US20150233614A1 - Method for setting a temperature, and tempering container - Google Patents

Method for setting a temperature, and tempering container Download PDF

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Publication number
US20150233614A1
US20150233614A1 US14/627,169 US201514627169A US2015233614A1 US 20150233614 A1 US20150233614 A1 US 20150233614A1 US 201514627169 A US201514627169 A US 201514627169A US 2015233614 A1 US2015233614 A1 US 2015233614A1
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Prior art keywords
container
peltier element
temperature
cooling
storage block
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US14/627,169
Inventor
Carsten Kindt
Helmut Eilers
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Anton Paar Provetec GmbH
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Anton Paar Provetec GmbH
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Publication of US20150233614A1 publication Critical patent/US20150233614A1/en
Assigned to ANTON PAAR PROVETEC GMBH reassignment ANTON PAAR PROVETEC GMBH ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: Kindt, Carsten, EILERS, HELMUT
Abandoned legal-status Critical Current

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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25BREFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
    • F25B21/00Machines, plants or systems, using electric or magnetic effects
    • F25B21/02Machines, plants or systems, using electric or magnetic effects using Peltier effect; using Nernst-Ettinghausen effect
    • F25B21/04Machines, plants or systems, using electric or magnetic effects using Peltier effect; using Nernst-Ettinghausen effect reversible
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/14Investigating or analyzing materials by the use of thermal means by using distillation, extraction, sublimation, condensation, freezing, or crystallisation
    • G01N25/145Accessories, e.g. cooling devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L7/00Heating or cooling apparatus; Heat insulating devices
    • B01L7/52Heating or cooling apparatus; Heat insulating devices with provision for submitting samples to a predetermined sequence of different temperatures, e.g. for treating nucleic acid samples
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25BREFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
    • F25B21/00Machines, plants or systems, using electric or magnetic effects
    • F25B21/02Machines, plants or systems, using electric or magnetic effects using Peltier effect; using Nernst-Ettinghausen effect
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4022Concentrating samples by thermal techniques; Phase changes
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/42Low-temperature sample treatment, e.g. cryofixation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00Additional constructional details
    • B01L2300/08Geometry, shape and general structure
    • B01L2300/0832Geometry, shape and general structure cylindrical, tube shaped
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00Additional constructional details
    • B01L2300/18Means for temperature control
    • B01L2300/1805Conductive heating, heat from thermostatted solids is conducted to receptacles, e.g. heating plates, blocks
    • B01L2300/1822Conductive heating, heat from thermostatted solids is conducted to receptacles, e.g. heating plates, blocks using Peltier elements
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10LFUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L2290/00Fuel preparation or upgrading, processes or apparatus therefore, comprising specific process steps or apparatus units
    • C10L2290/60Measuring or analysing fractions, components or impurities or process conditions during preparation or upgrading of a fuel
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25BREFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
    • F25B2321/00Details of machines, plants or systems, using electric or magnetic effects
    • F25B2321/02Details of machines, plants or systems, using electric or magnetic effects using Peltier effects; using Nernst-Ettinghausen effects
    • F25B2321/021Control thereof
    • F25B2321/0212Control thereof of electric power, current or voltage
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25BREFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
    • F25B2400/00General features or devices for refrigeration machines, plants or systems, combined heating and refrigeration systems or heat-pump systems, i.e. not limited to a particular subgroup of F25B
    • F25B2400/24Storage receiver heat
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N11/00Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N11/00Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
    • G01N2011/0006Calibrating, controlling or cleaning viscometers
    • G01N2011/0013Temperature compensation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N11/00Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
    • G01N2011/0006Calibrating, controlling or cleaning viscometers
    • G01N2011/002Controlling sample temperature; Thermal cycling during measurement
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N2035/00346Heating or cooling arrangements
    • G01N2035/00356Holding samples at elevated temperature (incubation)
    • G01N2035/00366Several different temperatures used
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N2035/00346Heating or cooling arrangements
    • G01N2035/00356Holding samples at elevated temperature (incubation)
    • G01N2035/00376Conductive heating, e.g. heated plates
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N2035/00346Heating or cooling arrangements
    • G01N2035/00425Heating or cooling means associated with pipettes or the like, e.g. for supplying sample/reagent at given temperature
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N2035/00346Heating or cooling arrangements
    • G01N2035/00445Other cooling arrangements
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02Details not specific for a particular testing method
    • G01N2203/022Environment of the test
    • G01N2203/0222Temperature
    • G01N2203/0226High temperature; Heating means
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02Details not specific for a particular testing method
    • G01N2203/022Environment of the test
    • G01N2203/0222Temperature
    • G01N2203/0228Low temperature; Cooling means
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/40Investigating hardness or rebound hardness
    • G01N3/54Performing tests at high or low temperatures
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/26Oils; viscous liquids; paints; inks
    • G01N33/28Oils, i.e. hydrocarbon liquids
    • G01N33/2811Oils, i.e. hydrocarbon liquids by measuring cloud point or pour point of oils

Definitions

  • the invention relates to a method for setting the temperature in a tempering container equipped for the reception of a sample using at least one Peltier element fixed to the outer wall surface of the container while ensuring a heat transfer contact. Furthermore, the invention relates to a tempering container for implementing this method.
  • tempering containers can have a different setup or form, for example, rectangular or circular circumference and be provided for different purposes.
  • tempering containers can comply with standard test and measurement conditions, in particular for petroleum products.
  • standard test conditions for example, for the measurement of CFPP (Cold Filter Plugging Point), which determines the limit of filterability of petroleum products.
  • filterability limit or Cold Filter Plugging Point of the temperature limit values of the filterability designates a low-temperature property of diesel fuel and heating oil EL (Extra Light). This is the temperature in degrees Celsius, at which a test filter under defined conditions clogs as the result of precipitated (n)-paraffin.
  • the sample is cooled down at a constant rate and thereby is conveyed at defined distances through a test filter.
  • CP Cloud Point
  • crystals are already formed, which, however, still pass through the filter. If the crystals become too large, the filter clogs.
  • the magnitudes tested are the Cloud Point, in which the turbidity of the sample is optically examined through mist clouds of the precipitated paraffin, etc.
  • the temperature of the sample is measured and with each temperature drop by a degree a sampling of the fuel forming the sample is made by means of the pump. With lower temperatures the paraffin in the diesel begins to flocculate, floating particles settle in the filter sieve and clog it. If the filling time for the test volume thus exceeds a specific time span or the fuel no longer completely returns from the test volume into the glass container, this is regarded as the filterability limit according to CFPP. According to standards, it is thereby provided, that the temperature in the tempering chamber is set in advance to ⁇ 34° C. and the sample is measured, that after the measurements at this temperature the container is cooled down to ⁇ 51° C. and is measured at this temperature and that finally a cooling and measurement takes place at ⁇ 67° C.
  • the cooling thereby has—as stipulated—to occur rapidly.
  • Very tight time constraints for the cooling process of the tempering container have to be adhered to, and accordingly the cooling capacity must be sufficient, in order, for example, within 150 seconds to cool down the tempering container enclosing the sample container in a stipulated time span by for example 17 degrees.
  • Typical cooling profiles for such a cooling have the form described in FIG. 3 , wherein the temperature T is spread over the time t. It is readily possible to perform other cooling processes or heatings with the tempering container according to the present invention.
  • Peltier technology competes with the conventional compressor-cooling and absorber-cooling systems. If one compares the costs of the cooling capacity of these cooling systems, then one comes to the conclusion, that Petier elements are more expensive. However, the advantages of the Peltier technology may not be overlooked. In applications that only require low cooling capacities, Peltier elements need substantially less space. The control of the capacity of a Peltier element via the operating current is easy and precise. By simple reversal of the polarity of the current direction Peltier elements can be used both for heating as well as for cooling. A further advantage of a Peltier cooling is an inexpensive external cooling supply for the counter cooling of the elements.
  • Peltier elements which should increase the capacity
  • Peltier elements which are mounted on top of each other, as well as elements in multiple-stage design.
  • Peltier elements are not suitable for rapid cooling steps, as they are required according to standards in the case of devices for testing petroleum. Such coolings occur with a Stirling cooler or compressor cooler.
  • compressor coolers must be designed as at least two-stage, which makes them extremely expensive and large. The same applies to Stirling coolers.
  • the tempering container or its sample receiving space must be cooled down rapidly to specific temperature levels and the temperature attained should be able to be kept constant, while the sample in the sample glass or a measurement container assumes the temperature of the temperature container via heat convection and/or heat radiation.
  • a method for setting a temperature in a tempering container configured for receiving a sample comprising:
  • the invention provides for the following:
  • the invention uses the possibility of storing and as required releasing heat or cooling energy with the aid of Peltier elements.
  • the storage block made of metal is located between the Peltier element and the additional Peltier element. This metal block is measured such that it can store a sufficient quantity of heat energy for the required application and can receive and release this heat quantity sufficiently rapidly.
  • Materials with high specific heat capacity and heat conductivity for example, aluminum, copper, brass, gold, silver, magnesium, etc. are well suited as material for such a heat- or cooling storage.
  • the temperature level in the container is adjusted with the Peltier element and thus is advantageously kept constant or is changed continuously.
  • the heating or cooling of the storage block occurs to an extent above or under the desired target temperature, that the heat- and cooling quantity contained in the storage block and which can be discharged to the container via the Peltier element is sufficient, to attain the desired target temperature of the container, preferably within a predefined time span.
  • the required assessment of the heat- or cooling quantity is possible simply by taking into consideration the quantities to be cooled and their specific heat, wherein at the same time possible environmental influences such as heat convection and radiation of heat are taken into consideration. For a person skilled in the art it represents no difficulty to select the required materials and dimensionings of the storage block and the tempering container, in order to achieve a rapid transfer of sufficient heat quantities.
  • the storage capacity of the storage block for storing heat- or cooling energy is assessed to be greater than the heat- or cooling quantity required for a desired temperature change of the container.
  • the container In order to have sufficient heat- or cooling quantities available, it is useful, if when the container is cooled down to or in the direction of the desired target temperature the temperature of the storage block is lowered to a lower value than the target temperature and for the cooling of the container the Peltier element is traversed with current such that it cools the container and permits the throughflow of the cooling quantities contained in the storage block.
  • this target temperature is kept constant with the Peltier element for a predefined time span and thus at least one, preferably abrupt or linear heating or cooling is performed to a desired target temperature.
  • the Peltier element or the Peltier element cascade is heated or cooled on its rear surface turned away from the container, preferably depending on the desired temperature setting in the storage block. This approach is assisted if when the container is cooled the Peltier element is switched to full power and shortly before or upon attaining the target temperature is switched in a control mode for keeping the temperature of the container constant.
  • the setting of the temperature is performed for a tempering container, in which a measuring unit is arranged for the determination of temperature-dependent material parameters, in particular of the viscous properties of samples, preferably of petroleum products, which measuring unit is tempered or is kept at a desired target temperature for the measurements.
  • the storage block Due to the arrangement of the storage block between the (first) Peltier element in heat contact with the container outer wall and the additional (further) Peltier element on the rear of the storage block turned away from the container, it is easily possible to rapidly cool the storage block and sufficiently rapidly to provide a heat quantity or cooling quantity, which suffices, in order to cool the tempering container to a desired temperature within a predefined time span. This temperature can be kept constant with the Peltier element arranged on the container outer wall or can be changed in a predefined manner.
  • Peltier elements it is possible to arrange a multiplicity of Peltier elements about the outer wall surface of the tempering container.
  • two to four Peltier elements are provided, which are arranged at equal distances along the circumference of the container.
  • Each of these Peltier elements is provided with its own storage block.
  • a continuous storage block could also be provided in the form of a storage ring.
  • an additional Peltier element is assigned to each Peltier element on the rear surface of the storage block turned away from the container.
  • an annular storage block a number of additional Peltier elements or Peltier element cascades can be provided exceeding the number of Peltier elements. It is essential, that the additional Peltier elements can cool the storage block sufficiently low or heat it within a desired time span.
  • the Peltier element or the Peltier element cascade are provided on their container-distant surface with a heat exchanger, with which the Peltier elements or the Peltier element cascade can be heated or cooled off.
  • the Peltier elements are welded on, soldered on, affixed or fastened in another way.
  • the flat Peltier elements are in good heat transfer contact with the container wall. That can be effected, for example, by areas of the container wall designed flat or by use of heat-conducting intermediate pieces or filling materials in the existing interspaces.
  • control unit adjusts the temperature level in the container with the Peltier element and if necessary keeps it constant or changes it continuously.
  • a temperature measuring unit which is connected to the control unit, is arranged inside the container or the sample receiving space.
  • the control unit controls the Peltier elements at the relevant points in time and at the same time measures the temperature inside the tempering container. Depending on the temperature measured, the control of the direct current flowing through the Peltier elements or the pole reversal or the change of current direction takes place, with which the current flows through the Peltier elements.
  • the present invention it is possible during the heating or cooling down of the storage block to adjust the temperature level in the container with the Peltier element and to collect the surplus energy at the beginning of such a ramp and make it available for attaining the target temperature in lower temperature ranges.
  • the ramp is operated in an energy-optimized manner and more extreme target temperatures become possible.
  • the tempering container according to the present invention is especially well suited for the tempering of measuring units for the determination of the viscous properties of samples, preferably of petroleum products or for the cooling of tempering containers, in which such measuring units are used and should be kept at a specific temperature and should be cooled or heated from this temperature in the direction towards a predefined target temperature.
  • FIG. 1 is a schematic diagram illustrating a principle setup of a device according to the invention
  • FIG. 2 is a schematic view of a measuring unit used in the tempering container, as it is used for the CFPP measuring of petroleum products, in particular diesel fuel;
  • FIG. 3 is a graph illustrating a tempering course typical for the measuring process according to the invention.
  • the Peltier element 3 that is connected with contact for heat transfer to the outer wall surface of a tempering container 2 .
  • the Peltier element 3 which is also referred herein as the first Peltier element, can be equipped with a counter-cooler 6 .
  • a storage block 4 is fastened to the surface of the Peltier element 3 that is averted from the container 2 .
  • An additional Peltier element 5 or a Peltier element cascade is connected to the container-distal rear surface of the storage block 4 .
  • the Peltier element 5 is equipped with a counter-cooling unit 6 , which is supplied with fluid by a fluid-cooling or heating unit 10 .
  • the storage block 4 can perform the function of the counter-cooler for the Peltier element 3 .
  • a temperature measuring unit 11 is located inside the tempering container 2 or its sample receiving space. An output signal of the temperature measuring unit 11 is applied to a control unit 7 .
  • the control unit 7 controls current regulators 8 and 9 (closed-loop control units).
  • the current regulator 8 regulates the current direction and the current strength of the direct current flowing through the Peltier element 3 .
  • the regulating unit 9 controls the current strength and the flow direction of the direct current through the additional Peltier element 5 .
  • the cross section of the tempering container 2 can be arbitrarily selected or is adapted to the outer form of the measuring unit 1 used in the container 2 .
  • the storage block 4 is at a rule formed from a cuboid metal block.
  • the Peltier element 3 can, for example, be switched on constantly in order to cool the storage block 4 .
  • the additonal Peltier element 5 can be switched, so that it also cools the storage block 4 and thus also lowers the temperature in the sample receiving space of the container 2 .
  • the Peltier element 3 can also generate just as much heat or cold, as is necessary, in order to keep the container 2 at a constant temperature and to cool down the storage block 4 as much as possible, wherefore the Peltier element 3 is actually operated in the heating circuit and the storage block 4 functions as counter cooling.
  • a positive flow of heat i.e., for raising the temperature
  • the amount of heat available is referred to as a heat quantity.
  • a negative flow of heat i.e., heat exchange for lowering the temperature
  • the amount of heat to be “absorbed” is referred to as a cooling quantity. If a process is described herein as a cooling quantity flowing in a given direction, it is synonymous with a corresponding heat quantity flowing in the opposite direction.
  • the container-close Peltier element 3 is traversed or switched in the reverse direction with current, so that the cooling quantity of the storage block 4 lying at a lower temperature runs into the container 2 and additionally still actively cools the container 2 .
  • the container-close Peltier element 3 will be operated primarily in the heating mode and the control- and regulating unit 7 regulates the heat supply and removal to or from container 2 according to the temperature determined with the at least one temperature sensor 11 .
  • the control- and regulating unit 7 regulates the heat supply and removal to or from container 2 according to the temperature determined with the at least one temperature sensor 11 .
  • several temperature sensors can also be installed in container 2 .
  • the temperature of the storage block 4 before the removal of the cooling quantity is substantially less than the temperature in container 2 .
  • the Peltier element 3 is switched into the heating mode and tempers container 2 and protects the latter at the same time against the temperature prevailing in the storage block 4 , which would otherwise cool container 2 via the Peltier element 3 .
  • the Peltier element 5 can always be operated with the same, preferably maximum, operating current and is switched on and off by the control- and regulating unit 7 only at the beginning and end of the measurement.
  • Peltier element cascades are used in order to obtain lower temperatures, depending on the temperature desired these can be switched on and off. Temperature jumps close to room temperature and also keeping the sample receiving space 15 of the container 2 constant at high temperatures require only one Peltier element 5 , whereas the Peltier element cascade is switched on to attain lower temperatures.
  • the Peltier element 3 on the container side is switched into the cooling mode at full power with maximum operating current and the temperature of the storage block 4 is available for the tempering of the sample receiving space 15 . No later than from the attaining of the desired target temperature of the sample receiving space 15 , the Peltier element 3 goes again into the regulating mode and the operating current is regulated depending on the target temperature attained.
  • a control algorithm is selected which reduces the cooling even before the target temperature is attained in the container 2 , in order to prevent a strong overload of the temperature values in the sample receiving space 15 .
  • Peltier elements can also be used as heating elements by reversal of the polarity of the current direction, the operation of the arrangement is in principle also possible as a heating mechanism.
  • FIG. 2 shows the principle measuring setup for determining the filterability limit of Diesel fuels or heating oil.
  • a measuring unit 1 is inserted into the sample receiving space 15 of the tempering container 2 , the setup of which is predefined by the relevant standards EN 116, ASTM D 6371 or DIN EN 16329.
  • the sample fluid to be determined is poured into a glass container 16 .
  • the fluid is sucked off into a test volume 14 via a filter 12 by way of a pump 13 , in particular a vacuum pump.
  • the suctioning and refluxing of the sample fluid at different temperatures from or into the sample receiving space 15 is carried out until a sucking in or a reflux of the sample fluid can no longer be carried out in the predefined time span due to precipitated paraffin particles.
  • the essential part of the measuring process is thereby the tempering of the sample receiving space 15 of the container 2 or the setting of the temperature in the measuring unit 1 , that is, of the temperature of the sample fluid.
  • This setting is optimally achieved with the tempering unit according to the present invention or with the approach according to the present invention.
  • FIG. 3 shows a tempering course typical for such a measuring process.
  • the tempering chamber 2 is cooled to ⁇ 34° C. in the course of the measurement preparation according to standards.
  • the Peltier elements 3 and 5 thereby cool at full power.
  • the temperature of the tempering chamber 2 is kept constant with the Peltier element 3 , while the Peltier element 5 continues to cool the storage element.
  • the glass container 16 with the sample to be tested or the entire measuring unit 1 are inserted into the sample receiving space 15 of the tempering container 2 .
  • the sample temperature is measured with an additional temperature measuring unit 17 in the sample glass or a filter holder and if necessary transmitted to a control- and evaluation unit 7 for the automatic test execution.
  • the measurement of the temperature-dependent properties takes place now according to standards starting from a sample temperature of 20° C. falling one degree at a time. In this time, the temperature of the tempering container 2 continues to be kept constant with Peltier element 3 and the storage block 4 continues to be cooled off with the additional Peltier element 5 . If the sample temperature has reached ⁇ 20° C., the rapid cooling off of the sample chamber to ⁇ 51° C. starts. The time stipulated according to standards for the temperature jump is reached here through rapid emptying of the storage block 4 . Additional temperature ramps and steps can be implemented in a comparable way.

Abstract

A method for setting a temperature in a tempering container with a Peltier element in heat transfer contact to the container, a storage block of metallic material in heat transfer contact with an opposite side of the Peltier element, and a further Peltier element or Peltier element cascade in heat transfer contact with a rear surface of the storage block. A temperature level of the container is changed towards a desired target temperature by heating or cooling the storage block with the further Peltier element or cascade towards the target temperature or beyond the target temperature. A rapid temperature change is caused in the container by switching a current flow direction of the Peltier element to heat or cool the container and at the same time releasing a transfer of a heat quantity or cooling quantity contained in the storage block to the container.

Description

    CROSS-REFERENCE TO RELATED APPLICATION
  • This application claims the priority, under 35 U.S.C. §119, of Austrian patent application A 50127/2014, filed Feb. 20, 2014; the prior application is herewith incorporated by reference in its entirety.
  • BACKGROUND OF THE INVENTION Field of the Invention
  • The invention relates to a method for setting the temperature in a tempering container equipped for the reception of a sample using at least one Peltier element fixed to the outer wall surface of the container while ensuring a heat transfer contact. Furthermore, the invention relates to a tempering container for implementing this method.
  • Such tempering containers can have a different setup or form, for example, rectangular or circular circumference and be provided for different purposes. In particular, it is also possible with such tempering containers to comply with standard test and measurement conditions, in particular for petroleum products. Here it is a matter above all of standard test conditions, for example, for the measurement of CFPP (Cold Filter Plugging Point), which determines the limit of filterability of petroleum products.
  • The term filterability limit or Cold Filter Plugging Point of the temperature limit values of the filterability designates a low-temperature property of diesel fuel and heating oil EL (Extra Light). This is the temperature in degrees Celsius, at which a test filter under defined conditions clogs as the result of precipitated (n)-paraffin. In this method, the sample is cooled down at a constant rate and thereby is conveyed at defined distances through a test filter. Before reaching the filterability limit at the so-called Cloud Point (CP) crystals are already formed, which, however, still pass through the filter. If the crystals become too large, the filter clogs. The magnitudes tested are the Cloud Point, in which the turbidity of the sample is optically examined through mist clouds of the precipitated paraffin, etc. and is irradiated at defined points in time, and the Pour Point Test, in which a test of the flowability of the tempered sample is performed. However, other tests of tempered samples with respect to their physical properties such as viscosity, rheological properties, etc. are conceivable using the method and the device according to the present invention.
  • For the most part, precise standards specifications, which specify temperature profiles to be complied with, form the basis of such measurement methods. For the CFPP of diesel, for example, these are EN116, ASTM D 6371 and DIN EN 16329. These standards stipulate precise temperature profiles for a tempering container, in this case a cooling chamber, in which a glass container is inserted at a distance to the inner wall of the cooling chamber, which glass container contains the sample to be tested. A lid is placed airtight on the glass container, which via a conduit in the lid transfers a defined sample quantity by means of a vacuum pump up to a mark in a test volume. For the CFPP-test, a sieve is mounted with defined mesh width in the sample path to the test volume, through which the sample is pumped. The temperature of the sample is measured and with each temperature drop by a degree a sampling of the fuel forming the sample is made by means of the pump. With lower temperatures the paraffin in the diesel begins to flocculate, floating particles settle in the filter sieve and clog it. If the filling time for the test volume thus exceeds a specific time span or the fuel no longer completely returns from the test volume into the glass container, this is regarded as the filterability limit according to CFPP. According to standards, it is thereby provided, that the temperature in the tempering chamber is set in advance to −34° C. and the sample is measured, that after the measurements at this temperature the container is cooled down to −51° C. and is measured at this temperature and that finally a cooling and measurement takes place at −67° C. The cooling thereby has—as stipulated—to occur rapidly. Very tight time constraints for the cooling process of the tempering container have to be adhered to, and accordingly the cooling capacity must be sufficient, in order, for example, within 150 seconds to cool down the tempering container enclosing the sample container in a stipulated time span by for example 17 degrees. Typical cooling profiles for such a cooling have the form described in FIG. 3, wherein the temperature T is spread over the time t. It is readily possible to perform other cooling processes or heatings with the tempering container according to the present invention.
  • The Peltier technology competes with the conventional compressor-cooling and absorber-cooling systems. If one compares the costs of the cooling capacity of these cooling systems, then one comes to the conclusion, that Petier elements are more expensive. However, the advantages of the Peltier technology may not be overlooked. In applications that only require low cooling capacities, Peltier elements need substantially less space. The control of the capacity of a Peltier element via the operating current is easy and precise. By simple reversal of the polarity of the current direction Peltier elements can be used both for heating as well as for cooling. A further advantage of a Peltier cooling is an inexpensive external cooling supply for the counter cooling of the elements.
  • However, due to the relatively low cooling capacity of the Peltier elements high dynamic performance requirements such as for tempering containers, which are needed particularly for satisfying the above-described standards, for the most part cannot be met. If large temperature differences must be overcome in the shortest time, a Peltier element cannot be used due to its limited cooling capacity at high temperature differences.
  • Of course there are single-stage and multiple-stage arrangements with Peltier elements, which should increase the capacity, for example, Peltier elements, which are mounted on top of each other, as well as elements in multiple-stage design. However, Peltier elements are not suitable for rapid cooling steps, as they are required according to standards in the case of devices for testing petroleum. Such coolings occur with a Stirling cooler or compressor cooler. However, compressor coolers must be designed as at least two-stage, which makes them extremely expensive and large. The same applies to Stirling coolers.
  • SUMMARY OF THE INVENTION
  • It is accordingly a primary object of the invention to provide a method and a device for setting a temperature of a tempering container which overcomes the above-mentioned and other disadvantages of the heretofore-known devices and methods of this general type and to provide a sample container with a tempering container, particularly for measurement processes according to standards, which is small and light and operates precisely and facilitates a rapid temperature change. In particular, the tempering container or its sample receiving space must be cooled down rapidly to specific temperature levels and the temperature attained should be able to be kept constant, while the sample in the sample glass or a measurement container assumes the temperature of the temperature container via heat convection and/or heat radiation.
  • With the foregoing and other objects in view there is provided, in accordance with the invention, a method for setting a temperature in a tempering container configured for receiving a sample, the method comprising:
  • providing the tempering container with
      • a first Peltier element in heat transfer contact to an outer wall surface of the container;
      • a storage block of metallic material in heat transfer contact with a surface of the Peltier element averted from the container;
      • a further Peltier element or a Peltier element cascade in heat transfer contact with a rear surface of the storage block averted away from the first Peltier element;
  • changing a temperature level of the container towards a desired target temperature, heating or cooling the storage block with the further Peltier element or Peltier element cascade towards the target temperature or beyond the target temperature; and
  • causing a rapid temperature change in the container by switching a current flow direction of the first Peltier element to heat or cool the container with the first Peltier element in the direction towards the desired target temperature and at the same time releasing a transfer of a heat quantity or cooling quantity contained in the storage block to the container in order to amplify a heating or cooling resulting from the first Peltier element.
  • In other words, the invention provides for the following:
      • a storage block made from metallic material is fixed to the surface of the Peltier element turned away from the container while ensuring a heat transfer contact;
      • an additional Peltier element or a Peltier element cascade is fixed to the rear surface of the storage block turned away from the Peltier element while ensuring a heat transfer contact;
      • to change the temperature level of the container towards a desired target temperature the storage block is heated or cooled down with the additional Peltier element or the Peltier element cascade in the direction of this target temperature or beyond; and
      • for the realization of a rapid temperature change in the container the current flow direction of the Peltier element is switched such that the latter heats or cools the container in the direction towards the desired target temperature and thus at the same time releases the transfer of the heat quantity or cooling quantity contained in the storage block by itself to the container in order to strengthen the heating or cooling resulting from the Peltier element.
  • Such an approach is useful particularly for the performance of measurements of petroleum products, preferably for determining the filterability of diesel fuels. In particular, the regulations according to DIN EN 116 can be satisfied with such a method.
  • The invention uses the possibility of storing and as required releasing heat or cooling energy with the aid of Peltier elements. For this purpose it is essential that the storage block made of metal is located between the Peltier element and the additional Peltier element. This metal block is measured such that it can store a sufficient quantity of heat energy for the required application and can receive and release this heat quantity sufficiently rapidly. Materials with high specific heat capacity and heat conductivity, for example, aluminum, copper, brass, gold, silver, magnesium, etc. are well suited as material for such a heat- or cooling storage.
  • It should be noted in this connection that with the method according to the present invention and the device according to the present invention both high cooling rates as well as heating rates can be achieved. However, special advantages arise in cooling the temperature of a tempering container receiving a sample.
  • In order not to influence or to specifically influence the temperature in the tempering container in the approach according to the present invention, it can be provided, that during the heating or cooling of the storage block the temperature level in the container is adjusted with the Peltier element and thus is advantageously kept constant or is changed continuously.
  • In order to attain a sufficiently rapid and reliable temperature change in the tempering container, it is provided according to the present invention, that the heating or cooling of the storage block occurs to an extent above or under the desired target temperature, that the heat- and cooling quantity contained in the storage block and which can be discharged to the container via the Peltier element is sufficient, to attain the desired target temperature of the container, preferably within a predefined time span. The required assessment of the heat- or cooling quantity is possible simply by taking into consideration the quantities to be cooled and their specific heat, wherein at the same time possible environmental influences such as heat convection and radiation of heat are taken into consideration. For a person skilled in the art it represents no difficulty to select the required materials and dimensionings of the storage block and the tempering container, in order to achieve a rapid transfer of sufficient heat quantities.
  • In order to cope with all eventualities, it is provided that the storage capacity of the storage block for storing heat- or cooling energy is assessed to be greater than the heat- or cooling quantity required for a desired temperature change of the container. Through appropriate activation of the Peltier element the heat transfer from the storage block to the tempering container can be interrupted upon attaining a predefined target temperature and then with this Peltier element the target temperature can be precisely adjusted or the tempering container can be maintained at this temperature or the temperature attained can be changed.
  • In order to have sufficient heat- or cooling quantities available, it is useful, if when the container is cooled down to or in the direction of the desired target temperature the temperature of the storage block is lowered to a lower value than the target temperature and for the cooling of the container the Peltier element is traversed with current such that it cools the container and permits the throughflow of the cooling quantities contained in the storage block.
  • If necessary it is possible, that after attaining the desired target temperature in the container this target temperature is kept constant with the Peltier element for a predefined time span and thus at least one, preferably abrupt or linear heating or cooling is performed to a desired target temperature.
  • For an efficient operation of the first Peltier element and of the further Peltier element and a rapid cooling of the storage block it is advantageous if the Peltier element or the Peltier element cascade is heated or cooled on its rear surface turned away from the container, preferably depending on the desired temperature setting in the storage block. This approach is assisted if when the container is cooled the Peltier element is switched to full power and shortly before or upon attaining the target temperature is switched in a control mode for keeping the temperature of the container constant.
  • According to the present invention it is provided, that the setting of the temperature is performed for a tempering container, in which a measuring unit is arranged for the determination of temperature-dependent material parameters, in particular of the viscous properties of samples, preferably of petroleum products, which measuring unit is tempered or is kept at a desired target temperature for the measurements.
  • With the above and other objects in view there is also provided, in accordance with the invention, a tempering that is characterized in:
      • that a storage block made from metallic material is fixed to the surface of the Peltier element turned away from the container while ensuring a heat transfer contact,
      • that an additional Peltier element or a Peltier element cascade is fixed to the rear surface of the storage block turned away from the Peltier element while ensuring a heat transfer contact,
      • that to change the temperature level of the container towards a desired target temperature or in the direction of this target temperature a control unit is provided for the current flow through the Peltier element and the additional Peltier element or the Peltier element cascade, with which control unit the storage block can be heated or cooled down with the additional Peltier element or the Peltier element cascade in the direction of this target temperature or beyond and
      • that the control unit for the realization of a rapid temperature change in the container or its sample receiving space switches the current flow direction of the Peltier element such that the latter heats or cools the container in the direction towards the desired target temperature and thus at the same time releases the transfer of the heat quantity or cooling quantity contained in the storage block to the container in order to strengthen the heating or cooling resulting from the Peltier element.
  • Due to the arrangement of the storage block between the (first) Peltier element in heat contact with the container outer wall and the additional (further) Peltier element on the rear of the storage block turned away from the container, it is easily possible to rapidly cool the storage block and sufficiently rapidly to provide a heat quantity or cooling quantity, which suffices, in order to cool the tempering container to a desired temperature within a predefined time span. This temperature can be kept constant with the Peltier element arranged on the container outer wall or can be changed in a predefined manner.
  • It is possible to arrange a multiplicity of Peltier elements about the outer wall surface of the tempering container. Advantageously, two to four Peltier elements are provided, which are arranged at equal distances along the circumference of the container. Each of these Peltier elements is provided with its own storage block. In principle, a continuous storage block could also be provided in the form of a storage ring. Advantageously, an additional Peltier element is assigned to each Peltier element on the rear surface of the storage block turned away from the container. When an annular storage block is used a number of additional Peltier elements or Peltier element cascades can be provided exceeding the number of Peltier elements. It is essential, that the additional Peltier elements can cool the storage block sufficiently low or heat it within a desired time span.
  • In order to assist the function of the additional Peltier elements, it can be provided, that the Peltier element or the Peltier element cascade are provided on their container-distant surface with a heat exchanger, with which the Peltier elements or the Peltier element cascade can be heated or cooled off.
  • The Peltier elements are welded on, soldered on, affixed or fastened in another way. In the case of a container having a curved outer surface, it should be ensured that the flat Peltier elements are in good heat transfer contact with the container wall. That can be effected, for example, by areas of the container wall designed flat or by use of heat-conducting intermediate pieces or filling materials in the existing interspaces.
  • It is useful for the operation, if the control unit adjusts the temperature level in the container with the Peltier element and if necessary keeps it constant or changes it continuously.
  • It is useful for the temperature setting if a temperature measuring unit, which is connected to the control unit, is arranged inside the container or the sample receiving space.
  • The control unit controls the Peltier elements at the relevant points in time and at the same time measures the temperature inside the tempering container. Depending on the temperature measured, the control of the direct current flowing through the Peltier elements or the pole reversal or the change of current direction takes place, with which the current flows through the Peltier elements.
  • According to the present invention it is possible during the heating or cooling down of the storage block to adjust the temperature level in the container with the Peltier element and to collect the surplus energy at the beginning of such a ramp and make it available for attaining the target temperature in lower temperature ranges. Thus, the ramp is operated in an energy-optimized manner and more extreme target temperatures become possible.
  • The tempering container according to the present invention is especially well suited for the tempering of measuring units for the determination of the viscous properties of samples, preferably of petroleum products or for the cooling of tempering containers, in which such measuring units are used and should be kept at a specific temperature and should be cooled or heated from this temperature in the direction towards a predefined target temperature.
  • Other features which are considered as characteristic for the invention are set forth in the appended claims.
  • Although the invention is illustrated and described herein as embodied in method for setting the temperature and tempering container, it is nevertheless not intended to be limited to the details shown, since various modifications and structural changes may be made therein without departing from the spirit of the invention and within the scope and range of equivalents of the claims.
  • The construction and method of operation of the invention, however, together with additional objects and advantages thereof will be best understood from the following description of specific embodiments when read in connection with the accompanying drawings.
  • BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING
  • FIG. 1 is a schematic diagram illustrating a principle setup of a device according to the invention;
  • FIG. 2 is a schematic view of a measuring unit used in the tempering container, as it is used for the CFPP measuring of petroleum products, in particular diesel fuel; and
  • FIG. 3 is a graph illustrating a tempering course typical for the measuring process according to the invention.
  • DETAILED DESCRIPTION OF THE INVENTION
  • Referring now to the figures of the drawing in detail and first, particularly, to FIG. 1 thereof, there is shown a Peltier element 3 that is connected with contact for heat transfer to the outer wall surface of a tempering container 2. The Peltier element 3, which is also referred herein as the first Peltier element, can be equipped with a counter-cooler 6. A storage block 4 is fastened to the surface of the Peltier element 3 that is averted from the container 2. An additional Peltier element 5 or a Peltier element cascade is connected to the container-distal rear surface of the storage block 4. The Peltier element 5 is equipped with a counter-cooling unit 6, which is supplied with fluid by a fluid-cooling or heating unit 10. The storage block 4 can perform the function of the counter-cooler for the Peltier element 3.
  • A temperature measuring unit 11 is located inside the tempering container 2 or its sample receiving space. An output signal of the temperature measuring unit 11 is applied to a control unit 7. The control unit 7 controls current regulators 8 and 9 (closed-loop control units). The current regulator 8 regulates the current direction and the current strength of the direct current flowing through the Peltier element 3. The regulating unit 9 controls the current strength and the flow direction of the direct current through the additional Peltier element 5.
  • The cross section of the tempering container 2 can be arbitrarily selected or is adapted to the outer form of the measuring unit 1 used in the container 2. The storage block 4 is at a rule formed from a cuboid metal block.
  • The Peltier element 3 can, for example, be switched on constantly in order to cool the storage block 4. At the same time, the additonal Peltier element 5 can be switched, so that it also cools the storage block 4 and thus also lowers the temperature in the sample receiving space of the container 2. The Peltier element 3 can also generate just as much heat or cold, as is necessary, in order to keep the container 2 at a constant temperature and to cool down the storage block 4 as much as possible, wherefore the Peltier element 3 is actually operated in the heating circuit and the storage block 4 functions as counter cooling.
  • With regard to the terminology used herein, a positive flow of heat (i.e., for raising the temperature) is referred to as heating and the amount of heat available is referred to as a heat quantity. A negative flow of heat (i.e., heat exchange for lowering the temperature) is referred to as cooling. The amount of heat to be “absorbed” is referred to as a cooling quantity. If a process is described herein as a cooling quantity flowing in a given direction, it is synonymous with a corresponding heat quantity flowing in the opposite direction.
  • If a large jump in temperature is needed, then the container-close Peltier element 3 is traversed or switched in the reverse direction with current, so that the cooling quantity of the storage block 4 lying at a lower temperature runs into the container 2 and additionally still actively cools the container 2. Thus, the possibility arises of tempering the tempering body with high dynamics. Since the temperature of the container 2 can be regulated (i.e., closed-loop controlled) by means of a single Peltier element, that is, the Peltier element 3, the regulation is possible very precisely.
  • In this way, cooling rates of 20 degrees in 150 second are readily available.
  • If a measurement of a sample starts, for example, at room temperature, then the preferably more strongly dimensioned additional Peltier element 5 begins to cool at full power. The storage block 4 cools down immediately. If a measuring is desired in container 2 at room temperature, the container-close Peltier element 3 will be operated primarily in the heating mode and the control- and regulating unit 7 regulates the heat supply and removal to or from container 2 according to the temperature determined with the at least one temperature sensor 11. In order to be able to regulate the temperature rapidly and precisely, several temperature sensors can also be installed in container 2.
  • In the event of cooling, the temperature of the storage block 4 before the removal of the cooling quantity is substantially less than the temperature in container 2.
  • To keep the temperature of container 2 constant the Peltier element 3 is switched into the heating mode and tempers container 2 and protects the latter at the same time against the temperature prevailing in the storage block 4, which would otherwise cool container 2 via the Peltier element 3.
  • In a simple design of the invention, the Peltier element 5 can always be operated with the same, preferably maximum, operating current and is switched on and off by the control- and regulating unit 7 only at the beginning and end of the measurement.
  • If Peltier element cascades are used in order to obtain lower temperatures, depending on the temperature desired these can be switched on and off. Temperature jumps close to room temperature and also keeping the sample receiving space 15 of the container 2 constant at high temperatures require only one Peltier element 5, whereas the Peltier element cascade is switched on to attain lower temperatures.
  • If a temperature jump to lower temperatures must be realized, then the Peltier element 3 on the container side is switched into the cooling mode at full power with maximum operating current and the temperature of the storage block 4 is available for the tempering of the sample receiving space 15. No later than from the attaining of the desired target temperature of the sample receiving space 15, the Peltier element 3 goes again into the regulating mode and the operating current is regulated depending on the target temperature attained.
  • Preferably, a control algorithm is selected which reduces the cooling even before the target temperature is attained in the container 2, in order to prevent a strong overload of the temperature values in the sample receiving space 15.
  • Since Peltier elements can also be used as heating elements by reversal of the polarity of the current direction, the operation of the arrangement is in principle also possible as a heating mechanism.
  • FIG. 2 shows the principle measuring setup for determining the filterability limit of Diesel fuels or heating oil. With this experimental arrangement a measuring unit 1 is inserted into the sample receiving space 15 of the tempering container 2, the setup of which is predefined by the relevant standards EN 116, ASTM D 6371 or DIN EN 16329. The sample fluid to be determined is poured into a glass container 16. The fluid is sucked off into a test volume 14 via a filter 12 by way of a pump 13, in particular a vacuum pump. The suctioning and refluxing of the sample fluid at different temperatures from or into the sample receiving space 15 is carried out until a sucking in or a reflux of the sample fluid can no longer be carried out in the predefined time span due to precipitated paraffin particles. The essential part of the measuring process is thereby the tempering of the sample receiving space 15 of the container 2 or the setting of the temperature in the measuring unit 1, that is, of the temperature of the sample fluid. This setting is optimally achieved with the tempering unit according to the present invention or with the approach according to the present invention.
  • FIG. 3 shows a tempering course typical for such a measuring process. The tempering chamber 2 is cooled to −34° C. in the course of the measurement preparation according to standards. The Peltier elements 3 and 5 thereby cool at full power. Upon attaining this target temperature the temperature of the tempering chamber 2 is kept constant with the Peltier element 3, while the Peltier element 5 continues to cool the storage element. Now the glass container 16 with the sample to be tested or the entire measuring unit 1 are inserted into the sample receiving space 15 of the tempering container 2. The sample temperature is measured with an additional temperature measuring unit 17 in the sample glass or a filter holder and if necessary transmitted to a control- and evaluation unit 7 for the automatic test execution. The measurement of the temperature-dependent properties (CFPP) takes place now according to standards starting from a sample temperature of 20° C. falling one degree at a time. In this time, the temperature of the tempering container 2 continues to be kept constant with Peltier element 3 and the storage block 4 continues to be cooled off with the additional Peltier element 5. If the sample temperature has reached −20° C., the rapid cooling off of the sample chamber to −51° C. starts. The time stipulated according to standards for the temperature jump is reached here through rapid emptying of the storage block 4. Additional temperature ramps and steps can be implemented in a comparable way.

Claims (20)

1. A method for setting a temperature in a tempering container configured for receiving a sample, the method comprising:
providing the tempering container with
a first Peltier element in heat transfer contact to an outer wall surface of the container;
a storage block of metallic material in heat transfer contact with a surface of the Peltier element averted from the container;
a further Peltier element or a Peltier element cascade in heat transfer contact with a rear surface of the storage block averted away from the first Peltier element;
changing a temperature level of the container towards a desired target temperature, heating or cooling the storage block with the further Peltier element or Peltier element cascade towards the target temperature or beyond the target temperature; and
causing a rapid temperature change in the container by switching a current flow direction of the first Peltier element to heat or cool the container with the first Peltier element in the direction towards the desired target temperature and at the same time releasing a transfer of a heat quantity or cooling quantity contained in the storage block to the container in order to amplify a heating or cooling resulting from the first Peltier element.
2. The method according to claim 1, which comprises, while heating or cooling the storage block, adjusting the temperature in the container with the first Peltier element and thereby keeping the temperature constant or continuously changing the temperature.
3. The method according to claim 1, which comprises heating or cooling the storage block to above or below the desired target temperature, respectively, so that a heat quantity or cooling quantity contained in the storage block and available for discharge to the container via the first Peltier element is sufficient to attain the desired target temperature of the container.
4. The method according to claim 3, which comprises setting the temperature in the storage block to attain the desired target temperature of the container within a predefined time span.
5. The method according to claim 1, which comprises setting a storage capacity of the storage block for storing heat quantities and cooling quantities to be greater than the heat quantity or cooling quantity required for a desired temperature change of the container.
6. The method according to claim 1, which comprises, during cooling of the container to or towards the desired target temperature, lowering the temperature of the storage block to a lower value than the target temperature and for the cooling the container, traversing the first Peltier element with current such that the first Peltier element cools the container and permits a throughflow of the cooling quantities contained in the storage block.
7. The method according to claim 1, which comprises, upon attaining a desired first target temperature in the container, keeping the first target temperature constant or changing same continuously with the first Peltier element for a predefined time span, and subsequently effecting a temperature change to a further target temperature.
8. The method according to claim 7, which comprises effecting the temperature change to the further target temperature by a substantially abrupt or linear heating or cooling.
9. The method according to claim 1, which comprises placing a measuring unit into the tempering container, the measuring unit being for a determination of temperature-dependent material parameters and tempering the measuring unit or keeping the measuring unit at a desired target temperature for the measurements.
10. The method according to claim 1, which comprises heating or cooling the further Peltier element or the Peltier element cascade on the rear surface averted from the container.
11. The method according to claim 1, which comprises heating or cooling the further Peltier element or the Peltier element cascade on the rear surface averted from the container in dependence on a desired temperature setting in the storage block.
12. The method according to claim 1, which comprises, when the container is cooled, switching the first Peltier element to full power and shortly before or upon attaining the target temperature, switching the first Peltier element to a closed-loop control mode for keeping the temperature of the container constant.
13. A tempering container formed with a sample receiving space, the tempering container comprising:
at least one first Peltier element fixed in heat transfer contact to an outer wall surface of the container;
a storage block of a metallic material fixed in heat transfer contact to surface of said first Peltier element averted from the container;
a further Peltier element or a Peltier element cascade fixed in heat transfer contact to a rear surface of the storage block averted from the said Peltier element;
a control unit connected to said first Peltier element and to said further Peltier element and configured to selectively change a temperature level of the container towards a desired target temperature by setting an electrical current flow through said first Peltier element and said further Peltier element or Peltier element cascade, said control unit being configured to heat or cool the storage block with the additional Peltier element or the Peltier element cascade towards the target temperature or beyond the target temperature; and
said control unit, for realizing a rapid temperature change in the container or the sample receiving space, switching a current flow direction of the first Peltier element to thereby heat or cool the container towards the desired target temperature and at the same time release a transfer of a heat quantity or a cooling quantity contained in the storage block to the container in order to amplify the heating or cooling resulting from the first Peltier element.
14. The tempering container according to claim 13 configured for implementing the method according to claim 1.
15. The tempering container according to claim 13, wherein said control unit is configured, during the heating or the cooling of the storage block, to adjust the temperature level in the container with the first Peltier element and to selectively keep the temperature constant or continuously changing.
16. The tempering container according to claim 13, wherein a capacity of said storage block for storing heat quantities or cooling quantities is greater than a heat quantity or cooling quantity required for a desired temperature change of the container.
17. The tempering container according to claim 13, which further comprises a heat exchanger disposed on a container-distal side of said further Peltier element or Peltier element cascade, for selectively heating or cooling the further Peltier element or Peltier element cascade.
18. The tempering container according to claim 13, which comprises a temperature measuring unit disposed inside the container or the sample receiving space and connected to said control unit.
19. The tempering container according to claim 18, wherein said measuring unit is configured for determining temperature-dependent material parameters.
20. A method of determining a temperature-dependent material parameter of a sample, the method comprising:
providing a tempering container according to claim 13;
placing the sample into the tempering container; and
measuring the temperature-dependent material parameter while setting a controlled temperature in the tempering container.
US14/627,169 2014-02-20 2015-02-20 Method for setting a temperature, and tempering container Abandoned US20150233614A1 (en)

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ATA50127/2014A AT515081B1 (en) 2014-02-20 2014-02-20 Method for setting the temperature and temperature control tank
ATA50127/2014 2014-02-20

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US11643898B2 (en) 2018-10-17 2023-05-09 Schlumberger Technology Corporation Systems and methods for monitoring and/or predicting sagging tendencies of fluids
US20210088499A1 (en) * 2019-09-23 2021-03-25 M-I L.L.C. Automated analysis of drilling fluid
CN111398040A (en) * 2020-03-20 2020-07-10 上海交通大学 Oblique reverse thrust cascade static test device for aircraft engine
GB2614520A (en) * 2021-10-19 2023-07-12 Stanhope Seta Ltd Analytical apparatus

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