After chromatographic column is passed through, elastic card claw 11 can set back.Now, the radial displacement of chromatographic column has limited with regard to limited claw 13.Different with quantity according to the distribution of elastic card claw 11, chromatographic column often around a circle, at least will pass through an elastic card claw 11.Because the gap of elastic card claw 11 and rigidity heat conduction flat board should be substantially suitable with column diameter, so need guide piece when being wound around, when not damaging chromatographic column face coat, auxiliary chromatographic column slips in annular gap smoothly.The utility model adopts the guiding bead 14 of circular conical surface or arc-shaped surface, when being wound around chromatographic column, can being that chromatographic column effectively avoids sharp edge, preventing chromatographic column from scratching.
Use plate-like compressing tablet 1, plate-like compressing tablet 22 and elastic card claw 11 stationary chromatographic post, not only achieve chromatographic column dull and stereotyped with the rigidity heat conduction of fitting of snail line mode, this canoe of what is more important is reversible, and namely user can locally amputate according to actual needs or all replace chromatographic column.The column oven that the Direct-heating column heating arrangement that this advantage makes this utility model provide adopts with traditional experiment room equipment has identical dirigibility in chromatographic column use.
Shown in Fig. 6-7, described chromatographic column 1, chromatographic column 24 can adopt individual layer to twine the mode of mode or Double wound.The utility model is applied to the canoe of the chromatographic column of different length.When the chromatographic column of required winding is shorter, individual layer can be adopted to twine mode, winding of single layer mode is side chromatographic column 1 being coiled in flat heater sheet 9, and make chromatographic column be fitted in rigidity heat conduction dull and stereotyped 1 with a plate-like compressing tablet 1, and at the opposite side of flat heater sheet 9, in order to reduce power dissipation and environmental temperature fluctuation to the impact of temperature control, adopting heat-insulation layer compressing tablet 15, insulation material 16 being covered in rigidity heat conduction dull and stereotyped 1.When the longer chromatographic column of use one or two independently chromatographic column time, then need the mode adopting Double wound.Now, plate-like compressing tablet 1, plate-like compressing tablet 22 is needed to use chromatographic column 1, chromatographic column 24 to be fixed on the both sides of flat heater sheet 9.When the chromatographic column that winding one is longer, pass, then respectively from center to edge coiling chromatographic column in the circular hole 17 needing just chromatographic column 1, chromatographic column 24 to process in advance from rigidity heat conduction flat board 1, rigidity heat conduction dull and stereotyped 1 and dull and stereotyped heating plate 9 or annular groove.And when coiling two independently chromatographic column time, the chromatographic column of both sides can independent coiling.Experiment shows, the chromatographic column of heating equal length, adopts bilayer arrangement mode lower than the average power consumption of individual layer arrangement mode by more than 40%.
As shown in Figure 8, the manufacturing process of the apparatus structure of automatic winding chromatographic column is: locate with circular hole 17, and chromatographic column heating arrangement is fixed on rotating driving device, the axis of circular hole 17 and rotation axis coincident.Alignment device 18 is placed in helix tangential direction, is in same plane with helix.First chromatographic column is wrapped on chromatographic column heating arrangement through alignment device.That chromatographic column by alignment device 18, through the guiding of the bead 14 that leads, will touch elastic card claw 11 when rotating driving device rotates.Regulating guiding bead 14 can produce certain tensile force, making chromatographic column successfully by elastic card claw 11 jack-up, can finally slip into the gap between plate-like compressing tablet and rigidity heat-conducting plate flat board when being wound around.The pre-tensioning regulating guiding bead 14 to produce can also tighten up chromatographic column when being wound around, and makes it tight coiling, very close to each other.
The utility model, when ensureing temperature modulation performance, effectively can improve the production efficiency of chromatographic column module, substantially increase the maintainability of module; Volume is little, caloic is low, with low cost; Do not limit the maximum operation (service) temperature of chromatographic column; Can reuse, reduce the wasting of resources, use cost significantly reduces, and production efficiency is high.
In order to verify the temperature modulation performance of this device, physics and chemistry test is carried out to it.First under different ramp rate conditions, power test has been carried out to it.The typical 30m of test use one is long, and the quartz capillary column of internal diameter 0.32mm adopts the mode that double-layer spiral line is wound around.Testing setup chromatogram thermal module is warming up to 300 DEG C with the heating rate of 100 DEG C/min, 400 DEG C/min and 600 DEG C/min from 50 DEG C respectively.Experimental result shows in temperature-rise period, and its average power consumption is respectively 42W, 102W and 147W.Compared with conventional post incubator, under same heating rate, the power consumption of the present embodiment be its 1/30, specifically see Fig. 9-10.
The above, be only the utility model preferred embodiment, therefore the scope that the utility model implements can not be limited according to this, the equivalence namely done according to the utility model the scope of the claims and description change with modify, all should still belong in scope that the utility model contains.
Claims (5)
1. a dull and stereotyped Direct-heating column temperature modulation device, is characterized in that: comprise plate-like compressing tablet one, plate-like compressing tablet two, chromatographic column one, chromatographic column two, pad one, pad two, rigidity heat conduction flat board one, rigidity heat conduction flat board one, flat heater sheet and fixed screw, plate-like compressing tablet one is identical with plate-like compressing tablet two, chromatographic column one is identical with chromatographic column two, pad one is identical with pad two, rigidity heat conduction dull and stereotyped one is identical with rigidity heat conduction flat board one, described flat heater sheet is clamped by rigidity heat conduction dull and stereotyped one and rigidity heat conduction dull and stereotyped one, chromatographic column one, chromatographic column two is coiled into snail line structure and precision is fitted in rigidity heat conduction flat board one respectively, the surface of rigidity heat conduction flat board one, plate-like compressing tablet one, plate-like compressing tablet two is by chromatographic column one, chromatographic column two is pressed in rigidity heat conduction flat board one respectively, the surface of rigidity heat conduction flat board one, inserts pad one between plate-like compressing tablet one and rigidity heat conduction flat board one, inserts pad two, plate-like compressing tablet one between plate-like compressing tablet two and rigidity heat conduction flat board one, plate-like compressing tablet two is fixedly connected with up and down by fixed screw, described plate-like compressing tablet one, plate-like compressing tablet two axially connects elastic card claw with elastic connection way.
2. dull and stereotyped Direct-heating column temperature modulation device according to claim 1, it is characterized in that: described elastic card claw comprises shell fragment, spacing claw and guiding bead, described shell fragment, by stamped metal sheets between spacing claw and guiding bead, mold injection integral type connects, also by riveted joint, screw welding, glued joint and interference fit connection, spacing claw and rigidity heat conduction flat board one, gap between rigidity heat conduction flat board one is less than chromatographic column one respectively, the diameter of chromatographic column two, and the displacement of the maximum flexibility that elastic card claw can realize is less than chromatographic column one, the diameter of chromatographic column two, the guiding bead of circular conical surface or arc-shaped surface is adopted to be used for chromatographic column one, lead when chromatographic column two is wound around and prevent chromatographic column one, chromatographic column two is composed post and is scratched.
3. dull and stereotyped Direct-heating column temperature modulation device according to claim 1, is characterized in that: chromatographic column one, chromatographic column two can adopt individual layer to twine the mode of mode or Double wound.
4. dull and stereotyped Direct-heating column temperature modulation device according to claim 1, is characterized in that: described rigidity heat conduction flat board one, rigidity heat conduction dull and stereotyped one are metal material heat conduction flat board.
5. dull and stereotyped Direct-heating column temperature modulation device according to claim 1, is characterized in that: described flat heater sheet is polyimide flex heating plate, silicon rubber flexible heater sheet, mica heating plate or ceramic heating flake.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520617247.8U CN204855466U (en) | 2015-08-14 | 2015-08-14 | Dull and stereotyped directly -heated type chromatographic column temperature modulating device |
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| CN201520617247.8U CN204855466U (en) | 2015-08-14 | 2015-08-14 | Dull and stereotyped directly -heated type chromatographic column temperature modulating device |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105647781A (en) * | 2016-03-07 | 2016-06-08 | 西北农林科技大学 | Heating plate system for studying thermal death dynamics of microorganisms |
| CN110646552A (en) * | 2019-10-23 | 2020-01-03 | 无锡市凯奥善生物医药科技有限公司 | Chromatographic column temperature control system and method |
| CN110785659A (en) * | 2017-09-21 | 2020-02-11 | 株式会社岛津制作所 | Column oven |
| CN112198240A (en) * | 2020-08-26 | 2021-01-08 | 浙江中环瑞蓝科技发展有限公司 | Miniature gas chromatography column box |
-
2015
- 2015-08-14 CN CN201520617247.8U patent/CN204855466U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105647781A (en) * | 2016-03-07 | 2016-06-08 | 西北农林科技大学 | Heating plate system for studying thermal death dynamics of microorganisms |
| CN110785659A (en) * | 2017-09-21 | 2020-02-11 | 株式会社岛津制作所 | Column oven |
| CN110646552A (en) * | 2019-10-23 | 2020-01-03 | 无锡市凯奥善生物医药科技有限公司 | Chromatographic column temperature control system and method |
| CN112198240A (en) * | 2020-08-26 | 2021-01-08 | 浙江中环瑞蓝科技发展有限公司 | Miniature gas chromatography column box |
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| C14 | Grant of patent or utility model | ||
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20151209 Termination date: 20190814 |