With Control Of Heat Added To Or Lost From A Sample Container (e.g., Isothermal Calorimetry) Patents (Class 374/33)
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Patent number: 7097352Abstract: A holder for materials for use in a measuring instrument includes a three-piece housing consisting of an upper housing member, an intermediate housing member and a lower housing member, the three-piece housing defining a first closed cavity and a second closed cavity. A first winding assembly is disposed within the first closed cavity, and a second winding assembly is disposed within the second closed cavity.Type: GrantFiled: October 5, 2004Date of Patent: August 29, 2006Assignee: PerkinElmer LAS, Inc.Inventor: Donald L. Groeschner
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Patent number: 7021820Abstract: A new adiabatic scanning calorimeter allows the thermal mass of a high-pressure reaction vessel to be dynamically compensated during a test. This allows the effective ? factor for the experiment to be reduced to 1.0 without the use of complex pressure balancing equipment. Endothermic events can be quantified and sample specific heats can be measured. The time required for test completion is much shorter than for conventional adiabatic calorimeters, thus considerably improving apparatus productivity. The sensitivity to exotherm detection is at least as good as existing adiabatic calorimeters employing the Heat-Wait-Search strategy, but does depend on the temperature-scanning rate. In addition, the heat of reaction is obtained without reference to the heat capacity of the sample, pressure is measured continuously, reactants may be injected into the test vessel and the sample can be mixed during the test.Type: GrantFiled: July 12, 2004Date of Patent: April 4, 2006Inventor: Simon Chippett
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Patent number: 6953280Abstract: The invention relates to a calorimeter comprising a reactor (1) that is fitted in an intermediate thermostat (2). Said intermediate thermostat (2) cooperates with an external thermostat (3) and comprises a metal block (4) as the heat transfer medium. The inventive calorimeter can be produced at lower costs than those comprising a double-walled reaction vessel and allows especially IR probe analysis.Type: GrantFiled: August 23, 2001Date of Patent: October 11, 2005Assignee: Eidgenössische Technische Hochschule ZürichInventors: Ulrich Fischer, Konrad Hungerbühler, Max Wohlwend, Andreas Zogg
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Patent number: 6869214Abstract: A calorimeter that includes a sample cell, a reference cell, a pressure system that applies a variable pressure to the sample cell, and a pressure controller that controls the pressure applied by the pressure system to the sample cell. By applying identical pressure perturbations to both the sample and reference cells over a range of temperatures, the calorimeter can be used to accurately calculate both the thermal coefficient of expansion of various substances, and the volume change of molecules undergoing a structural transition.Type: GrantFiled: January 30, 2003Date of Patent: March 22, 2005Assignee: MicroCal LLCInventors: Valerian V. Plotnikov, John F. Brandts, J. Michael Brandts
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Patent number: 6860632Abstract: A housing for a material holder includes an intermediate housing member having a generally horizontal member, an upper recess and a lower recess, an upper housing member having a generally horizontal member and a wall defining a material holding chamber, the upper housing member being seated within the upper recess of the intermediate housing member, and a lower housing member having a generally horizontal member, the lower housing member being seated within the lower recess of the intermediate housing member. The upper recess, the generally horizontal member of the intermediate housing member and the generally horizontal member of the upper housing member define a first cavity adapted to receive a first winding assembly, and the lower recess, the generally horizontal member of the intermediate housing member and the generally horizontal member of the lower housing member define a second cavity adapted to receive a second winding assembly.Type: GrantFiled: July 28, 2003Date of Patent: March 1, 2005Assignee: PerkinElmer Instruments LLCInventor: Donald L. Groeschner
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Publication number: 20040001524Abstract: A method and apparatus for thermally investigating a material by driving the material through a temperature profile composed of isothermal and non-isothermal segments is disclosed, which enable determination of a kinetic component in a measured heat flow signal caused by the exposure of the material to the temperature profile.Type: ApplicationFiled: June 9, 2003Publication date: January 1, 2004Inventors: Urs Jorimann, Thomas Hutter
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Patent number: 6648504Abstract: A system and method for obtaining the contact thermal resistance for a sample and pan without a priori knowledge of the properties of either sample, by measuring the reversing heat capacity of a sample and its pan (or an empty pan on the reference side of the DSC) at a long period and a short period during a quasi-isothermal MDSC experiment and then finding the value of contact thermal resistance that makes the short and long period heat capacities match. Several different methods may be used to find the contact thermal resistance using quasi-isothermal MDSC with a long and a short period. Two methods are direct calculation methods that use the results from an MDSC experiment used with model equations to calculate the contact thermal resistance. A third method is another direct calculation method, based upon the phase angle between the heat flow and temperature signals. A fourth and fifth method use curve fitting of the apparent heat capacity for multiple values of pan contact thermal resistance.Type: GrantFiled: March 1, 2002Date of Patent: November 18, 2003Assignee: Waters Investment LimitedInventor: Robert L. Danley
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Patent number: 6632015Abstract: With input compensation-type differential scanning calorimeters of the related art, the power supplied fluctuated even with non-endothermic reference materials, and the reference material side temperature therefore also fluctuated. Mutual interference between feedback loops also made precise temperature control difficult. In the present invention, power supplied to the sample side is changed to compensate for a temperature difference between the sample side and the reference material side using a differential thermal feedback loop, power to be supplied to the reference material side heater to make the reference material side temperature correspond to the program temperature is controlled, and the same amount of the power is also supplied to the sample side with the average temperature feedback loop.Type: GrantFiled: April 18, 2001Date of Patent: October 14, 2003Assignee: Seiko Instruments Inc.Inventor: Jun Nagasawa
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Patent number: 6627451Abstract: A water bath accommodating a calorimetric bomb (2) for measuring the combustion heat of substances with the aid of a calorimeter. The inner tank (3) is enclosed by an outer container (5) forming a water jacket and is shielded from the environment. If several measurements are conducted subsequently, the water found in the inner tank (3) and heated above its initial value through the combustion process taking place in connection with a previous measurement can be at least partially transferred into the outer container (5) with a second or other succeeding measurement prior to conducting it so that at least a part of the combustion heat of the preceding measurement can be used for heating up at least the water jacket in the outer container (5) in connection with the next measurement. Consequently, energy for tempering the water in the water jacket and/or in the water bath can be saved.Type: GrantFiled: May 18, 2001Date of Patent: September 30, 2003Assignee: IKA-Werke GmbH & Co., KGInventors: Hubert Pinhack, Armin Wiesler, Alf-Bernd Ambs
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Patent number: 6572263Abstract: A calorimeter for use in assaying radioactive sources. The calorimeter includes a constant temperature shield and a series of temperature matched shields in which temperature control is provided by electrical resistance, thereby eliminating the need for a water jacket, while providing improved temperature and heat flow control. A labyrinth plug which eliminates air exchange between the sample well and the outside is used to seal the calorimeter. A computer control system monitors the calorimeter to reduce errors introduced by system fluctuations.Type: GrantFiled: April 2, 2001Date of Patent: June 3, 2003Assignee: Westinghouse Savannah River CompanyInventors: Lee A. Refalo, Henry W. Randolph
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Patent number: 6561692Abstract: A modulated differential scanning calorimeter (MDSC) and a method for practicing MDSC that uses two separate temperature difference signals—the difference between the temperatures of the sample and reference positions and the difference between the temperatures of the sample position and a base position. This approach accounts for heat flows associated with the sample and reference pans, and for the difference in sample and pan heating rates to provide more accurate heat flow measurement and improve resolution. It also greatly reduces or eliminates the frequency dependence of the heat capacity calibration factor, which allows for the use of shorter modulation periods. Shorter modulation periods allow the use of higher underlying heating rates, allowing users to decrease the duration of their MDSC experiments.Type: GrantFiled: January 26, 2001Date of Patent: May 13, 2003Assignee: TA Instruments-Waters LLCInventor: Robert L. Danley
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Publication number: 20030086473Abstract: A sampling device for thermal analysis of solidifying metal, particularly compacted graphite iron is disclosed, comprising a container (2) essentially cylindrical, open at the top intended to be immersed down into and filled with a liquid metal to be analyzed, at least one temperature responsive sensor member (4), preferably two, a protective tubing (14) concentrically enclosing said sensor(s), arranged inside said container (2) and supported by a sensor support member (15) arranged above said container and attached to the container (2) by legs (16) and intended to guide and keep the sensors (4) in position, when immersed in the solidifying metal sample quantity (3) during analysis, said container (2) comprises an interior surface (17) intended to contact the sample quantity (3) during analysis, and an exterior surface (18) intended to contact the ambient atmosphere, said surfaces (17 and 18) being joined at the mouth (12) of the container (2), being equally spaced forming a closed insulating space (8), whereType: ApplicationFiled: December 2, 2002Publication date: May 8, 2003Inventors: Patrik Popelar, Henrik Nystrom
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Patent number: 6523998Abstract: An improved differential thermal analysis/differential scanning calorimetry (collectively, DSC) assembly with a furnace block assembly having a measurement chamber and a furnace heater. The measurement chamber has a sensor assembly for receiving a sample material and a reference material. The furnace block assembly is coupled to a generally cylindrical cooling flange through a distributed thermal resistor that allows a constrained heat flow between the furnace assembly and cooling flange. The thermal resistor can also withstand the mechanical stresses associated with the differential expansion and contraction of the furnace assembly and cooling flange without permanent deformation of the thermal resistor. The cooling flange can be coupled to various cooling devices, permitting operation of the overall DSC instrument in a variety of temperature regimes for a variety of applications.Type: GrantFiled: January 26, 2001Date of Patent: February 25, 2003Assignee: TA Instruments, Inc.Inventors: Robert L. Danley, John W. Schaefer
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Publication number: 20030026319Abstract: To provide a differential scanning calorimeter in which rise and fall of temperatures of a sample and a reference substance follow rise and fall of temperature of a heat sink with excellent response maintaining a structure of a differential scanning calorimeter having a structure of providing stability of a base line constituting a characteristic of a heat flux type while achieving response equivalent to or faster than that of a power compensation type, in a structure of a heat flux type differential scanning calorimeter in which a heat flow path between a sample holder and a heat sink is formed by a metallic material having excellent heat conductance, heaters for power compensation are attached to the sample holder and a reference holder.Type: ApplicationFiled: July 12, 2002Publication date: February 6, 2003Inventor: Ryoichi Kinoshita
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Patent number: 6497509Abstract: A method of measuring the absolute value of thermal conductivity of low thermal conducting solid materials is disclosed. Thermal conductivity and heat capacity of the sample are determined simultaneously in a single measurement with the prerequisite that these values are frequency independent. This method is realized on power-compensated differential scanning calorimeters without any modification in the measuring system. DSC is calibrated in a standard way for temperature and heat flow. The method uses temperature-time profiles consisting of one fast temperature jump of 0.5 to 2 K and an isotherm. The measuring time for each temperature is less than 1 min. As input parameters only sample thickness and contact area with the DSC furnace (or sample diameter if the sample is disk shaped) are needed together with sample mass. In addition to the sample thermal conductivity and heat capacity the effective thermal contact between sample and DSC furnace is determined.Type: GrantFiled: June 8, 2001Date of Patent: December 24, 2002Assignee: PerkinElmer Instruments LLCInventors: Mikhail Merzliakov, Christoph Schick
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Patent number: 6488406Abstract: A method for calculating sample heat flow in a differential scanning calorimeter. A preferred embodiment of the invention calculates the heat flow to the sample while accounting for the effect of heat storage in the sample pans and the difference in heating rate between sample and reference. Accounting for heat flow associated with the pans and the difference between sample and reference heating rates gives a more accurate sample heat flow measurement and improves resolution, which is the ability to separate closely spaced thermal events in the heat flow result.Type: GrantFiled: January 24, 2001Date of Patent: December 3, 2002Assignee: TA Instruments-Waters, LLCInventor: Robert L. Danley
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Patent number: 6431747Abstract: A sensor for a heat flux differential scanning calorimeter in which one absolute temperature measurement and two differential temperature measurements are used. The sensor is calibrated and used based on a four-term model heat flow equation. The calibration is carried out in two experiments which are used to calculate the sensor thermal resistance for the sample and reference positions, respectively, and the sensor heat capacity for the sample and reference positions, respectively. Differential scanning calorimeters using this sensor exhibit improved resolution, improved baseline performance and improved dynamic response.Type: GrantFiled: August 23, 2000Date of Patent: August 13, 2002Assignee: TA Instruments, Inc.Inventor: Robert L. Danley
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Patent number: 6428203Abstract: A power compensation differential scanning calorimeter that uses one absolute temperature measurement, two differential temperature measurements, a differential power measurement, and a five-term heat flow equation to measure the sample heat flow. The calorimeter is calibrated by running two sequential calibration experiments. In a preferred embodiment, the first calibration experiment uses empty sample and reference pans, and the second calibration experiment uses sapphire specimens in the sample and reference holders. In an alternate embodiment, sapphire calibration specimens are used in both the first and second calibration experiments.Type: GrantFiled: August 23, 2000Date of Patent: August 6, 2002Assignee: Ta Instruments, Inc.Inventor: Robert L. Danley
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Patent number: 6402369Abstract: Provided are, among other things, devices for and methods for performing thermal signature assays on a two or more samples in an array, using active/control base thermopiles, the method comprising: [a] performing a heat transfer to the two or more samples in each of a two or more containers, using at least one base thermopile in thermal communication with the two or more containers; and [b] determining a total heat transferred to the samples by the base thermopile in step [a]; and [c] sensing in real time a temperature difference between a first sample and a second sample of the two or more samples resulting from performing step [a].Type: GrantFiled: November 2, 1999Date of Patent: June 11, 2002Assignee: Sarnoff CorporationInventors: David Norman Ludington, Thomas Louis Fare, Dominic Joseph Lo Iacono, Timothy James Davis, Helen Jiang Semus, Paul John Stabile, Frank Guarnieri, Russell Todd Granzow, Peter J. Zanzucchi, William Chiang
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Patent number: 5902043Abstract: A heat meter for measuring the amount of heat consumed in a region. A heat exchanger is supplied with heated fluid through an inlet pipe which carries temperature sensors for sending signals to a control. The control also receives signals from a temperature sensor in an outlet pipe carrying fluid away from the region. A low power electric heater is mounted between the sensors to add a known amount of heat to the fluid. The control calculates the heat power consumed in the region based on the temperature difference across the regions and the temperature difference across the region and the temperature difference across the heater.Type: GrantFiled: July 2, 1996Date of Patent: May 11, 1999Assignee: British Gas plcInventors: Barry Leonard Price, Graham Richard Roberts, David Richard Wightman
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Patent number: 5876118Abstract: A calorimeter apparatus includes a facility for rapid cooling of a heating vessel therein. A jacket surrounds the vessel wall. A partition member between the jacket and the vessel wall defines an inlet plenum adjacent the jacket and a spatial gap adjacent the vessel wall. Pressurized cooling gas is conveyed into the inlet plenum after termination of heating the vessel. The partition member has a distributed plurality of orifices such that the gas is jetted through the orifices to impingement cool the vessel wall. The gas is discharged from the spatial gap through an outlet plenum at an end wall of the vessel. The plurality of orifices are distributed in a pattern of varying density across the partition member such that uniform cooling of the vessel wall by the jetted gas is effected.Type: GrantFiled: December 8, 1995Date of Patent: March 2, 1999Assignee: The Perkin-Elmer CorporationInventor: Herman Vogel
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Patent number: 5806979Abstract: Apparatus for measuring heat capacity of a sample where a series of measurements are taken in succession comprises a sample holder in which a sample to be measured is disposed, a temperature sensor and sample heater for providing a heat pulse thermally connected to the sample, and an adiabatic heat shield in which the sample holder is positioned and including an electrical heater. An electrical power supply device provides an electrical power output to the sample heater to generate a heat pulse. The electrical power from a power source to the heat shield heater is adjusted by a control device, if necessary, from one measurement to the next in response to a sample temperature-versus-time change determined before and after a previous heat pulse to provide a subsequent sample temperature-versus-time change that is substantially linear before and after the subsequent heat pulse.Type: GrantFiled: November 19, 1996Date of Patent: September 15, 1998Assignee: Iowa State University Research Foundation, Inc.Inventors: Karl A. Gschneidner, Jr., Vitalij K. Pecharsky, Jack O. Moorman
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Patent number: 5779363Abstract: A capillary calorimetric cell comprises a solid metallic block having a plurality of channels formed therein. Each channel has first and second ends opening to a first end face and a second end face, respectively, of the block. First and second members are disposed at the first and second end faces of the block, respectively, and cooperate with the block so that adjacent first ends and adjacent second ends of the channels are connected to thus form a single, continuous channel through the block.Type: GrantFiled: September 27, 1995Date of Patent: July 14, 1998Assignee: The Johns Hopkins UniversityInventors: Ernesto Freire, Vincent V. Kavina, George P. Privalov, Peter L. Privalov
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Patent number: 5779362Abstract: A calorimeter is disclosed comprising a sample chamber (12) adapted to enclose a sample, a thermally conductive reference surface (14) surrounding and insulated from the sample chamber (12) and a casing (16) surrounding and insulated from the reference surface. Temperature transducers, in communication with a micro-computer, record the temperatures of the sample chamber (VS) and reference surface (V1) at periodic intervals. The micro-computer is programmed to calculate the theoretical temperature (VT) of the sample chamber from the measured values of the temperature of the reference surface (V1) and estimated values of the thermal power of the sample (I), the thermal resistance from the sample to the sample chamber (RS) and the thermal capacity of the sample (CS), and to optimize the fit between the theoretical calculations (VT) and the corresponding measured values (VS) of the temperature of the sample chamber.Type: GrantFiled: July 13, 1995Date of Patent: July 14, 1998Inventor: John Adrian Lightfoot
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Patent number: 5744696Abstract: Sample analysis in a portable analytical instrument, preferably in the form of a gas chromatograph, benefits from temperature control of one or more thermal zones in the instrument by way of a thermal isolation system that includes a novel pumping assembly to effect a selective amount of thermal isolation of the thermal zone. The pumping assembly includes a pumping element in the form of a tubular or planar palladium structure. The pumping assembly makes use of the unique properties of palladium to allow selective control of a nominal gas pressure within a vacuum cavity. A component system, which may include a separation column and a thermal device for heating and/or cooling the component system, may be provided within the vacuum cavity. The thermal device and the pumping assembly are individually controlled by a control system.Type: GrantFiled: March 10, 1997Date of Patent: April 28, 1998Assignee: Hewlett-Packard CompanyInventors: Tak Kui Wang, James Ward Baker, Terry A. Berger
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Patent number: 5707149Abstract: A method for measuring the heat of reaction resulting from the mixture of a plurality of reagents comprising the steps of providing a first reagent into a compartment; providing a second reagent into the compartment so as to mix the second reagent with the first reagent within the compartment; withdrawing a predetermined amount of the mixed first and second reagents from the compartment; depositing the withdrawn predetermined amount of the mixed first and second reagents back into the compartment; generating electrical signals based on the heat of reaction of the mixed first and second reagents; and deriving data indicative of the heat of reaction based on the electrical signals.Type: GrantFiled: September 27, 1995Date of Patent: January 13, 1998Assignee: Johns Hopkins UniversityInventors: Ernesto Freire, George P. Privalov, Peter L. Privalov, Vincent V. Kavina
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Patent number: 5672289Abstract: A Control circuit for a differential scanning calorimeter which includes a sample heater, a reference heater, a system for generating a sample heater DC voltage and a system for generating a reference heater DC voltage. A balanced operational amplifier arrangement is provided which includes a circuit for controlling the differential heater voltage and a circuit for independently controlling the average heater voltage, so that the average heater power and the differential heater power are independently controlled.Type: GrantFiled: January 11, 1996Date of Patent: September 30, 1997Assignee: The Perkin-Elmer CorporationInventor: Michael J. O'Neill
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Patent number: 5587522Abstract: Vessel, useful in heat transmission regulation, includes a sealable, outer housing and a sample compartment generally enclosed therein such that a hollow portion between at least a part of the housing and compartment is present. The hollow compartment can contain a predetermined quantity of a gas. The sample compartment may be supported, and a multiple-part vessel can be provided. Such a vessel can be made to include standard-manufacture components, being easy to make and use, and/or be especially useful in viscosity testing.Type: GrantFiled: December 26, 1995Date of Patent: December 24, 1996Inventor: Theodore W. Selby
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Patent number: 5547282Abstract: A calorimetric measuring apparatus is provided with a decomposition vessel whose interior is configured as a reaction chamber and which can be tightly sealed, the decomposition vessel being removably arranged inside a jacket, and having at least one temperature sensor for measuring the temperature reached inside the decomposition vessel. Characteristic of the measuring apparatus is that the jacket has a measuring vessel which accommodates the decomposition vessel; at least some areas of the wall zone of this measuring vessel comprise a heat-conductive material; the inner walls of this measuring vessel are spaced from the outer walls of the decomposition vessel, thereby forming an interspace in which a gaseous intermediate medium is provided; and the measuring apparatus has at least a second temperature sensor for measuring the temperature change establishing itself in the heat-conductive wall zone of the measuring vessel.Type: GrantFiled: April 28, 1994Date of Patent: August 20, 1996Assignee: Ika-Analysentechnik GmbHInventors: Hubert Pinhack, Jurgen Fuhrmann, Rolf Gegg
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Patent number: 5474385Abstract: The interpretation of dynamic differential calorimetry ("DDSC") data is enhanced by parsing the data according to whether it is obtained while the sample is being heated, cooled, or re-heated. Each DDSC scan is split up into three separate components, depending upon whether the sample is undergoing heating, cooling or reheating. Each component can then be analyzed separately to investigate the sample response to temperature change as the sample is being heated, cooled, or re-heated. Each file is deconvoluted separately, using a deconvolution routine that first removes the effect of the phase lag due to the instrument's finite response time.Type: GrantFiled: August 24, 1994Date of Patent: December 12, 1995Assignee: TA Instruments, Inc.Inventor: Michael Reading
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Patent number: 5439291Abstract: The present invention is a modulated differential thermal analysis technique for determining the composition, phase, structure, identification, or other properties of a material that undergoes a transition as function of temperature or other driving variable. As applied to differential scanning calorimetric analysis (DSC), the preferred embodiment comprises (1) heating a sample of the material with a linear temperature ramp that is modulated with a sinusoidal heating rate oscillation; (2) simultaneously heating a reference at the same linear temperature ramp; (3) measuring the differential temperature of the sample and reference; and (4) deconvoluting the resultant heat flow signal into rapidly and non-rapidly reversible components.Type: GrantFiled: December 22, 1993Date of Patent: August 8, 1995Assignee: TA Instruments, Inc.Inventor: Michael Reading
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Patent number: 5415024Abstract: A composition analyzer and a method of use for determination of the masses of individual components in a multiphase multicomponent fluid system containing a gas. Data and relationships not measured by the analyzer during operation but required by the method are predetermined or researched and stored, and other required data is instantaneously obtained from the composition analyzer during process operation. All these data are used in an iteration process to accurately determine the mass composition of each fluid component. The preferred means for adding energy to the fluid mixture in the test apparatus is comprised of an electrically conductive conduit through which the fluid mixture flows and which heats the fluid mixture when electrically energized.Type: GrantFiled: December 16, 1992Date of Patent: May 16, 1995Assignee: Marathon Oil CompanyInventors: Arthur C. Proffitt, William C. Barron
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Patent number: 5346306Abstract: The present invention relates to differential analytical techniques for determining the composition, phase, structure, identification or other properties of a material that undergoes a transition as function of a driving variable. As applied to differential scanning calorimetric analysis (DSC), the preferred embodiment comprises: (1) heating a sample of the material with a linear temperature ramp that is modulated with a sinusoidal heating rate oscillation; and (2) deconvoluting the resultant heat flow signal into rapidly reversible and non-rapidly reversible components.Type: GrantFiled: May 7, 1993Date of Patent: September 13, 1994Assignee: TA Instruments, Inc.Inventors: Michael Reading, Brian K. Hahn, Benjamin S. Crowe
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Patent number: 5335993Abstract: A method and apparatus for measuring the thermal conductivity of materials using modulated differential scanning calorimetry (MDSC). Two MDSC heat capacity measurements are made consecutively. One measurement is made under conditions which ensure obtaining a fairly accurate value for the heat capacity of the material ("quasi-ideal conditions"). Another measurement is made under conditions such that the measured effective heat capacity differs from the accurate value of the heat capacity due to thermal conductivity effects. Generally, the non-ideal conditions differ from the ideal conditions by one parameter, such as the size of the sample, the modulation frequency used to measure the heat capacity, or, for thin films, the presence or absence of a specimen on the thin film. The thermal conductivity of the material is then calculated from the difference between the heat capacity measured under quasi-ideal conditions and the effective heat capacity measured under non-ideal conditions.Type: GrantFiled: June 30, 1993Date of Patent: August 9, 1994Assignee: TA Instruments, Inc.Inventors: Sanford M. Marcus, Michael Reading
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Patent number: 5295745Abstract: The calorimeter comprises an external accommodating head (23) with two cavities (26, 27) which are capable of receiving a measurement cell (29), in which the specimen to be examined is inserted, and a reference cell (31); the cells (29, 31) are surrounded by a thermoresistor (229), the variation of the resistance of which is determined by a temperature variation, and a heater (129). The two cavities (26, 27) are closed by covers (35, 37) traversed by tubular stems (47-49) capable of supporting the cells (29, 31) for the insertion, into one of them, of a specimen contained in a tubular container (53), which is immersed in a chamber (29A) in which a fluid having high thermal conductivity is present; said cavities (26, 27) are reached by conduits (41, 43; 45) so as to be subjected to vacuum or to controlled pressure using replaceable gases (air, hydrogen, etc.).Type: GrantFiled: September 9, 1992Date of Patent: March 22, 1994Assignee: Consiglio Nazionale Delle RichercheInventors: Mario Cassettari, Fabio Papucci, Giuseppe Salvetti, Elpidio Tombari, Stefano Veronesi
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Patent number: 5228778Abstract: A heat analyzer equipped to automatically perform operations necessary for protection of measured data and for restart when a problem occurs or a measurement ends and to quickly turn off all power sources by a command input manually by an operator to a system section after daily use. At least one measurement-section power source 6 which can be turned off by an associated measurement controller 5 and a system-section power source 14 which can be turned off by a system controller 11 are included.Type: GrantFiled: July 16, 1992Date of Patent: July 20, 1993Assignee: Seiko Instruments Inc.Inventor: Rintaro Nakatani
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Patent number: 5224775Abstract: The present invention relates to differential analytical techniques for determining the composition, phase, structure, identification or other properties of a material that undergoes a transition as function of a driving variable. As applied to differential scanning calorimetric analysis (DSC), the preferred embodiment comprises: (1) heating a sample of the material with a linear temperature ramp that is modulated with a sinusoidal heating rate oscillation; and (2) deconvoluting the resultant heat flow signal into rapidly reversible and non-rapidly reversible components.Type: GrantFiled: March 2, 1992Date of Patent: July 6, 1993Assignee: TA Instruments, Inc.Inventors: Michael Reading, Brian K. Hahn, Benjamin S. Crowe
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Patent number: 5211477Abstract: A method and apparatus for simultaneous differential scanning calorimetry and microdielectrometry is disclosed. The apparatus includes a sample cell containing a sensor for measuring the dielectric and thermal properties of the sample. The method applies a voltage to a material while heating the material over a temperature range and then simultaneously measuring the current gain of the material, the temperature of the material and the energy input to the material.Type: GrantFiled: May 29, 1999Date of Patent: May 18, 1993Assignee: Ford Motor CompanyInventor: Chi Li
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Patent number: 5163753Abstract: There is provided a differential thermal analysis calorimeter for performing thermal hazard testing procedures which can be utilized as an ancillary plug-in device with commercial thermal analysis data acquisition systems. Simultaneous measurement of heat flow of sample reactants and direct measurement of sample pressure is provided during a reaction within a substantially hollow furnace enclosure defining a heated zone having a heated top plate. A pair of longitudinally elongated heat conductive sample and reference tubes having upper and lower ends are each connected to the top plate adjacent their respective upper ends. The tubes depend downwardly from the top plate within the hollow furnace enclosure, and are heated by the heating means, whereby heat is conducted to the lower end of each tube longitudinally therealong. A pressure transducer is connected adjacent the upper end of the sample tube for directly measuring the pressure in the sample tube within the heated zone of the furnace.Type: GrantFiled: September 20, 1991Date of Patent: November 17, 1992Assignee: The Dow Chemical CompanyInventors: Lawrence F. Whiting, Stephen H. Humphrey
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Patent number: 5158362Abstract: The unknown amount or mass of liquid contained in a storage tank is measured by calibrating the tank in an empty and partially full condition. The calibration includes measuring the mass of the empty tank, and is accomplished by applying a measured amount of heater power or energy to the tank and its contents, and measuring the temperature response to determine the product of total mass multiplied by specific heat. The specific heat depends upon the mass or amount of liquid in the tank, but a linear relationship is established between total mass and the product of total mass times specific heat. The unknown mass of liquid is then determined by applying a known amount of heater power or energy to the tank and its contents, and measuring the temperature rise or rate of rise in response thereto.Type: GrantFiled: February 8, 1991Date of Patent: October 27, 1992Assignee: General Electric CompanyInventors: Laura E. Brauer, Siu H. Chun, Keith Davies, Joseph A. Pulkowski
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Patent number: 5083289Abstract: A temperature reference jacket includes an optical absorber for executing calorimetric measurement of optical power to be measured, a heater, a cooler, and a temperature sensor. The monitor monitors the optical power to be measured. A shutter selectively transmists/shields the optical power to be measured with respect to the optical absorber. A memory stores a first control amount for the cooler corresponding to the optical power to be measured and second and third control amounts for the heater in advance. A controller controls opening/closing of the shutter, reads out the first and second control amounts from the memory in accordance with the monitoring result from the monitor while the shutter is closed, and reading out the first and third control amounts from the memory while the shutter is open. The controller finely adjusts a voltage for the heater so that the temperature reference jacket and the optical absorber are set in an isothermal state while the shutter is closed and open, respectively.Type: GrantFiled: January 29, 1990Date of Patent: January 21, 1992Assignee: Anritsu CorporationInventors: Kenji Kuroda, Koki Sasaki
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Patent number: 4968150Abstract: In an arrangement for measuring the energy of a microwave pulse a container (2) is placed on the end of a waveguide (1). In container (2) there is an absorption liquid (3) with a given heat content, which absorbs the energy of the irradiated microwave pulse. The increase of the heat content thus caused which corresponds to the energy of the microwave pulse is determined by the volume expansion of the absorption liquid (3). For this purpose container (2) is connected to a capillary (4). Preferably container (2) is covered with a reflection layer (12). Further, it is additionally connected to a balancing volume (5) and is cooled with a cooling coil (14).Type: GrantFiled: March 2, 1989Date of Patent: November 6, 1990Assignee: Asea Brown Boveri Ltd.Inventors: Hans-Gunter Mathews, Oskar Schafheitle
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Patent number: 4963499Abstract: A calorimeter for measuring the thermodynamic and kinetic characteristics of chemical reactions, microbial fermentations, and other processes of industrial importance is described. The present invention also relates to a method of operation of this apparatus.Type: GrantFiled: February 24, 1989Date of Patent: October 16, 1990Assignee: American Cyanamid CompanyInventors: Gerald W. Stockton, Dale H. Chidester, Susan J. Ehrlich
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Patent number: 4923306Abstract: A stable isothermal calorimeter wherein the material under study is contained in a thermally conductive reactor vessel which is surrounded by a heat transfer fluid. The material is maintained at the boiling point of the heat transfer fluid which is in turn cntrolled by controlling the pressure of the fluid's vapor space. The heat transfer fluid is vaporized by the heat released by exothermal reaction of the material under study and the vaporized fluid condensed in a condenser. The rate of liquid accumulation in the condenser is proportional to the energy release rate of the material.Type: GrantFiled: August 3, 1989Date of Patent: May 8, 1990Assignee: Westinghouse Electric Corp.Inventor: Hans K. Fauske
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Patent number: 4892707Abstract: A calorimeter for measuring the thermodynamic and kinetic characteristics of chemical reactions, microbial fermentations, and other processes of industrial importance is described. The present invention also relates to a method of operation of this apparatus.Type: GrantFiled: July 25, 1983Date of Patent: January 9, 1990Assignee: American Cyanamid CompanyInventors: Gerald W. Stockton, Dale H. Chidester, Susan J. Ehrlich
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Patent number: 4861167Abstract: An apparatus and method for measurement of the thermal conductivity of polymer melts is disclosed. A sample of material to be measured is placed in an elongated cylindrical container and is heated to a preselected base temperature. A probe placed in the container in contact with the sample contains a transient heating element and a temperature sensor. To determine the thermal conductivity of the sample material, the transient heating element is energized and the resulting changing temperature of the sample material is measured for a short period of time. The rate of temperature change is a measure of the thermal conductivity of the sample material at the base temperature.Type: GrantFiled: September 28, 1988Date of Patent: August 29, 1989Assignee: Cornell Research Foundation, Inc.Inventors: Hubert Lobo, Kuo K. Wang
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Patent number: 4859077Abstract: A precision calorimeter which comprises a heater, an agitator and a detection bath which are disposed in a temperature controlled bath and in which gaps formed between them are filled with a liquid; and a detection unit placed in the detection bath, a gap formed therebetween being filled with a liquid; the detection unit being comprised of a detection element, a pipe for passing a sample therethrough provided with a mixer and a reference heater which are arranged between metallic pieces.Type: GrantFiled: July 2, 1987Date of Patent: August 22, 1989Assignee: Shoziro ItoInventors: Shoziro Ito, Akihiro Ito, Hiroyasu Ito
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Patent number: 4838706Abstract: A method and apparatus for thermal analysis of a solid or liquid sample which evolves or absorbs gas on heating or cooling, wherein the sample is heated or cooled in an enclosed space, the temperature of the sample and the pressure of the gas are continuously monitored by temperature and pressure sensors respectively, and measurements of sample temperature and gas pressure are input to a data processor which also controls the temperature change of the sample. The value of gas pressure as a function of sample temperature and the rate of change of this value with respect to sample temperature are calculated; these functions are characteristic of the sample or of a component of the sample under analysis.Type: GrantFiled: March 19, 1987Date of Patent: June 13, 1989Assignee: The Provost, Fellows and Scholars of the College of the Holy and Undivided Trinity of Queen Elizabeth Near DublinInventors: John M. D. Coey, Dominic H. Ryan
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Patent number: 4833688Abstract: A device and associated method comprising a probe (18) for drawing throttled two-phase steam into a tank (26) which has been evacuated and which can be closed when the pressure of the sample steam in the tank equals the pressure of the source steam mixture (14). The throttling tank operates on the basic thermodynamic principle that a two-phase mixture when throttled into a closed tank becomes superheated. The state of the superheated mixture is determined by temperature and pressure measurements (42, 36). The initial state of the source mixture can then be determined by application of the First Law of Thermodynamics, which is considerably simplified as a result of the way in which the sample is drawn.Type: GrantFiled: January 7, 1988Date of Patent: May 23, 1989Assignee: Combustion Engineering, Inc.Inventor: William R. Smith
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Patent number: 4813270Abstract: Water, oil and gas mixtures such as produced from oil and gas wells are analyzed as to the proportionate content of each component in the total mixture by calorimetric processes in systems which separate the gas from the fluid mixture, withdraw a sample of the liquid mixture and subject the sample at a given or determined flow rate to a heat exchange process. The remaining main flow of the liquid mixture is also subjected to a heat exchange process and a heat balance is calculated for the flowstream based on the change in temperature of main liquid flowstream and the change in temperature of the heat exchange medium. The processes are carried out on the main flowstream by interposing a heat exchanger in the flowstream or by reinjecting into the flowstream a measured amount of heat exchange fluid such as separated water or crude oil.Type: GrantFiled: March 4, 1988Date of Patent: March 21, 1989Assignee: Atlantic Richfield CompanyInventor: Lloyd A. Baillie