WO1999060356A1 - Procede et dispositif permettant de reguler un flux thermique a des fins de calorimetrie, de protection adiabatique, de reglage fin de la temperature, etc. - Google Patents

Procede et dispositif permettant de reguler un flux thermique a des fins de calorimetrie, de protection adiabatique, de reglage fin de la temperature, etc. Download PDF

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Publication number
WO1999060356A1
WO1999060356A1 PCT/EP1999/003485 EP9903485W WO9960356A1 WO 1999060356 A1 WO1999060356 A1 WO 1999060356A1 EP 9903485 W EP9903485 W EP 9903485W WO 9960356 A1 WO9960356 A1 WO 9960356A1
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WO
WIPO (PCT)
Prior art keywords
temperature
shield
heat flux
sample
flux control
Prior art date
Application number
PCT/EP1999/003485
Other languages
English (en)
Inventor
Giuseppe Salvetti
Carlo Ferrari
Fabio Papucci
Elpidio Tombari
Original Assignee
Consiglio Nazionale Delle Ricerche
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from IT98PI000044 external-priority patent/IT1306122B1/it
Priority claimed from IT98PI000073 external-priority patent/IT1306610B1/it
Application filed by Consiglio Nazionale Delle Ricerche filed Critical Consiglio Nazionale Delle Ricerche
Priority to AU48991/99A priority Critical patent/AU4899199A/en
Priority to EP99932695A priority patent/EP1080350A1/fr
Publication of WO1999060356A1 publication Critical patent/WO1999060356A1/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00—Investigating or analyzing materials by the use of thermal means
    • G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
    • G01N25/48—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation
    • G01N25/4846—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation for a motionless, e.g. solid sample
    • G01N25/4866—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation for a motionless, e.g. solid sample by using a differential method
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
    • G01K17/00—Measuring quantity of heat
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
    • G01K17/00—Measuring quantity of heat
    • G01K17/04—Calorimeters using compensation methods, i.e. where the absorbed or released quantity of heat to be measured is compensated by a measured quantity of heating or cooling

Definitions

  • the present invention relates to a heat flux control method for calorimetry, adiabatic shielding, precise temperature setting and the like.
  • the invention relates to a method for analysing the thermodynamic characteristics on samples and the kinetics of the active processes in said samples.
  • the present invention relates also to an active shield for controlling the heat flux for calorimetry, adiabatic shielding, and the like.
  • the invention relates to a calorimeter that uses this shield, operating both in adiabatic and in modulated way as well as in temperature scanning way.
  • calorimeters For carrying out precise heat measures of quantities such as for example heat capacity of bodies or substances, or the heat delivered by chemical reactions, it is necessary to provide calorimeters having good sensitivity, precision, adaptability, to the characteristics of the sample, as well as the possibility of inspecting wide temperature ranges.
  • calorimeters of this kind can be used for controlling industrial processes and for product testing, provided they are not too complicated and they can be put in automatic measuring procedures.
  • the shield In an adiabatic functioning, the shield is kept at a temperature equal to the object, whereby said heat flux between the object and the shield is substantially zeroed.
  • a temperature scanning functioning successive steps are provided of heating the object for transmitting to the object a predetermined heat flux and/or for bringing in turn the object to different chosen temperatures, the heating step of the shield keeping the temperature of the shield at predetermined distance from the temperature of the object.
  • an apparatus for controlling the heat flux for calorimetry, adiabatic shielding, precise temperature setting and the like, on an object comprises
  • thermal bath arranged about the shield kept at a known temperature in any case lower than the temperature of the shield;
  • a embodiment of the apparatus for carrying out also temperature scanning calorimetry comprises heating means distributed uniformly on at least a portion of the object, suitable for transmitting to the object a predetermined heat flux, the means for controlling the heat flux operating the heating means of the shield setting in turn a fixed difference between the signals of the means for measuring the temperature of the shield and the signals of the means for measuring the temperature of the object.
  • FIG. 1 shows a sectional view according to a vertical plane of a calorimeter associated to an active heat shield that carries out the method according to the invention
  • FIG. 2 shows a sectional view according to a vertical plane of the assembly of a calorimetric head and of a cell of a calorimeter according to the invention
  • figure 2A shows the calorimetric head of the calorimeter of figure 1;
  • figure 2B shows the calorimetric cell associated to the head of the calorimeter of figure 1;
  • FIG. 3 shows a sectional view according to a vertical plane of a calorimeter according to the invention having a double cell
  • FIG. 4A and 4B show two different embodiments of the cell of figure 2, 2B or 3 ;
  • FIG. 4C shows a cross sectional view of a shield according to the invention capable of housing four cells like those shown in figures 2, 2B, 3, 4A, 4B .
  • FIG. 5 shows a block diagram of the calorimeter that carries out the method according to the invention
  • FIGS. 6A-6D show flow-sheets of the operations controlled by the software of the calorimeter of figure 5 in the adiabatic way;
  • FIG. 7A-7D show flow-sheets of the operations controlled by the software of the calorimeter of figure 5 in a modulated way and in a temperature scanning way. Description of the preferred embodiments
  • a calorimeter having a shielding side surface or shield 1 having cylindrical symmetry closed by plugs of insulating material 6.
  • Shield 1 of the calorimeter is associated to a first uniformly distributed winding thermoresistor 5, for heating shield 1, and to a second thermoresistor 3 for measuring the average temperature of shield 1 and for the calculus the radial heat flux.
  • a thermal bath 7 is provided having a predetermined reference temperature, in any case lower than the temperature of shield 1.
  • the control of shield 1 is carried out by adjusting the power fed by a programmable supplier 8 (PPS) to heater 5, for keeping it at the working temperature that must, as above said, be higher than the temperature of the thermal bath 7 in which it is located.
  • PPS programmable supplier 8
  • PPS Proportional-Integrative-Derivative procedure
  • - object 2 houses energy production processes that cause a variation of enthalpy ⁇ H;
  • a good shield 1 according to the invention can, with the interventi of control to the range about of the second, keep the temperature fixed to less of 0.001°C, also for time very long.
  • the equation (2') contains all the information necessary for investigating calorimetric of the sample. for ricavarla with the maximum of sensitivity and precision is necessary ricorrere to modi calorimetric different which, in type, require also the use instruments different . According to the invention, instead, a same calorimeter hereinafter described with reference to figures 2, 2A, 2B, can be used for working both in way adiabatic that in way to modulation of temperature.
  • the calorimeter 20 comprises a head 30 and a cell 40, in which is inserted a sample 25, suspended to a wire 21.
  • the head 30 (figure 2A) of the calorimeter comprises a block 7 cylindrical of aluminium or other material metal to high heat conductivity, with a hole central 32 of diameter sufficient to containing the calorimetric cell 40.
  • the block 7 houses a 0-ring of kept 33, for support of a plug cylindrical 34, connected to the block 7 and fact of equal material, suitable for supporting the calorimetric cell 40 and provided of passing electrical 34a.
  • on the plug 34 is fixed coaxially a tube 35 to thin walled, for example of steel stainless of length and diameter such by to allow the introduction of the sample 25 from the outer.
  • the calorimetric head 30 is sized in order to work from thermal bath 7 of figure 1, designed in order to assuring the necessary steadiness heat ( ⁇ 0.002°C) and the temperature working minimum demand, the function unwound from the calorimetric head 30 it is therefore that of creating an environment at a temperature uniform and exchanges heat radial about the calorimetric cell 40.
  • the gap 41 between the head 30 and the calorimetric cell 40 are minimum in order to prevent from the convection and reducing to the maximum the exchanges along the axis of the cell 40.
  • Nel block 7 of the head 30 is made a hole 36 for housing the probe of a thermometer of reference, for example a thermometer to the platinum, necessary for adjustment absolute of the calorimeter both in direct phase of testing that for possible check following.
  • the cross section vertical of the calorimetric cell shown in Figure 2B comprises
  • a cylinder of metal 49 with a recess inner 48 suitable to receive the sample 25, for example a test tube containing a substance from analyse .
  • Shield 1 is closed in low with a plug hollow metal 6 that houses in a cylinder of material insulating 50 and is shaped with a flange 16 to the precise of reducing the exchanges heat towards the low and assuring the centering of cell 40 inside of the recess 32 of the calorimetric head 30.
  • a plug metal upper 51 is screwed to stop shield 1. It supporta both of the support insulating 43, in tube capillare of steel stainless to which is fixed the cylinder metal 49, which passing for conducting electrical (not shown) .
  • Sul cylinder 49 are arranged, in way uniform and uninductive, two windings: a first winding inner 46 formed by a resistor of manganine, longer and a second winding inner 4, shorter, formed by two thermoresistors in material thermoresistive, for example platinum or alloy 99 delivered by Driver-Harris.
  • the three resistors are suitably insulated between of thereof with the material insulating to the web of Teflon, varnish polymeric, material ceramic etc. the characteristics fisico-chemical of the material used to the insulating electrical cause the temperature range wherein the calorimeter can be used.
  • Sullo shield 1 are made, in way similar to figure 1, a first winding outer 5 (i.e.
  • the first windings longer, -5 and 46, are, respectively, the heaters of shield 1 and of the sample cell 40, whereas the seconds windings shorter 3 and 4 are the thermoresistors for measuring the temperature average and for definition the heat flux radial used hereinafter, the windings 5 and 3 extends for height equal, respectively to windings 46 and 4.
  • Cell 40 (figure 2) is fixed to the plug 34 of the head 30 from the support 43.
  • the gap circular 41 that separates cell 40 from the block 7 of the head 30 is for example of 1-2 mm, to the precise of substantially prevent from exchanges for convection.
  • a characteristic relevant of the head 30 and of the calorimetric cell 40, according to the invention, is the cylindrical symmetry of the whole structure, which achieves the maximum reduction of the exchanges heat along the axis vertical.
  • the head 30 has a single block cylindrical 7, of aluminium or other material metal to high heat conductivity with a hole central 32 of diameter sufficient to containing the cells 40a and 40b, formed by the single shield 1 on which are provided the windings 5 and 3.
  • the head 30 has a structure that avoids the continuity heat between the cells and the outer. More precisely, a plug cylindrical 62 upper, which comprises the insulating axial 66, is connected to the block 7 to keep hanging the cells 40a and 40b and the passing electrical (not shown) , by means of a thin walled stainless tube 65.
  • a lower plug 64 contains another axial insulation 66.
  • two tubes 35a and 35b, to thin walled of steel stainless, are connected protruding from the plug upper 62, of length and diameter such by to allow the introduction from the outer of the sample 25a from analyse and of the sample 25b of reference.
  • the cell of reference is virtual and is simulated through a thermogram obtained, once for tutte, in a measure preliminary fatta on cell 40 without sample 25. During the measure preliminary the data are recorded in order to being utilizzabili in all the measuring following, made in equal conditions.
  • the use of the reference virtual it is possible since the temperature of the sample cell 40, of shield 1 and of the thermal bath 7 follow equal time ranges, connected by the program, and are fixedmente under control in every measure. Eventi improvided that dovessero invalidare the assunzioni on which is basa the use of the reference virtual not can then sfuggire to the operator, which can tenerne conto or repeat the measure .
  • the cell of reference 40b is actualmente present and the presence of the two cells twin 40a and 40b allows a calorimetry differential of high sensitivity, for example particularly suitable to the studio of samples biologici .
  • the gain in sensitivity is due to the possibility measuring with the techniques lock-in the difference of temperature between the two cells 40a and 40b, by subtracting thus also the contributo of the cell of reference 40b, enpty or containing quanto of inpredetermined is sommi to the exco and/or to the substance present in 25a that is to be quietare.
  • the calorimeters of figures 2 and 3 can adapt to different dimensions of sample, as shown in figure 4A, with the cell for volumi smaller (i.e. from 0.1 to 0.2 cc) , and in figure 4B, with the cell for volumi any more grandi (i.e. from 10 to 15 cc) .
  • shield 1 has four recess 32 for corresponding cells, not shown, and has five holes 69 with the function of reducing the heat capacity of the shield same.
  • figure 5 is shown the block diagram of the calorimeter of figure 2, with the indicacade also of the control electronic unit.
  • a PC 70 wherein resides a software hereinafter described, is connected con: - suppliers 71 and 72, of the first winding inner 46 and of the first winding outer 5 of shield 1;
  • a amplifier lock-in, 73 which measure with thetician big sensitivity the resistance of the sensor of temperature 3 located on the cell sample;
  • a multimeter scanner 74 which measure the resistance of the other two sensors of temperature coupled ;
  • the particular configuration of the calorimeter of figure 2 (o of figure 3) according to the invention allows to obtain, cambiando single the software, different functionings, from choose according to the characteristics of the sample and the object of the measure, is thus possible working.
  • shield 1 is essential since beyond to the task of thermal bath, has the task additional of follow the evolution heat of the cell sample, keeping to a distances fixed ⁇ T with the operation to heat flux fixed.
  • the way of operation adiabatic to scanning b) is obtained setting the flow total to a value negative suitable, setting i.e. the temperature of shield 1 some degrees any more in low of that of the sample cell 40.
  • adiabatic to scanning it is possible to make measuring very accurate of heat capacity in heating, supplying a succession of pulses of energy equal, ⁇ Q, to the sample cell 40, to the range of time predetermined.
  • the chosen temperature range is swept following ⁇ T xi steps.
  • the heat capacity C p of the sample at temperature T + T xi /2 is calculated by the equation:
  • C P (T+ ⁇ T xi /2) ⁇ Q(l/ ⁇ T xi - 1/ ⁇ Toi) (3) wherein ⁇ Toi is the correspondingly measured temperature step, in equal conditions, with the container 25 of the empty sample holder.
  • Ts(t) Ti + ⁇ t + Tmcos ⁇ t (5)
  • Ti is the starting temperature
  • ⁇ is the sweeping difference
  • Tm is the amplitude of modulation at the frequency ⁇ /2 ⁇ .
  • the term ⁇ H/dt contains the difference of variation of the enthalpy given to the occurring of processeszaro-fisici in the sample and the response of the internal energy of the sample to the modulation
  • the software provides the analysis of the signal of power acquisito in the ⁇ range time n ⁇ ⁇ ⁇ ⁇ (n+l) ⁇ versus trasformata discreta of Fourier to the frequency ⁇ , assumendo that the enthalpy deliver ⁇ H/ ⁇ T both approssimabile with a production in multitude of Taylor limitato at the end of first ordine, and that the components of the heat capacity possano considerarsi constants during the range of time ⁇ .
  • thermometer digital with the probe PtlOO, adjusted to the standard secondary of temperature, located hole 36 of the head 30 (figure 2A) .
  • the temperature of the bath has been swept to steps of 1-5°C with delays of 15000s.
  • the value absolute of the temperature of the sample can be chosen at the temperature average of the surface external of the cell, since is located in conditions steady and without temperature gradient, the steadiness of the thermal bath allows to obtain the calibrations of the three sensors with a big precision (better of ⁇ 0.001°C) .
  • the calibration absolute of the scale of temperature needs of a reference inner, which can be formed by a sample of water, which can be easily product from the operator or provided to the kit of the instrument from the manufacturer, the sample of water is preferably water ultrapure put into sample holder, partially filled and sealed forn being subcooled of many degrees, when the water freezes the heat latent of transition is thus big that not allows to all the mass of the liquid of solidficare: to the beginning is obtained a mixture water, ice and vapour at the ternperature of the triple point of the water (+0.01°C) .
  • This condition can be kept time if the heat capacity of the cell empty is not too big with respect to that of the sample water and if is active automatically the way of step adiabatic, i.e. the shield salt quickly at the temperature of the cell sample, the thermometrical scale of the instrument, this way, has a precision better of 0.01°C
  • the other calibration necessary is power P, delivered by heater 5 of the cell. This depends from the measuring precision of the voltage applied to the ends of the heater, a given this of kit of the multimeter used, considering of the even little according at the temperature of the electrical resistance of the manganine, of which is preferably made the heater, to obtain the calibration of the amount of heat, Q, is suitable also a calibration of the time scale.
  • the precision obtainable is, using a multimeter with six digits: absolute temperature ⁇ 0.01°C; power ⁇ 0.001 mW; amount of heat ⁇ O.OOlmJ.
  • a program which can be used is LabVIEW 3.0 of National Instruments, Austin, Texas, U.S.A.
  • the flow diagrams of the software can drive the calorimeter in two main functioning: the adiabatic way (Figure 6A-6D) and the temperature scanning modulated way (Figure 7A-7D) .
  • the Adiabatic way program starts with a step of thermalisation at the lowest temperature of the experiment (T threshold ) ; then it continues with a while-loop, which continuoes up to when temperature T c of the sample achieves predetermined value Tax,- every iteration of the loop is a temperature step during which is measures the step of temperature of the sample caused by the deliver of a known heat amount. At the end of every iteration there is a variable delay so that the duration of the iteration is exactly 3000 milliseconds .
  • Figure 6B is shown the routine of the ther alisation program of the sample at T threshold of figure 6A.
  • a first while-loop is active so that the temperature T c of the sample reaches a value T threshold .
  • a second loop of 300 iterations brings the temperature of the shield T s to that of the sample T c by means of a procedure PID (proportional-integrative-derivative) that calculates the power P s to deliver to the heater of the shield.
  • PID proportional-integrative-derivative
  • the program carries out the linear interpolation of the last 100 data recorded (see Figure 6D) .
  • Figure 6C are given in detail the operations carried out during the measure.
  • a single loop of 300 iterations has two different steps: in the first 30 iterations a predetermined power P c is delivered to the sample; in the following iterations the power P c is set equal to zero.
  • T s is linked to T c by means of the PID procedure.
  • FIG. 6D is given the diagrammatical operative view of the linear interpolation.
  • the program graphs and stores on Hard Disk in real time the values of T c and T s every three seconds and the values C p and m every 300 iterations of three seconds.
  • the duration of a step is measured by the value of the characteristic heat relaxation time of the cell sample, determined through the exponential start of the step, when the temperature of the cell relaxates towards the value of equilibrium.
  • the described program contains the most favourable parameters for a cell of the type of Figure 4B, containing a sample of water of lOcc.
  • FIG 7B the step is shown of thermalisation of the sample at temperature T threshold .
  • T threshold There is a single for- loop of 500 iterations of 3000ms each, during which two different procedure PID bring temperatures Tc and T s of the sample cell and of the shield, respectively to the values T threshdroiti d and T tnreshold - ⁇ T s by means of the control of the power P c and P s supplied to the heaters.
  • Temperature T c is in this case linked, by means of the PID, according to a temperature Tro e chosen previously (i.e. a slope) and modulated with a sinusoidal function of amplitude dT and frequency ⁇ .
  • Temperature T s is linked at temperature T C - ⁇ T S .

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Abstract

Procédé et dispositif permettant, pour un objet (2), de réguler un flux thermique à des fins de calorimétrie, de protection adiabatique, de réglage fin de la température, etc. Selon le procédé, on dispose un écran (1) autour d'un objet (2); on chauffe uniformément (5) l'écran et on contrôle (3) l'étape de chauffage de façon à maintenir l'écran (1) à la température choisie; on dispose autour de l'écran un bain thermique (7) à une température connue, inférieure à celle de l'écran (1); on mesure la température de l'objet (2); et on régule (8) le flux thermique (5) entre l'objet (2) et l'écran (1) en surveillant la température (4) de l'objet (2) et la température de l'écran (1). L'application de l'invention dans le domaine de la calorimétrie permet d'utiliser avantageusement le même calorimètre avec la technique classique aussi bien qu'avec la technique du balayage thermique et la technique modulée.
PCT/EP1999/003485 1998-05-20 1999-05-20 Procede et dispositif permettant de reguler un flux thermique a des fins de calorimetrie, de protection adiabatique, de reglage fin de la temperature, etc. WO1999060356A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AU48991/99A AU4899199A (en) 1998-05-20 1999-05-20 Heat flux control method and apparatus for calorimetry, adiabatic shielding, precise temperature setting and the like
EP99932695A EP1080350A1 (fr) 1998-05-20 1999-05-20 Procede et dispositif permettant de reguler un flux thermique a des fins de calorimetrie, de protection adiabatique, de reglage fin de la temperature, etc.

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
IT98PI000044 IT1306122B1 (it) 1998-05-20 1998-05-20 Calorimetro a scansione di temperatura operante in modo adiabatico omodulato
ITPI98A000044 1998-05-20
IT98PI000073 IT1306610B1 (it) 1998-10-19 1998-10-19 Dispositivo con schermo termico attivo per la calorimetria e ilcontrollo della temperatura di oggetti non passivi
ITPI98A000073 1998-10-19

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WO1999060356A1 true WO1999060356A1 (fr) 1999-11-25

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WO (1) WO1999060356A1 (fr)

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WO2006086708A1 (fr) 2005-02-10 2006-08-17 Perkinelmer Las, Inc. Calorimetre a compensation de puissance (dsc) comprenant un fourneau a temperature regulee
WO2006090247A1 (fr) * 2005-02-22 2006-08-31 Cnr Consiglio Nazionale Delle Ricerche Calorimetre multimode economique
ITPI20080066A1 (it) * 2008-07-18 2008-10-17 Consiglio Naz Delle Ricerche Dipartimento Calorimetro multimodo differenziale
WO2009080861A1 (fr) * 2007-12-24 2009-07-02 Consejo Superior De Investigaciones Científicas Dispositif et procédé adiabatique pour mesurer le coefficient d'absorption spécifique d'un matériau soumis à un champ magnétique alternatif
JP2010527451A (ja) * 2007-05-16 2010-08-12 エナジエテイツク・ジエノミクス・コーポレイシヨン 大型アレイ式示差走査熱量計のｄｓｃ測定装置
US8292495B2 (en) 2010-04-07 2012-10-23 Arizant Healthcare Inc. Zero-heat-flux, deep tissue temperature measurement devices with thermal sensor calibration
US8292502B2 (en) 2010-04-07 2012-10-23 Arizant Healthcare Inc. Constructions for zero-heat-flux, deep tissue temperature measurement devices
US9068895B2 (en) 2009-04-15 2015-06-30 3M Innovative Properties Company Deep tissue temperature probe constructions
US9310257B2 (en) 2009-04-15 2016-04-12 3M Innovative Properties Company Deep tissue temperature probe constructions
US9354122B2 (en) 2011-05-10 2016-05-31 3M Innovative Properties Company Zero-heat-flux, deep tissue temperature measurement system
CN111830080A (zh) * 2020-06-22 2020-10-27 航天材料及工艺研究所 一种精密绝热量热计及其量热方法

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US7448796B2 (en) 2004-02-10 2008-11-11 Perkinelmer Las, Inc. Differential scanning calorimeter (DSC) with temperature controlled furnace
EP2290356A3 (fr) * 2005-02-10 2012-03-14 PerkinElmer Health Sciences, Inc. Calorimètre à balayage différentiel doté d'un four à température contrôlée
JP2008530560A (ja) * 2005-02-10 2008-08-07 パーキンエルマー・エルエーエス・インコーポレーテッド 温度制御炉を備えた示差走査熱量計（ｄｓｃ）
WO2006086708A1 (fr) 2005-02-10 2006-08-17 Perkinelmer Las, Inc. Calorimetre a compensation de puissance (dsc) comprenant un fourneau a temperature regulee
US7914201B2 (en) * 2005-02-22 2011-03-29 Cnr Consiglio Nazionale Delle Richerche Low cost multimode calorimeter
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US8746967B2 (en) 2007-05-16 2014-06-10 Waters Technologies Corporation Large array differential scanning calorimeter, DSC measuring unit
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JP2010527451A (ja) * 2007-05-16 2010-08-12 エナジエテイツク・ジエノミクス・コーポレイシヨン 大型アレイ式示差走査熱量計のｄｓｃ測定装置
WO2009080861A1 (fr) * 2007-12-24 2009-07-02 Consejo Superior De Investigaciones Científicas Dispositif et procédé adiabatique pour mesurer le coefficient d'absorption spécifique d'un matériau soumis à un champ magnétique alternatif
ES2333762A1 (es) * 2007-12-24 2010-02-26 Consejo Superior De Investigaciones Cientificas Equipo adiabatico para medida del coeficiente de absorcion especifico de un material sometido a un campo magnetico alterno.
ITPI20080066A1 (it) * 2008-07-18 2008-10-17 Consiglio Naz Delle Ricerche Dipartimento Calorimetro multimodo differenziale
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US8292495B2 (en) 2010-04-07 2012-10-23 Arizant Healthcare Inc. Zero-heat-flux, deep tissue temperature measurement devices with thermal sensor calibration
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US8801282B2 (en) 2010-04-07 2014-08-12 3M Innovative Properties Company Constructions for zero-heat-flux, deep tissue temperature measurement devices
US8292502B2 (en) 2010-04-07 2012-10-23 Arizant Healthcare Inc. Constructions for zero-heat-flux, deep tissue temperature measurement devices
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US10274383B2 (en) 2011-05-10 2019-04-30 3M Innovative Properties Company Zero-heat-flux, deep tissue temperature measurement system
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