Classifications

• • G—PHYSICS
  • G01—MEASURING; TESTING
  • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
  • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
  • G01N30/02—Column chromatography
  • G01N30/26—Conditioning of the fluid carrier; Flow patterns
  • G01N30/28—Control of physical parameters of the fluid carrier
  • G01N30/30—Control of physical parameters of the fluid carrier of temperature

Definitions

• the invention relates generally to the field of gas and liquid chromatography and specifically to the design of chromatographic column assemblies which facilitate the heating of chromatographic columns using microwave heating methods.
• Gas and liquid chromatography are physical methods for the separation, identification, and quantification of chemical compounds. These methods are used extensively for applications that include the measurement of product purity in analytical chemistry, the determination of environmental contamination, the characterization of natural substances, and the development of pharmaceuticals.
• a sample mixture is injected into a flowing neutral carrier stream and the combination then flows through a tube or chromatographic column.
• the inner surface of the column is coated or packed with a material called the stationary phase.
• the stationary phase As the sample mixture and carrier stream flow through the column, the components within the mixture are retained by the stationary phase to a greater or lesser degree depending on the relative volatility (in the case of gas chromatography) or the relative solubility (in the case of liquid chromatography) of the individual components and on their respective affinities for the stationary phase.
• the stationary phase When the individual mixture components are released into the carrier stream by the stationary phase, they are swept towards the column outlet where they are detected and measured with a detector. Different chemical compounds are retained for different times by the stationary phase.
• the specific compounds in the mixture can be identified.
• the relative concentration of the compounds is determined by comparing the peak amplitudes measured with the detector for each compound.
• the primary difference between gas and liquid chromatography is the mode of separation. In gas chromatography, the sample is volatilized and propelled down the analytical column by a moving stream of gas. In liquid chromatography, the sample is dissolved and propelled down the analytical column in a moving stream of liquid. Another difference between gas and liquid chromatography is that the columns used in liquid chromatography are generally filled or packed with the stationary phase, while those used in gas chromatography can also have the stationary phase coated or bonded to the interior wall, instead. GC and LC measurements are facilitated by the application of heat to the chromatographic column to change its temperature.
• Heating an LC column affects the relative solubility of the mixture's components in the two phases and can enhance the separation as well as improve the repeatability of the elution times of the component chemicals.
• the resistive element heating method has several limitations. To achieve even heating of the column, a large volume of air is rapidly circulated around the chromatographic column. In addition to heating the column, the air heats the oven itself. Because the thermal mass of the oven is much larger than that of the column, the rate at which the column can be heated is commensurately reduced. A related problem is cooling time. After heating the oven to a high temperature during an analysis, it takes significantly longer to cool the oven plus the column to their initial temperature so that the next sample may be analyzed than it would to cool the column alone. Together, these limitations reduce the throughput of the chromatograph. Attempts to localize the resistive heat element onto the column itself so as to reduce or eliminate peripheral heating of the 'oven' are described in U.S.
• Patent 3,169,389 to Green et al. U.S. Patents 3,232,093 to Burow et al., and in U.S. Patent 5,005,399 to Holtzclaw et al.
• Each of these patents describe methods for directly wrapping or cladding the chromatographic column with a resistive heating element. Methods are also described for positioning the resulting metal clad column adjacent to a cooling source to decrease cooling times. This method of heating can be difficult to implement in practice because of uneven heating of the column due to local hot or cold spots in the resistive heating element surrounding the column.
• microwave heating as described in U.S. Patent 4,204,423 to Jordan. Potential advantages of microwave heating are efficiency and selectivity. Suitable objects placed in a microwave oven will be heated when the oven is operated, but the temperature of the oven itself will not change. Microwave heating occurs in materials which absorb the microwave energy and convert it into heat. Current chromatographic columns are generally made of materials that do not absorb microwave energy at an appreciable rate. For example, most GC capillary columns are made of polyimide and fused silica.
• any column material can be placed in a microwave oven except for conductive materials such as metals which will reflect the electromagnetic energy (by shorting out the electric field) in the microwave oven, thus rendering it inoperable.
• conductive materials such as metals which will reflect the electromagnetic energy (by shorting out the electric field) in the microwave oven, thus rendering it inoperable.
• any such non-metal material can be placed in a microwave oven, but they will not necessarily be heated by the oven.
• U.S. Patent 3,023,835 to Brashear describes an apparatus for heating packed chromatographic columns by exposing them to radio frequency (RF) radiation. Brashear describes heating chromatographic columns via dielectric heating or via inductive heating (i.e., magnetic heating). In the case of dielectric heating, Brashear specifies that the column and the packing filler are constructed of electrically insulating materials.
• Brashear specifies that: (1 ) the column is constructed of a metal containing some magnetic components to enable inductive heating to occur; (2) the filler contains a metal powder to promote heat conduction from the column into the filler; and (3) the metal powder may also be magnetic to promote local inductive heating.
• inductive heating of the filler would not occur inside the metal column because it would be shielded from the electromagnetic field by the metal column in which it is sheathed.
• metal-filled packing material inside columns is not generally a good scheme. The sample material passing down the column can be exposed to the metal. If the metal is not chemically inert, then some components of the sample can react with the metal thus distorting the resulting chromatogram.
• Microwave heating occurs in materials having dielectric or magnetic loss factors sufficiently high that when exposed to high frequency electromagnetic radiation these materials absorb sufficient energy from the electric or magnetic field to heat at an appreciable rate. Materials with high dielectric loss factors absorb energy from electric fields. Conversely, materials with high magnetic loss factors absorb energy from magnetic fields. Microwave heating apparatuses have both electric and magnetic fields within them so either loss mechanism will result in heating. Food is heated well in microwave ovens because it contains water. Water has a high dielectric loss factor at microwave frequencies and is thus readily heated by energy absorbed from the electric field. The water in turn heats the rest of material in the food through conventional heat conduction and convection mechanisms.
• Chromatographic columns can be modified in one of two ways to make microwave heating practical. First, the column itself can be modified to incorporate a microwave absorbing material such that direct heating of the column is achieved. Second, the column can be positioned adjacent to (i.e., in contact with, or in close proximity to) a microwave absorbing material in an assembly that provides adequate heat transfer so that the column is heated by the microwave absorbing material via conduction or convection.
• microwave absorbing material(s) used in chromatographic columns assemblies By carefully selecting the microwave absorbing material(s) used in chromatographic columns assemblies, intrinsic over- temperature protection can be built into the column so that it cannot be heated in a microwave heating apparatus to a temperature beyond a desired maximum temperature. Dielectric and magnetic loss factors are usually temperature dependent. If a microwave absorbing material is selected for which the loss factor decreases rapidly at the maximum desired column temperature, then the column assembly using this material cannot be heated appreciably above the desired temperature in a microwave heating apparatus. One way to achieve this is to select a ferromagnetic absorbing material having the correct Curie temperature. The loss factor of a ferromagnetic absorber decreases dramatically at its Curie temperature.
• a microwave-absorbing column assembly heated in a microwave apparatus can be heated much more quickly and efficiently and subsequently cooled more quickly because: (1 ) the total thermal mass of the material to be heated or cooled is much smaller than in a conventional oven; and (2) the microwave energy selectively heats the desired material and not the whole of the oven.
• microwave-absorbing columns assemblies can be enclosed in insulating materials to better isolate them thermally from their environment. Standard chromatograph columns are not insulated in this manner from the oven environment. Materials used to insulate a microwave absorbing column assembly must be selected so as not to disturb the heating of the column by the microwave heating apparatus. To allow the heat to escape from the column when cooling is desired, the column insulator can be designed to allow air or some other heat sink material to be circulated around the column when needed to cool the column assembly.
• the present invention provides a chromatography column for microwave heating that either incorporates microwave absorbing material into the column itself or positions the column adjacent to microwave absorbing material so that the column and the chromatography sample contained therein are heated by the microwave absorbing material via conduction, convection or radiation.
• a microwave absorbing material e.g., ferrite, iron, cobalt, nickel, or carbon
• Microwave absorbing material can also be incorporated into an external element (e.g., an outer tube, sleeve, or spool) positioned adjacent to the chromatography column.
• a layer of thermal insulation can be placed around the column to decrease the rate of heat loss to the column's surroundings.
• a gap can be provided between the chromatography column and thermal insulation to further reduce heat loss during the heating cycle and accelerate cooling at the end of the heating cycle by making it possible to ventilate the heated column.
• the chromatography column assembly can be protected from overheating by selecting a microwave absorbing material having a loss factor that decreases rapidly above a predetermined maximum temperature.
• FIG. 1 shows the cross section of a typical chromatograph column.
• FIG. 2 and 3 show the cross-sections of a two chromatograph columns with a microwave absorbing material added in accordance with the present invention.
• FIG. 4 shows the cross-section of a chromatograph column with a microwave absorbing material mixed into one of the existing column layers in accordance with the present invention.
• FIG. 5 shows the cross-section of a chromatograph column assembly constructed in accordance with the present invention where an existing column is inserted inside a second tube made at least in part with a microwave absorbing material.
• FIG. 6 and 7 show two different views of a chromatograph column assembly constructed in accordance with the present invention where an existing column is placed adjacent to sheets of microwave absorbing material.
• FIG. 8 is a graph illustrating the loss factor of a microwave absorbing material that could be used to limit the maximum temperature to which a chromatographic column assembly built in accordance with this invention can be heated in a microwave heating apparatus.
• FIG. 9 is a graph showing the heating profile of a column assembly built with intrinsic over-temperature protection in accordance with this invention.
• FIG. 10 and 11 show the cross sections of apparatuses designed to help control the heat loss from column assemblies built in accordance with this invention.
• FIG. 12 shows a column configuration in which the microwave absorbing material is essentially perpendicular to the direction of the electric field in a microwave heating apparatus.
• Microwave heating can occur in a material if its dielectric or magnetic loss factor is significantly greater than zero. When such a material is exposed to a high frequency electric or magnetic field, the material will absorb power from the field and convert this power into heat.
• the average power per unit volume absorbed by a given material is described by the following equation:
• E ⁇ g is the rms electric field strength
• ⁇ 0 is the permeability of free space
• ⁇ " eff is the magnetic loss factor
• H ms is the rms magnetic field strength.
• the dielectric loss factor ⁇ " ⁇ ff is a parameter which describes losses associated with the movement of electrical charge in a material; i.e. conduction losses.
• conduction losses There are two distinct sources of conduction losses. The first is associated with very short range electrical currents called displacement currents that result from the rotation of permanent dipoles within a material in response to an electric field.
• the second source of conduction loss is associated with long range charge transport within a dielectric material that is somewhat conductive.
• the dielectric loss factor includes all electrical losses associated with the conduction of electrical charge through a material in response to an electric field. The material will heat at a rate in °C/sec given by:
• Heating Rate P av / p c p (2)
• p is the density of the material
• c p is the specific heat of the material
• Equation 1 the rate at which the temperature of a material will heat when exposed to microwave radiation is proportional to the dielectric and magnetic loss factors of the material.
• Table 1 summarizes the properties of some materials at 25°C and at a frequency of 2.5 GHz, which is a frequency commonly used for microwave heating.
• FIG. 1 shows the cross section of the most common type of GC capillary column. It is a tube fabricated of fused silica (glass) 10 coated externally with polyimide 20 for added strength.
• the fused silica has an ID ranging from 0.1 to 0.53 mm in diameter.
• the wall thickness of the fused silica is 0.1 to 0.2 mm.
• the wall thickness of the polyimide is typically about 5 ⁇ m.
• the interior 30 of tube 10 consists of a thin stationary phase of typically 1 ⁇ m or less that is bonded to the inside of the fused silica (not shown in FIG. 1) and the remainder is gas most of which is the inert carrier gas.
• the total length of the capillary column varies typically from 15 to 60 m.
• An LC column generally consists of a metal or plastic tube packed with a porous support material such as crushed silica to which is bound a stationary phase. Tube dimensions generally range from an internal diameter of 1 mm to 10 mm and a length of 5 cm to 30 cm. Taking FIG. 1 as an LC column, element 10 is the tube and element
• the external coating 20 is not used with a LC column.
• High loss factor in this case means any material with a high enough loss factor to enable a chromatographic column to be heated at a rate of at least a few degrees Centigrade per minute and preferably at a rate of 100°C per minute or more. Such a material would likely have a loss factor of at least 0.05.
• microwave absorbing materials having loss factors less than 0.05 can be used if they are heated in microwave heating apparatuses with very high quality factors. A microwave heating apparatus with a high quality factor will not itself absorb much microwave power.
• the total microwave losses in a microwave absorbing material used to heat a column or column assembly in a microwave heating apparatus should be at least as great as the total losses that occur elsewhere in the microwave heating apparatus such that the microwave heating apparatus is at least 50% efficient in delivering available microwave power in the microwave heating apparatus to the microwave absorbing material.
• Microwave absorbing materials with high dielectric or magnetic loss factors could be used.
• materials with high dielectric loss factors include carbon and some forms of titanium oxide.
• materials with high magnetic loss factors include ferrites, iron, nickel, and cobalt. Carbon, iron, nickel, and cobalt are electrically conductive and as such not good microwave absorbing material candidates by themselves in a microwave heating application because they will tend to short out or distort the electromagnetic field in a microwave heating apparatus.
• an electrically insulating material such as epoxy, rubber, or plastic
• the resulting matrix typically has a much lower conductivity and so does not disable a microwave heating apparatus, yet retains a significant portion of the microwave absorbing characteristics of the additive.
• the iron-filled epoxy in Table 1 is such a mixture.
• Carbon- loaded materials are another example of such mixtures.
• moderately conductive carbon is added to a dielectric material in precise quantities to give the resulting mixture a desired volume resistivity.
• Such mixtures are the basis for carbon-film resistors.
• microwave absorbing material refers broadly to any material with a high enough dielectric or magnetic loss factor that can be heated in a microwave heating apparatus at a sufficiently fast rate and to a high enough temperature to be of practical value in gas or liquid chromatographic applications. This typically requires a loss factor of at least 0.05.
• Microwave absorbing material also includes materials such as iron or carbon that are electrically conductive and therefore are not good absorbers by themselves, but are good microwave absorbers when added in powdered form as fillers to non- conductive materials, such as epoxies or plastics. In such a mixture, it is the filler material that absorbs the microwave energy and is heated as a result.
• microwave absorbing material refers to the filler material that actually absorbs the microwave energy, rather than to the matrix as a whole. It should be clear to one of ordinary skill in the art that “microwave absorbing material” refers to any material' or combination of materials that can be used to significantly enhance microwave heating of a chromatographic column.
• microwave absorbing matrix will be used to refer to mixtures of microwave absorbing materials and insulating materials. These material mixtures will often have specific advantages in chromatographic applications in that they overcome common physical limitations of most microwave absorbing materials by themselves. Gas chromatographic columns must typically be flexible, chemically inert, and capable of withstanding frequent temperature cycling. Similarly, liquid chromatographic columns must typically be chemically inert, and capable of withstanding high pressure and frequent temperature cycling. Few, if any microwave absorbing compounds or elements by themselves meet these requirements. However, when a microwave absorbing material is mixed into an insulating material with suitable physical properties, such as polyimide, the resulting mixture has physical properties similar to those of the insulating material yet absorbs microwave energy because of the microwave absorbing filler.
• suitable physical properties such as polyimide
• microwave absorbing matrices can be engineered that combine good physical and microwave absorbing properties.
• the resulting material matrix should typically have an overall loss factor of at least 0.05.
• Preferred embodiments of such microwave absorbing matrices include mixtures of a high grade plastic such as polyimide or polyetherether ketone (PEEK) and an additive such as iron, ferrite, nickel, cobalt, or carbon.
• PEEK polyetherether ketone
• the term "microwave” will also be used broadly to cover electromagnetic radiation in the frequency range from
• Chromatographic columns can be augmented with a microwave absorbing material in two ways to enhance the effectiveness of microwave heating devices in heating the columns.
• a microwave absorbing material can be added directly to a column resulting in direct conductive heating of the reminder of the column (e.g., a combination of a continuous phase material and the microwave absorbing material).
• microwave absorbing material can be placed adjacent to (i.e., in thermal contact with, or in close proximity to) a column such that the column is heated indirectly by thermal conduction or convection.
• microwave absorbing material and a column which achieve one or both of these configurations.
• FIG. 2 shows the cross section of a chromatographic column where an extemal layer 70 comprising microwave absorbing material is added to the outside of an existing column.
• tube 50 represents a fused silica or glass tube. It is coated with an optional layer of a polymer 60, such as polyimide.
• the polyimide layer 60 is optional for this modified chromatograph column because the microwave absorbing layer 70 could provide the same function as the polyimide layer in existing columns.
• tube 50 is a glass or plastic tube.
• Tube 50 could even be metal if the microwave absorbing material 70 shields it sufficiently to prevent the metal from short circuiting the electric field in a microwave heating apparatus.
• the polymer layer 60 would not be present.
• FIG. 3 A better configuration is shown in FIG. 3.
• a microwave absorbing material layer 90 is added to the existing chromatograph column tube 50.
• the tube 50 could be fused silica, glass, plastic, or metal.
• the polymer sheath 100 covers the outside of the microwave absorbing material 90. Together, the tube 50 and sheath 100 physically isolate the microwave absorbing layer 90 from the environment. Sheath 100 could consist of a material such as polyimide or polytetrafluoroethylene, sold under the trademark TEFLON.
• column tube 120 is a fused silica, glass, or plastic tube in which a microwave absorbing material has been mixed.
• the resulting microwave absorbing matrix can be readily heated in a microwave heating apparatus.
• tube 120 is coated with a thin layer 130 of material such as polyimide to strengthen and environmentally isolate the column.
• the microwave absorbing material could be mixed into the outer polymer layer 130 rather than into the tube 120.
• the electrical effect on the column would be much the same.
• this structure is illustrated in Fig. 3 where the microwave absorbing layer 90 consists of a polyimide-microwave absorbing material mixture and the sheath 100 is absent.
• the polyimide can be impregnated with iron, nickel, ferrite, carbon, or other microwave absorbing materials to form a composite material that can be readily extruded over the column during manufacture.
• an inner layer of fused silica, glass, or plastic is surrounded by an intermediate layer containing a microwave absorbing material.
• a polymer, such as polyimide, is then applied over the intermediate layer to form a third, outer layer that provides a degree of physical protection, thermal insulation, and added strength for the column assembly.
• a microwave absorbing material can be added to a chromatographic column so as to make it possible to heat the column in a microwave heating apparatus.
• the microwave absorbing material can be mixed into one of the column components or it can be bonded to the column as an exterior or interior layer. Some combination of these physical configurations could also be used. It should be clear to one of average skill in the art that the invention lies in the addition of the microwave absorbing material to an existing chromatographic column and not in the manner in which it is added.
• a chromatographic column can be heated in a microwave heating apparatus by a microwave absorbing material if the column is located adjacent to the microwave absorbing material such that heat is transferred by the absorbing material to the column via thermal conduction, convection, or radiation.
• the column assembly should keep the temperature difference between the microwave absorbing material and the column to a minimum.
• FIG. 5 shows the cross-section of one column assembly built in accordance with the present invention. At least a portion of a standard chromatographic column 160 is inserted into a larger sleeve or tube 170 made of a microwave absorbing material.
• the inner diameter of microwave absorber tube 170 must be large enough as compared to the outside diameter of column 160 to facilitate threading many tens of meters together.
• the gap should be small enough to keep the interior of the microwave absorber tube 170 at isothermal conditions over the cross-section.
• FIG. 6 and 7 show two views of another column assembly built in accordance with this invention. This assembly is easier to implement than that shown in FIG. 5. Chromatographic columns are often very long and slender - up to 100 meters in length by less than 1 mm in diameter.
• An effective column assembly for microwave heating purposes can be constructed by coiling a chromatographic column adjacent to a heating member containing a microwave absorbing material.
• the column assembly can be constructed by coiling an existing chromatographic column around a core containing a microwave absorbing material.
• FIG. 6 shows the cross section of such an assembly.
• FIG. 6 highlights several adjacent column sections 210 sandwiched between two layers 200 and 220 containing a microwave absorbing material. The sandwich can help maintain more stable thermal conditions at different points along the column.
• FIG. 7 shows a side view of the column assembly. A loop of the column 230 is coiled around a sheet 200 containing a microwave absorbing material.
• a second microwave absorbing sheet 220 is wrapped outside the column 230.
• the column 230 and the microwave absorbing sheets 200 and 220 are in effect the concentric cylinders slipped together. If only one microwave absorbing sheet is used instead of two, it could be positioned either inside or outside the column coil.
• the chromatography column can also be coiled inside a container made of a microwave absorbing material.
• the column can be placed adjacent to the heating member containing a microwave absorbing material in any of a number of possible configurations.
• the column can be placed directly in contact with the microwave absorbing material, or placed adjacent to the microwave absorbing material to provide adequate heat transfer.
• microwave absorbing materials and chromatographic columns that will keep the column in proximity to the heating member such that the column is heated indirectly by the absorbing material in a microwave heating apparatus. It should be clear to one of average skill in the art that the invention lies in combining a microwave absorbing material and a chromatographic column in an assembly that makes microwave heating possible and not in the specific physical configuration of the assembly.
• Microwave absorbing materials used in chromatographic column or column assemblies built in accordance with this invention must have dielectric or magnetic loss factors that are high enough to make microwave heating feasible. Dielectric and magnetic loss factors are often temperature dependent. This characteristic can be utilized to design column assemblies that can only be heated in a microwave heating apparatus to a target temperature and no higher. This design feature can prevent over-temperature conditions that can damage or destroy a column.
• Intrinsic over-temperature protection is achieved by selecting a microwave absorber for which the dielectric or magnetic loss factor decreases rapidly at temperatures approaching the maximum desired use temperature of the chromatographic column. As the loss factor of the selected microwave absorber decreases with increasing temperature, the rate at which it absorbs energy in a microwave heating apparatus will also decrease. At some critical point, the temperature will stabilize at a fixed value. This mechanism is illustrated in FIG. 8 and 9.
• FIG. 8 shows the loss factor as a function of temperature for a microwave absorbing material that could be used to give a chromatographic column intrinsic over-temperature protection.
• the loss factor is stable at lower temperatures, but decreases rapidly above some critical temperature.
• the loss factor of a suitable microwave absorbing material need not be constant at low temperatures as shown in FIG. 8. The loss factor must simply remain high enough for microwave heating to be efficient at temperatures below the critical temperature, but decrease rapidly over a narrow temperature range to a level at which microwave heating is no longer efficient.
• FIG. 9 shows the heating profile for a chromatographic column that is heated in a microwave apparatus where the column is built with a microwave absorbing material that has the loss factor vs. temperature characteristic shown in FIG. 8.
• the rate of temperature increase is substantially constant.
• the rate of temperature increase slows down.
• the temperature at which the heat generated in the microwave absorbing material by the absorption of microwave energy matches the heat lost to the environment the temperature stabilizes at a fixed value. This temperature is the maximum operating temperature of the column.
• Intrinsic over-temperature protection can be achieved by selecting a microwave absorbing material that is ferromagnetic and has an appropriate Curie temperature.
• the Curie temperature of ferromagnetic materials is the temperature at which they cease to be ferromagnetic and becomes paramagnetic.
• the Curie temperature also indicates the temperature at which the material's magnetic loss factor approaches zero Thus, a ferromagnetic material cannot be readily heated in a microwave oven beyond its Curie temperatures provided that its dielectric loss factor is also very low.
• Table 2 shows the Curie temperature of some ferromagnetic materials.
• nickel is the most suitable for preventing over- temperature conditions in polyimide for which the maximum use temperature is approximately 400°C.
• Ferrite materials are available with a range of Curie temperatures less than approximately 450°C.
• thermal energy can be specifically applied to appropriately designed columns or column assemblies and not to the rest of the oven. Because the column or column assemblies have little total material or mass, they also have little thermal mass; therefore, they can be heated or cooled quickly. However, in some circumstances the thermal mass may be so small that heating rates can be compromised by heat lost to the column's environment. Even air surrounding the column may carry away a significant fraction of the thermal energy. An additional problem can arise when cooling the column. If a column is kept at high temperatures for a long period of time, heat loss to the oven environment can eventually raise the temperature of other parts of the oven enough to make quick cooling of the column and the oven difficult. To address these problems, column assemblies built in accordance with this invention can be packaged in a manner which allows the heat flow from the column to be better controlled.
• the first element needed to control heat loss from the column is thermal insulation. Columns can be packed in a thermally insulating envelope to minimize the heat loss from them to the rest of the microwave oven. It is not standard practice in the chromatograph business to thermally insulate columns because the columns are heated indirectly in large resistively heated ovens.
• FIG. 10 shows one embodiment of a column insulating system.
• the perspective in FIG. 10 is the same as in Fig. 6.
• a column or column assembly 260 built in accordance with this invention is sandwiched between two thermal insulators 250 and 270 which reduce the heat loss from the column to the environment.
• the column assembly insulators 250 and 270 are made into concentric cylinders with the column assembly 260 coiled between them. This structure is as shown in FIG. 7.
• Insulators 250 and 270 need not be the same material and one or the other may be eliminated in some circumstances.
• a gap can be left between the thermal insulators 250, 270 and the column assembly 260 for ventilation to facilitate rapid cooling of the column assembly 260 after completion of the heating cycle.
• FIG. 10 shows one embodiment of a column insulating system.
• FIG. 10 shows one embodiment of a column insulating system.
• FIG. 10 shows one embodiment of a column insulating system.
• FIG. 10 shows one embodiment of a column insulating system.
• a column 300 built in accordance with this invention is sheathed within a layer of thermal insulation 310 that reduces heat loss from the column. If the material layer 100 in FIG. 3 is a good thermal insulator, a separate layer of thermal insulation may not be necessary. As described in reference to FIG. 3, an outer layer of polyimide is attractive because it helps to shield the microwave absorbing material
• polyimide is a good insulator, it can also help thermally shield the column.
• thermal insulators that could be used in this invention: plastics, ceramics, and fiberglass to name a few.
• Another possible insulator is a vacuum. If most of the air is pumped out of a microwave heating apparatus so that a column assembly is heated in a vacuum, then very little heat will be lost from the column at useful chromatographic temperatures.
• the two requirements for the insulation material are that: (1 ) it must be transparent to high frequency electromagnetic radiation such that it does not shield the column assembly from this radiation and thus prevent the column assembly from heating; and (2) it must have low dielectric and magnetic loss factors so that it will not be heated directly by microwave radiation.
• the second element needed to control heat loss from the column is a means for quickly removing the heat from the column or column assembly when cooling is required.
• a means of circumventing the thermal insulation and accelerating thermal loss is most easily achieved by blowing cool air, a cryogenic gas, or some other convenient material 280 over the column assembly as shown in FIG. 10 and 11 until the temperature is reduced to the desired level. If the heating process is performed in a vacuum, then blowing cool air through the oven during the cool down cycle will quickly reduce the column temperature to the desired level. If the column assembly is equipped with an outer layer of thermal insulation as depicted in Figure 10, a blower or ventilation system can be used to induce a flow of air through the gap between the insulation layer and the column to accelerate cooling after completion of each heating cycle.
• Microwave absorbing material must be added to a column or column assembly in order to heat them in microwave heating apparatuses.
• Many microwave absorbing materials or matrices are least partly conductive electrically.
• Carbon-loaded polyimide can be quite conductive for example.
• the conductivity of microwave absorbing materials or matrices used to heat chromatographic columns in microwave heating apparatuses must not be too high. The upper conductivity limit depends upon the orientation of the microwave absorbing material with respect to the electric field within a given microwave heating apparatus.
• a microwave absorbing material oriented essentially perpendicular to the electric field in a microwave heating apparatus has no significant electrical current path length parallel to the electric field.
• An example of such a structure is shown in FIG. 12.
• a column 400 with a microwave absorbing material coated on the outside as shown in FIG. 2 is coiled into a circular column bundle 410.
• the column bundle 410 is placed in a microwave heating apparatus 420 in which the electric field 430 is perpendicular to the plane 440 of each loop of the column bundle 410.
• the volume conductivity of the microwave absorbing material can be as high as approximately 5000 mho/cm.
• the microwave absorbing material is positioned in a microwave heating apparatus such that there is a conductivity path of sufficient length (greater than 2% of the free space wavelength) that is parallel to the electric field, then the maximum conductivity of the microwave absorbing material is approximately 100 mho/cm.

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