CN103424495A - Chromatographic column heating device for gas chromatograph - Google Patents
Chromatographic column heating device for gas chromatograph Download PDFInfo
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- CN103424495A CN103424495A CN2013103572135A CN201310357213A CN103424495A CN 103424495 A CN103424495 A CN 103424495A CN 2013103572135 A CN2013103572135 A CN 2013103572135A CN 201310357213 A CN201310357213 A CN 201310357213A CN 103424495 A CN103424495 A CN 103424495A
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Abstract
The invention discloses a chromatographic column heating device which comprises a container, a heating element, a temperature measuring element and a cooling convection system. The heating element is used for heating the container. The temperature measuring element is used for measuring the temperature in the container. The cooling convection system is used for accelerating cooling speed of the whole device. Thermal insulation materials are disposed outside the container to lower heating power consumption. The device further comprises a heating container machined by high-thermal-conduction insulation materials, a heating wire and a platinum resistance wire temperature sensor. The heating container comprises at least two parts, and a chromatographic column can be operated when the heating container is opened. The heating wire is embedded in the container so as to heat the whole device. The platinum resistance wire having certain length is wound at the middle end of the chromatographic column and used for measuring average temperature of the chromatographic column. The chromatographic column heating device is small in size, low in power consumption, fast in heating, even in temperature distribution, and the like.
Description
Technical Field
The invention belongs to the field of analytical chemistry and heating devices, and relates to a chromatographic column heating device for a gas chromatograph.
Background
Gas chromatography is an important method of analytical chemistry. The sample and the carrier gas (usually inert gas) are first mixed fully at the injection port, then enter the chromatographic column along with the carrier gas flowing, and continuously flow to the end of the chromatographic column, in the process, the sample generates retention phenomenon between the carrier gas and the stationary phase of the chromatographic column, the retention effect of different samples is different, and the time of reaching the end of the chromatographic column is also different. In general, the retention of the high-boiling components is greater and the time to peak is later.
The time from the sample entering the gas chromatograph to the chromatogram peak is called retention time, and different retention times correspond to different compound types and are important qualitative bases of the gas chromatograph. In the actual analysis process, the temperature of the column is exponential to the retention time of each sample, and the retention time is rapidly reduced with increasing temperature. If the temperature of the selected chromatographic column is too low, the retention time of a high-boiling-point sample is extremely long, the analysis efficiency is low, and sample residues are possibly generated to influence the next analysis result; if the temperature of the selected chromatographic column is too high, the retention time of the low-boiling samples is very small, the samples are almost mixed together and are difficult to distinguish, and meanwhile, part of unstable compounds can be decomposed at high temperature, and the measurement result is deviated.
Therefore, a temperature programmed process is often used in gas chromatography to ensure that low boiling samples are separated sufficiently, while the retention time of high boiling samples is not too long. The faster the fastest temperature rise rate that can be achieved by the gas chromatograph, the higher the analysis efficiency that can be achieved.
For similar reasons, after the end of the temperature program, the column temperature is lowered to the initial value before the next sample can be analyzed. The faster the temperature drop of the column, the shorter the waiting time between analyses and the higher the analysis efficiency.
Another important indicator is the uniformity of the temperature distribution in the column. Only the chromatographic column with uniform temperature distribution can ensure that the analysis result has high repeatability and precision every time, otherwise, retention time drift can be caused, and the phenomena of supercooling condensation and overheating decomposition of a sample at the local position of the chromatographic column can occur when the temperature distribution is serious.
Most of the gas chromatographs currently on the market use a furnace for air bath heating of the column. The hearth structure is usually a large metal plate cavity, thick heat-insulating cotton materials are wrapped outside the hearth structure, heat is provided by heating wires inside the hearth structure, and forced convection heat exchange is carried out by using a large fan. Taking a 7890 gas chromatograph hearth of Agilent as an example, the heating device has the advantages of large volume (500 mmX350mmX350 mm), high power consumption (2400W), slow temperature rise and temperature reduction speed (the temperature rise rate is not more than 60 ℃ per minute when the hearth temperature is 300 ℃, the temperature reduction time is generally not less than 4 minutes), and low sample analysis efficiency.
A new technology in recent years is direct heating of gas chromatography columns, represented by the LTM low thermal mass module of RVM Scientific, inc (see references 1 to 4), in which a heating wire wrapped with an insulating material is wound around the column for direct heating and a length of platinum resistance wire is wound around the column for measuring the temperature of the column, which has the outstanding advantages of small volume (120 mmX100 mm), low power consumption (about 300W), and extremely fast temperature rise (up to 1200 degrees celsius per minute); on the other hand, the whole heating module is completely and fixedly connected before leaving the factory, a user cannot disassemble and assemble the heating module by himself, once the chromatographic column is damaged or the service life is reached, the whole heating module must be replaced, the price of the whole heating module is very high and generally exceeds 5000 dollars, and the price of the whole heating module is 5 times to 10 times that of a single gas chromatographic column. In addition, in practical application of the gas chromatograph, according to different types of samples to be analyzed, a user may replace different types of chromatographic columns for analysis, the number of times of replacement of the LTM module is limited, and the whole module is scrapped after the user replaces the LTM module for 3 to 5 times. After the gas chromatography column is contaminated by a high boiling point sample, the gas chromatography column can be continuously used only by cutting off the foremost section (0.3 m to 1 m), but the heating structure of the LTM chromatography column cannot be disassembled, and once the chromatography column is contaminated, only the whole expensive module can be replaced. These drawbacks greatly limit the range of applications for LTM modules.
Another heating device is the heating device invented by Griffin corporation (see reference 5), in which the heating block and the outer frame are separated by an electrically insulating material, the chromatographic column is directly placed on a heat sink extending from the heating block, and the temperature rise speed of the outer frame is greatly behind that of the heating block during heating, so that the heating power consumption can be effectively reduced. However, during and after temperature stabilization, since the outer frame is at a much lower temperature than the heating block, a large temperature gradient is formed in the inner cavity of the heating device for accommodating the chromatography column, and the temperature difference between different regions of the same chromatography column is large, which does not guarantee the analytical performance of the gas chromatography system.
The related documents are:
1. U.S. Pat. No. 5, 5782964, Gas chromatography column analysis control, 07/21/1998, Robert V.Mustacich
2. U.S. Pat. No. 5, 6209386, Electrically insulating gas chromatography and method of degrading same, 04/03/2001, Robert V.Mustatich et al
3. U.S. Pat. No. 5, 6490852, Electrically insulating gas chromatography and method of degrading same, 12/10/2002, Robert V.Mustatich et al
4. U.S. Pat. No. 4, 6530260, Gas chromatography analysis system, 03/11/2003, Robert V.Mustacich et al
5. U.S. Pat. No. 4, 8043565, Analytical instrumentation and processes, 10/25/2011, Patterson, Garth E, et al.
Disclosure of Invention
The invention aims to provide a chromatographic column heating device which can be used for a gas chromatograph.
This heating device includes the container that includes base and apron that insulating material processing of high thermal conductivity goes out, the platinum resistance wire on the gas chromatography post of winding that is used for heating the heater strip of container and is used for measuring the inside temperature of container, furthermore, it can reduce the thermal contact resistance between the two to increase flexible sheet metal between base and apron, thereby improve the inside temperature distribution homogeneity of whole heating device, it can accelerate whole heating device's cooling rate to increase cooling fan, it can reduce the required consumption of device heating to increase outside insulation material, the effect is more obvious when the device is in the higher temperature, it can make the installation of chromatographic column more reliable and more stable to increase chromatographic column fixing device, the chromatographic column drops when avoiding the device to receive vibrations.
The cover plate of the device is a flat plate and is installed on the concave base through screws to form a hollow container, the gas chromatographic column is placed in the container, and ventilation holes are formed in two sides of the container and used for air intake and heat dissipation. The heating wire and the base are cast and molded together, and the heating wire is positioned inside the base after casting molding to directly heat the base. A platinum resistance wire (such as 0.5 m) with a certain length is wound on the gas chromatographic column, and two ends of the platinum resistance wire are connected out through a high-temperature-resistant (not lower than 450 ℃) wire. The flexible metal sheet is fixed on the base, and the cover plate is clamped between the base and the cover plate after being pressed on the base to reduce contact thermal resistance, so that the temperatures of the cover plate and the base are consistent, and the uniformity of the temperature distribution in the whole cavity is ensured. The cooling fan is installed in the gas chromatograph frame, is located heating device's side, when needs are cooled down to the device, opens the fan, and the cold wind that the fan blew off flows through the heating device outside to blow through the container through the ventilation hole of container both sides inside, cool down the container inside and outside simultaneously, accelerate cooling speed. The heat-insulating cotton material is wrapped outside the whole container, so that the heat dissipation speed of the container to the air can be greatly reduced, the heating and maintaining power consumption of the heating container is reduced, particularly when the container is at a high temperature (for example, 200 ℃ or higher), the heat-insulating cotton can effectively reduce the power consumption of the heating container, and other components (such as a circuit board, a power supply, a shell and the like) of the gas chromatograph are prevented from being influenced by the heat dissipation of the heating device. The chromatographic column fixing device is an elastic buckle, and two ends of the elastic buckle are clamped on the fixing holes on the side surface of the base and used for fixing the chromatographic column to prevent the chromatographic column from sliding out of the cavity of the base.
The base can be made into a flat plate, correspondingly, the cover plate is processed into a concave structure, and after the base and the cover plate are connected through screws, a cavity for accommodating the chromatographic column can be formed. After the device is installed and formed, the structure of the device is the same as that of the device.
Another way of processing the container is to directly cast a container with an internal cavity during processing, and the heating wire is cast at the bottom of the container, which is equivalent to fixedly connecting the base and the cover plate and can not be detached. The structure has the advantages of better heat conduction, elimination of thermal contact resistance between the cover plate and the base due to the integrated design, better uniformity of temperature distribution of the cavity of the container and avoidance of possible damage to the device in the process of installation and disassembly. On the other hand, the operation of replacing the column in the integrated design is relatively complicated, requires gradual insertion from one side, requires special care in operation or otherwise easily damages the column. It is also possible to cast the column and the container together and leave 2 to 3 turns of the column coiled in the cavity of the container for shearing and replacing the column. The heating structure is easy to process, lower in cost and better in performance. The base and the cover plate can be glued into an integral structure by high-temperature glue, so that the structure similar to integration is realized.
Except that screw connection, also can fix with the spout between base and apron, process out the spout on the base, push the apron along the spout to realize being connected between the two, perhaps vice versa, process out the spout on the apron, push the base along the spout. The cover plate can be provided with a protrusion or processed, the base is provided with a clamping groove, when the cover plate is closed, the protrusion is clamped into the clamping groove, the structure is designed to be in interference fit, and the cover plate and the base are clamped. The cover plate may be formed with a slot and the base may be formed with a protrusion, but it is understood that the cover plate and the base may be connected by two or more fixing methods.
The ventilation hole also can be located the top and the bottom of container, and cold air gets into from the bottom vent, rises along the container inner wall after being heated, flows out from the top ventilation hole, and the natural convection current of air will heat the inside heat of container and take out, also can realize the cooling of device when not using external fan, and when using external fan, the natural convection current also can improve fan cooling efficiency. On the other hand, such a design may cause the cold air to penetrate through the inner cavity of the real heating container, resulting in poor uniformity of the temperature distribution inside the heating container. It will be apparent that the vent holes may alternatively be open in any two or more of the four directions top, bottom, left side, and right side to provide a path for air to cool the interior of the container. The open pore mode of strengthening the natural convection of air can improve the cooling efficiency, but can reduce the temperature homogeneity to a certain extent.
The heating wires in the heating device can also be replaced by heating sheets, the base material of the heating sheets can be made of high-temperature-resistant heat conduction materials (including but not limited to mica and the like), and the inner layers of the heating sheets are provided with resistance wires and temperature sensors according to specific power requirements and used for heating the whole container. When the heating plate is used, the heating plate can be directly fixed on the back of the base through the screw or the clamping groove to heat the base, part of the heating plate is easy to damage due to the fact that the material is fragile, and a metal thin plate is added on the outer side of the heating plate to serve as protection.
Instead of molding the heater wire and the base of the container together, the base of the container may be formed in two parts, a groove may be formed in one or both of the parts, the heater wire may be wound in the groove, and the two parts may be fixedly connected by a screw or a high temperature resistant heat conductive glue (e.g., a ceramic glue). The processing method has low requirements on processing conditions, does not need integral casting, only needs a standard ceramic forming process, and can reduce the processing cost. On the other hand, the connection between the heating wire and the ceramic base in the structure is not as tight as that in the integral casting molding, and the heat conduction efficiency is slightly poor.
When the platinum resistance wire is used for measuring the temperature, the platinum resistance wire can be directly wound in the cavity of the container for one circle, the leads are led out from two ends of the platinum resistance wire, and compared with the winding method of the platinum resistance wire on a chromatographic column, the winding method is more convenient to install and is more beneficial to replacing and maintaining the chromatographic column, but the measured temperature is the average temperature of the cavity of the container, and has a certain difference with the temperature of the chromatographic column, so that the accuracy of temperature measurement is reduced to a certain degree.
The platinum resistance wire can also be replaced by a platinum resistance temperature sensor (RTD) or a thermocouple temperature sensor. When a platinum resistance temperature sensor (RTD) or a thermocouple temperature sensor is used, a high-temperature-resistant lead of the sensor is bonded on the bottom plate, a measuring probe is extended into a cavity inside the heating container to measure the air temperature inside the cavity, an elastic fixing frame can be used, hooks at two ends of the elastic fixing frame are clamped in holes reserved on the base, the lead of the sensor is pressed by elastic force, or a concave cover is processed, the cover is fixed on the base by using screws, and the cover is pressed on the insulated lead by screwing the screws.
The flexible metal sheet is used for reducing contact thermal resistance, can be replaced by high-temperature-resistant heat-conducting silicone grease, and can also be directly plated with a layer of flexible metal on the contact surface of the container base and the cover plate. The flexible metal sheet (including but not limited to beryllium bronze, aluminum foil and the like) with good heat conduction is deformed after being extruded, can fill a tiny gap between the base and the cover plate, replaces air for heat conduction, greatly reduces contact thermal resistance between the base and the cover plate, and accordingly enables the temperature distribution of the base and the cover plate to be more uniform. The flexible metal sheet can be unfixed, directly clamped between the container base and the cover plate, and can also be fixed by a plurality of methods: if welding on the contact surface of base or apron, perhaps also can bend into the U nature with the edge of flexible sheetmetal, cover on base or apron contact surface, at the side trompil to use the fix with screw, also can adopt high temperature resistant glue to bond flexible sheetmetal on the contact surface of base and apron.
The high temperature resistant heat conductive silicone grease and the flexible metal layer plated on the surface of the base or the cover plate play a similar role, and the uniformity of the temperature distribution of the cavity in the container is improved by filling a tiny gap between the cover plate and the base with a material with high heat conductivity. On the other hand, after the cover plate is opened to maintain the chromatographic column, the heat-conducting silicone grease is coated again, and then the cover plate is covered, so that the poor thermal contact of partial areas caused by the loss of the heat-conducting silicone grease is prevented.
Cooling fan installs on gas chromatograph's outer frame, is just facing to one side ventilation hole of heating container, blows in cold wind inside the container through these ventilation hole fans, then flows out from the ventilation hole of opposite side, reduces the inside temperature of container, and simultaneously, partly blow over from the container outside from the wind that the fan blew off, to the container surface cooling, the inside and outside cooling can reduce the time that cooling process needs simultaneously. In addition, the fan can be changed into an exhaust fan, and cold air is forced to flow through the inside and the outside of the container simultaneously, so that the aim of quickly cooling is fulfilled.
The heat insulation cotton material comprises but not limited to glass fiber, ceramic fiber and other high-temperature resistant materials with low heat conductivity, the heat insulation cotton with a certain thickness (such as 20 mm) is wrapped outside the container to play a heat insulation role on the heating container, and a large amount of heat is prevented from being dissipated into the air when the container is heated, so that the heating power requirement is reduced, when the temperature of the heating device is high (such as 200 ℃ or higher), the wrapped heat insulation cotton has a very obvious effect on reducing the power consumption, and 30% or more of energy can be saved. Because the heating device is the part with the highest power consumption of the gas chromatograph, the power consumption of the heating device can be reduced, and the power consumption requirement of the whole gas chromatograph can be obviously reduced. Meanwhile, heat emitted by the heating device is easy to accumulate in the case to cause the case to be overheated integrally, so that the heat dissipation requirement of the whole case is reduced while the power consumption is reduced.
On the other hand, the temperature reduction speed of the heating device is reduced due to the heat insulation cotton material, so that a groove can be processed on the outer surface of the heating container, the hard heat insulation material obtained by vacuum sintering or other processing means is used, after the heat insulation material is installed, the groove for allowing enough cold air to flow through is ensured to be left between the outer surface of the cavity and the heat insulation material, and when the fan is started, the cold air flows through the inner surface and the outer surface of the container simultaneously and rapidly reduces the temperature of the container.
Another kind is that the cotton takes away the heat preservation when the cooling, and the cooling efficiency of this kind of cooling mode is higher, can open the heat preservation cotton by user's manual, but this needs the user to operate the instrument at every turn the experiment beginning, has reduced work efficiency, and the user is scalded by inside high temperature cavity easily simultaneously. The linear motor can be used for automatically pulling the heat insulation cotton outwards, the heat insulation cotton is fixed on the linear motor, the motor is controlled by software to work, the heat insulation cotton is pulled when the cavity needs to be cooled, and the heat insulation cotton is closed when the cavity needs to be heated and kept at a high temperature, so that the mode is safe to use, but the linear motor and the corresponding transmission device need to be added.
The winding of gas chromatography post has designed a little elasticity buckle in the cavity of base, and power is flattened the buckle, and the card is gone into the aperture that the base side was processed for prevent that the chromatographic column from following to deviate from, when the chromatographic column was taken out to needs, flattens the buckle again and takes out, just can take out the gas chromatography post.
The device of the invention can reduce the size of the gas chromatograph, reduce the required power consumption, heat the chromatographic column quickly and uniformly, and improve the analysis efficiency and performance of the gas chromatograph.
Drawings
Fig. 1 is a perspective view of a column heating apparatus for use in a gas chromatograph according to an embodiment of the present invention, in which a column 40 has been placed.
Fig. 2 is a perspective view of the heating apparatus shown in fig. 1 with the cover plate 12 removed.
Fig. 3 is a cross-sectional view "a-a" shown in fig. 1.
FIG. 4 is a schematic diagram of a platinum resistance wire temperature sensor wrapped around a chromatography column of a heating device of one embodiment of the invention.
Fig. 5 is a schematic view of the air flow path inside the heating device when the heating device cools down according to an embodiment of the invention.
Fig. 6 is a schematic view of an external air flow path when the heating device cools down according to an embodiment of the present invention.
Fig. 7 is an exploded view of a heating device according to an embodiment of the present invention, which is wrapped with insulation wool.
Fig. 8 is an exploded view of the outer surface of a heating device of one embodiment of the present invention after machining grooves.
Fig. 9 is a schematic view of a heating structure of a heating apparatus according to an embodiment of the present invention, in which vent holes are opened at the top and bottom.
Fig. 10 is a schematic structural view of an embodiment of the present invention in which a heating device is heated by a heating plate instead of a heating wire.
Detailed Description
The invention will be further described with reference to the following examples.
In fig. 1 the column heating device is in a first operating state (heating vessel 10 closed) in which it is capable of heating the column. The apparatus of the figure has been fitted with a chromatography column 40, to be noted: the column 40 is not part of the column heating apparatus of the present invention.
To facilitate handling of the chromatography column 40 in the cavity inside the vessel, the heating vessel 10 is designed as two parts, a base 11 and a cover 12, which can be removed or opened and which are fastened with screws 13. When it is desired to install or remove the column, the vessel lid 12 and screws 13 are removed first, and then the gas chromatography column 40 placed on the base 11 is operated.
The heating wire 20 is arranged in the base 11, is cast and molded together with the base during processing, is integrated with the base 11, and is not taken out after being processed. This manner of casting the heater wire and the base together ensures excellent contact between the heater wire 20 and the base 11 of the vessel, improves heating efficiency, and simplifies the system structure.
Here, the heating vessel 10 functions to heat the chromatography column 40. Although a specific heating vessel 10 is shown in fig. 1, it should be readily understood by those skilled in the art that this is merely an example for the purpose of explaining the principles of the present invention and is not intended to limit the invention to such a situation. For example, the outer shape of the heating container 10 is not limited to a cylindrical shape (or a circular ring shape). Those skilled in the art can design their specific shape according to various considerations, for example, operability, strength, material saving, aesthetics, or even personal preference.
For another example, several (e.g., 3) wedge-shaped rib structures 118 may be added around the base flange to enhance the strength of the flange, so that the flange is not easily broken when the flange is accidentally knocked during operation or when the instrument is subjected to vibration and impact.
The heating vessel 10 is preferably formed with as thin a wall thickness as possible while maintaining strength of use, which reduces the overall thermal mass of the vessel and facilitates increasing the rate of temperature rise and decrease of the heating device.
The material used to make the heating vessel 10 can also be selected by one skilled in the art as appropriate, and typically can be selected to have a thermal conductivity greater than 0.1W/m K and an electrical conductivity less than 1S/m, including but not limited to ceramics, quartz, mica, various alloys, and the like.
The gas chromatographic column is connected with the sample injector and the detector, and the three parts work together to form the whole analysis system. The transition portion 115 in the base 11 is used to connect the column to the sample injector and detector, and is a cylindrical structure above the section B-B in the figure, unlike the lower annular structure 119 which is repeatedly wound around the column, the transition portion 115 is cylindrical and the column passes through it in a single piece. To avoid cold spots at the joint, the transition portion 115 is included as part of the base and is heated by the heater wire with the rest of the base to maintain the joint temperature at the joint. The transition portion 115 in the figure is merely an example, and a person skilled in the art can design the specific structure of the transition portion as required.
The column heating apparatus shown in fig. 2 is in a second operating state (heating vessel 10 is open) in which the column is free to operate.
On the base 11 there is a machined groove structure 114 and the column is coiled and then mounted in the groove structure 114. In order to reduce the thermal resistance presented by the air layer, and to reduce the size and thermal mass of the container, the width of the grooves is selected to be as small as possible; on the other hand, too small a groove width would cause difficulties in practical operation. The width of the groove can be selected by the skilled person according to the actual need, e.g. whether the applied test sample is clean, whether the column needs to be changed frequently, the skill of the operator, the diameter and length of the column in general, the maximum temperature rise rate of the set method, etc.
The width of the groove is selected to be 1.5mm in this embodiment, and since the diameter of a common capillary chromatography column is not more than 0.53mm, an operator can freely operate the chromatography column. The method is suitable for users with low requirements on the temperature rise speed and high requirements on the simplicity and convenience of operation of replacing the chromatographic column.
In FIG. 2, the front vents 112 provided in the base 11 are used to cool the entire container, as will be described in more detail below in connection with FIG. 5
To more uniformly heat the chromatography column, the interface 116 between the vessel base 11 and the vessel lid 12 may be coated with a thermally conductive material, including (but not limited to) thermally conductive silicone, thermally conductive grease, etc.; in addition, flexible metal sheets, including but not limited to beryllium bronze sheets, tin foil, etc., may also be clamped over the contact surface; the contact surface 116 may also be plated with a layer of a flexible metal, including but not limited to beryllium copper or the like. This can greatly reduce the thermal contact resistance on the contact surface, reduce the temperature difference between the base and the cover plate, and improve the temperature uniformity in the whole heating cavity.
For convenience of use, the container base 11 and the container lid 12 may be connected by a hinge or other connection means (not shown), and the column may be operated by opening the container lid 12. The structure does not need to disassemble the screw and the cover plate, and is easier for users to operate and use.
For better fixation of the chromatography column, high temperature resistant wires, including but not limited to glass fiber wires, copper wires, etc., may be used to fix the chromatography column in a bundle before installing it in the heating chamber.
Fig. 3 is a sectional view showing the structure of the heater wire, in which the heater wire 20 is wound in a proper shape in the vessel base 11 before the vessel base 11 is formed, and then cast-formed. The heater strip 20 is embedded in the processed container base 11, and the heater strip 20 is not taken out any more.
It is also possible to machine the vessel base 11 into two upper and lower parts, machine a proper groove on the contact surface of the two parts for installing the heater wire 20, and then fix the two upper and lower parts of the vessel base 11 into a whole by sintering or bonding. The integrated structure can reduce the thermal resistance between the heating wire and the container and improve the heating efficiency. Meanwhile, a protection and fixing device of the heating wire is omitted, and the heating wire is convenient to install and use.
It is also possible to machine grooves in the back of the base 11 of the container, to fix the heating wire therein, and then to protect and fix the heating wire with a thermally and electrically insulating plate. The scheme has lower processing cost, and part of structures in the scheme can be repeatedly utilized during maintenance, so that the maintenance cost is reduced; on the other hand, the scheme has poor heating efficiency and is complex to install and use.
By way of further example, a shaped heating plate or heating rod may be used to close the heating vessel and provide corresponding protection and fixing means. This solution has the lowest processing costs, but the heating efficiency is also the worst.
Fig. 4 is a schematic diagram of a platinum resistance wire temperature sensor wound around the middle section of a chromatographic column. The gas chromatography column had been wrapped with a length of platinum resistance wire prior to delivery to the user. The platinum resistance wire temperature sensor 30 with a certain length is wound on the chromatographic column 40, and the connector and the electric wire are led out after the platinum resistance wire temperature sensor is wound on the heating container for one circle along with the chromatographic column, so that the average temperature of the whole chromatographic column temperature zone can be measured.
The platinum resistance wire is wound at a certain middle position of the gas chromatographic column, so that the front end and the rear end of the chromatographic column can be shortened according to the normal use requirement of a user, and the position of the chromatographic column wound with the platinum resistance wire can be selected according to the application requirement. Generally, the front end of a sample inlet of a chromatographic column is heavily polluted and often needs to be cut short, so that the position of a platinum resistance wire can be properly backwards wound. The position of the wound platinum resistance wire selected in this example is the total length position of 2/3 from the front end of the column. For example, a 30 meter long column, the platinum resistance wire is selected to be wound starting at a position 20 meters from the front end of the column.
The total length L of the platinum resistance wire wound along the column is slightly less than the circumference of one turn around the internal cavity of the heating vessel. Thus the platinum resistance wire can measure the average temperature of the whole cavity. Because the container is made of an electric insulating material, short circuit cannot occur between the sensor and the container, and the length of the platinum resistance wire slightly smaller than the perimeter of the cavity can prevent the platinum resistance wire from being short-circuited.
Another way is to wrap the column and platinum resistance wire together with an insulating material such as fiberglass, which can be wound around the cavity for any length and better reflect the overall temperature conditions of the cavity, but this layer of insulating material can reduce the accuracy and sensitivity of the temperature measurement.
The temperature at a point in the cavity can also be measured with a temperature sensor and used to characterize the temperature of the column. The scheme has low cost, can select the conventional chromatographic column on the market, does not need to wind a platinum resistance wire temperature sensor at the designated position before leaving the factory, and is convenient for a user to use; on the other hand, there is a certain deviation between the measured temperature and the average temperature of the column due to the difference in temperature at various points in the cavity.
Fig. 5 to 6 show the air flow condition of the heating device with a fan arranged on the left side for blowing air and cooling. Each arrow in fig. 5 indicates the air flow direction inside the container, and each arrow in fig. 6 indicates the air flow direction outside the container. In the cooling process of the heating device, two air flowing cooling modes exist simultaneously.
The front vent hole 112 and the rear vent hole 113, which provide air inlets and outlets of the internal cavity, are disposed in a bilaterally symmetric structure. A pressure differential is created by a fan or pump on one or both sides of the heating device to force the gas to flow through the entire heating vessel. The forced air at normal temperature is divided into two parts, one part of the air flows along the outer wall of the container, and the other part of the air enters from the vent hole at one side (such as the front vent hole 112) and then flows out from the vent hole at the other side (such as the rear vent hole 113). The two air flow paths respectively realize the forced convection cooling of the inner wall and the outer wall of the container. Because the container is made of a material with high thermal conductivity, the temperature of the whole container and the internal chromatographic column can be rapidly reduced by simultaneously cooling the inside and the outside.
In fig. 5, ambient air is shown entering the interior cavity of the container through the left front vent 112 and flowing down the cavity, exiting the rear vent 113 and transition section 115, under the influence of the left side fan. This air flow realizes cooling the container inner wall.
In fig. 6, the air at normal temperature is blown by the left fan to bypass the heating container 10, so as to cool the outer wall of the container.
The inner wall and the outer wall are cooled simultaneously, so that the time required by cooling the container can be effectively reduced.
Fig. 7 shows another embodiment, in which a heat-insulating cotton cover 51 and a heat-insulating cotton box 52 are wrapped around the outside of the heating container 10. Under the condition of not wrapping the heat preservation cotton, along with the temperature rise of the heating container, the heat dissipation power consumption of the container to the air through the outer surface is improved, and the temperature rise speed is reduced; after the outer layer is wrapped by the heat insulation cotton, the heat dissipation speed of the heating container can be greatly reduced, so that the closer heating rate can be kept at different temperatures; on the other hand, because the container is wrapped with the heat preservation cotton, the cooling speed of the heating device is obviously slowed down.
A notch may be formed in each of the left and right sides of the thermal cotton box 52, for example, a first notch 521 is formed in the left side and a second notch (not shown) is formed in the right side as shown in the figure. When needs are cooled down heating device, the air current that fan or pump produced flows through inside the heating container through these two breachs, to the container inner wall cooling. This scheme only realizes the cooling to the container inner wall, and mode speed for the interior outer wall of container is cooling obviously slows down simultaneously.
In addition, a corresponding device can be designed to move the heat insulation cotton away from the surface of the heating cavity, so that the inner wall and the outer wall of the container can be cooled simultaneously. The scheme can improve the cooling speed, but improves the complexity of the system.
Fig. 8 shows another embodiment, a groove 117 is formed on the outer surface of the heating container 10, the insulation cotton cover 51 and the insulation cotton box 52 are made of hard insulation material formed by vacuum sintering, when the insulation cotton cover 51 and the insulation cotton box 52 are closed, the groove 117 on the outer surface is not blocked to form an air channel, and the normal temperature air blown by the fan can flow through the air channel formed by the groove and flow out from the other side. Thus, the temperature of the heating structure can be simultaneously reduced on the inner surface and the outer surface without opening the heat-preservation cotton cover 51 and the heat-preservation cotton box 52.
In fig. 9, another embodiment is shown, the rear vent 113 and the front vent 112 are respectively located on the upper and lower surfaces of the container 10, and at the same time, the upper and lower corresponding positions of the thermal insulation cotton box 52 are also provided with a first notch 521 and a second notch 522, so that after the thermal insulation cotton is installed, the front vent 112 and the rear vent 113 are not partially shielded by the thermal insulation cotton. When the temperature needs to be reduced, the air with the normal temperature flows in from the front vent hole 112 at the lower part of the heating container 10, is heated by the inner wall of the heating container 10, and flows out from the rear vent hole 113 at the upper part, so that natural convection is formed. The natural convection mode can cool the heating device without using a fan.
Fig. 10 shows another embodiment in which a heating plate 21 is used instead of a heating wire to heat the rear surface of the heating container 10. This type of heating is less demanding to process, but the greater thermal contact resistance results in a temperature difference between the heating plate 21 and the heating container 10.
The embodiments described above are intended to facilitate one of ordinary skill in the art in understanding and using the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (8)
1. A chromatographic column heating device comprises a container, a heating element for heating the container and a temperature measuring element for measuring the temperature in the container, and is characterized in that: the container is also provided with an external heat-insulating material to reduce the power consumption required by heating of the device.
2. The chromatography column heating apparatus of claim 1, wherein: the container comprises a base and a cover plate, and a heat conducting piece is arranged between the base and the cover plate to reduce the contact thermal resistance between the base and the cover plate; or,
preferably, the cover plate is a flat plate and is mounted on the concave base through a movable connecting structure to form a hollow container, the gas chromatographic column is placed in the container, and ventilation holes are formed in two sides of the container and used for air intake and heat dissipation; or,
preferably, the base adopts a flat plate, the cover plate is of a concave structure, and the base and the cover plate are connected through a movable connecting structure to form a cavity for accommodating the chromatographic column; or the base and the cover plate are of an integrated structure, and the heating element is arranged in the base to directly heat the base; or,
preferably, the chromatographic column and the container are cast and formed together, and two to three circles of the chromatographic column are reserved and coiled in the cavity of the container for shearing and replacing the chromatographic column; or the base and the cover plate can be glued into an integral structure by high-temperature glue; or,
preferably, the base and the cover plate are fixed by adopting a sliding chute, the sliding chute is arranged on the base, and the cover plate is pushed in along the sliding chute, so that the connection between the base and the cover plate is realized; or, a sliding groove is arranged on the cover plate, and the base is pushed in along the sliding groove; or, a protrusion structure is arranged on the cover plate, a clamping groove structure is arranged on the base, when the cover plate is closed, the protrusion is clamped into the clamping groove, the structure is designed to be in interference fit, and the cover plate and the base are clamped; or the cover plate is provided with a clamping groove structure, the base is provided with a protrusion structure, when the cover plate is closed, the protrusion is clamped into the clamping groove, and the structure is designed to be in interference fit, so that the cover plate and the base are clamped; or,
preferably, the container base comprises two parts, wherein a groove is arranged on the surface of one part or two parts, the heating element is wound in the groove, and then the two parts are fixedly connected through a movable connecting structure or high-temperature-resistant heat-conducting glue; or,
preferably, the heating element and the base are cast together.
3. The chromatography column heating apparatus of claim 1, wherein: the cooling convection system includes: a forced convection device is arranged on the gas chromatograph frame and is positioned on the side surface of the heating device; the container is provided with vent holes on two sides so as to blow cooling air flow through the interior of the container; or,
preferably, the vent holes are opened in any two or more directions of the four directions of the top, the bottom, the left side and the right side of the container, and provide a path for air to cool the inside of the container; or,
preferably, the forced convection device is arranged on an outer frame of the gas chromatograph, is opposite to a vent hole on one side of the heating container, blows cold air into the container through the vent holes, then flows out from the vent hole on the other side, reduces the temperature in the container, and simultaneously blows a part of air blown out from the fan through the outside of the container to reduce the temperature of the outer surface of the container; or,
preferably, the forced convection device is a blowing fan or an exhaust fan; or,
preferably, the heat-insulating cotton material is a high-temperature-resistant material with low thermal conductivity, and comprises glass fibers and ceramic fibers; or,
preferably, the outer surface of the heating container is provided with a groove, the hard heat-insulating material obtained by vacuum sintering or other processing means is mounted, and then the groove through which enough cold air flows is ensured to be reserved between the outer surface of the cavity and the heat-insulating material; or,
preferably, the heat-insulating cotton material is provided with an opening and closing control device, and the opening and closing control device is connected with the linear motor through a transmission piece to control the heat-insulating cotton material to be pulled outwards or folded inwards.
4. The chromatography column heating apparatus of claim 1, wherein: the heating element adopts a heating wire or a heating sheet; preferably, the base material of the heating sheet is made of a high-temperature-resistant heat conduction material; or,
preferably, the heat conducting material comprises mica, and a resistance wire and a temperature sensor are arranged in the inner layer of the heating sheet according to specific power requirements and are used for heating the whole container; fixing a heating plate on the back of the base through a movable connecting structure or a clamping groove to heat the base; or,
preferably, a metal sheet is added on the outer side of the heating plate for protection.
5. The chromatography column heating apparatus of claim 1, wherein: the temperature measuring element is a platinum resistance wire wound on the gas chromatographic column or a platinum resistance temperature sensor or a thermocouple temperature sensor; or,
preferably, the platinum resistance wire is wound in the cavity of the container for one circle, and leads are led out from two ends of the platinum resistance wire; or,
preferably, the high-temperature resistant lead of the platinum resistance temperature sensor or the thermocouple temperature sensor is bonded on the bottom plate, and the measuring probe is extended into the cavity inside the heating container to measure the air temperature inside the cavity; or, an elastic fixing frame is used, hooks at two ends of the elastic fixing frame are clamped in holes reserved on the base, and the wire of the sensor is pressed by elastic force; or a concave cover is provided and the cover is screwed to the base to compress the insulated conductor.
6. The chromatography column heating apparatus of claim 1, wherein: the heat conducting piece is a flexible metal sheet or high-temperature-resistant heat-conducting silicone grease or a layer of flexible metal directly plated on the contact surface of the container base and the cover plate; or,
preferably, the flexible metal sheet comprises a beryllium bronze sheet and an aluminum foil; or,
preferably, the flexible metal sheet is sandwiched directly between the container base and the cover plate, or is secured by one of the following means: welding the base or the cover plate on the contact surface; bending the edge of the flexible metal sheet into a U shape, covering the contact surface of the base or the cover plate, forming a hole on the side surface, and fixing by using a screw; and bonding the flexible metal sheet on the contact surface of the base and the cover plate by adopting high-temperature-resistant glue.
7. The chromatography column heating apparatus of claim 1, wherein: the chromatographic column is provided with a fixing device to prevent the chromatographic column from falling off when the device is vibrated.
8. The chromatography column heating apparatus of claim 7, wherein: the gas chromatographic column is wound in the cavity of the base, the fixing device is an elastic buckle, and two ends of the elastic buckle are clamped in fixing holes in the side face of the base and used for fixing the chromatographic column.
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