Calisto – Calibration Procedure

CONTENTS
Introduction – Calibration Temperature Correction – Method Temperature Correction – Processing Sensitivity Coefficient – Enthalpy Calibration Sensitivity Coefficient – Joule Effect Calibration 1 2 3 5 7

Introduction – Calibration To calibrate using heat of fusion standards, it is necessary to know; (1) the melting temperature, (2) the Enthalpy. The Calisto software allows the user to generate a temperature correction coefficient based on known melts of certain standards and a sensitivity coefficient to convert the heat flow in terms of energy. Heat of Fusion Standard Naphthalene Indium Tin Lead Zinc Aluminum Silver Gold Melt (°C) 80.23 156.59 231.94 327.47 419.56 660.33 961.78 1064.18 Enthalpy (J/g) 147.6 28.5 60.2 23.0 107.4 401.3 104.8 64.5

Above is a list of just some popular standards used in calibrating your apparatus. For “Calvet” designed sensors; such as the SenSys or C80 (3 dimensional sensor), the sensitivity coefficient is generated by performing a Joule Effect calibration. Any new or repaired sensor will be accompanied by a sensitivity coefficient data-sheet, performed at our factory before delivery.

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then cool and use the second heating to analyze the value of Tonset. make sure that no previously stored temperature correction is being used. it is recommended to perform a pre-melting first. Also in your method.Calisto – Calibration Procedure Temperature Correction – Method When writing your experimental method to perform a melting of a standard. otherwise you will be performing a correction of a correction. Page 2 of 8 .

For temperature calibration. which will obtain the onset point for the melting. the onset point is where the tangent of the initial slopes’ maxima is projected back to the baseline.Calisto – Calibration Procedure Temperature Correction – Processing Use the data-file to integrate the results. this intersect is taken as Tonset and is regarded as the melting point of the standard. Page 3 of 8 .

select the item “Temperature correction” to obtain the table below. under the menu-bar heading “Maths”. Note: Each standard can be run twice.Calisto – Calibration Procedure In the “Processing” application. once at a low heating and repeated at a faster heating. Page 4 of 8 . thus producing two data sets per sample. It is recommended to produce at least five data-sets to obtain a relatively accurate polynomial. This can be populated with the results from the onset point of each heat-of-fusion experiment.

µV. If the intension is to recalibrate the sensitivity coefficient. the Joule can be expressed as the Watt-Second. Typically. Again. it is considered that the peak Area of the endothermic effect will be equal to the Enthalpy. which has the following relationship: Sensitivity = Area = [µV.s/mg] = mV. J/g. the Enthalpy calibration is performed by generating a sensitivity coefficient.s Enthalpy [J/g] J Also.Calisto – Calibration Procedure Sensitivity Coefficient – Enthalpy Calibration For non-Calvet type sensors. measured here in. then any existing coefficient must be set to zero. SETARAM allows the user to generate a ‘Sensitivity’ coefficient.s Page 5 of 8 . Enthalpy is expressed in. When viewing the heat flow data. so in order to calibrate each heat-flow sensor. Sensitivity = mV = W µV mW = W.s/mg. J Thus. use a standard to perform a heat-of-fusion experiment.

select the item “Regression” to obtain the table below. this would be wrong. (mW). in the “Processing” application.Calisto – Calibration Procedure Therefore. As a general rule the sensitivity coefficient is parabolic in shape: Avoid choosing too high an order of polynomial that may attempt to do a “best-fit” sinusoid. the value of Heat Flow is expressed in units of Power. Page 6 of 8 . once the sensitivity coefficients are determined. under the menu-bar heading “Maths”. For the temperature column.A preview of the regression is available for viewing. enter the Tonset value for each melting. It is recommend to do as many different standards as possible to ensure the whole temperature range is calibrated in terms of Enthalpy. Again. The sensitivity coefficient is generated by populating a Regression table. TIP:.

during a time.Calisto – Calibration Procedure Sensitivity Coefficient – Joule Effect Calibration The Joule Effect principle is where the transformation of electrical energy is made into heat. an electrical current. I. R. In this case the EJ3 and software has to be started manually. Heat Capacity is defined by the ratio of heat quantity exchanged by the system with the surrounds during a temperature change. generates a heat quantity. flowing through a conductor of resistance. To be more precise. When using Calisto the EJ3 can also be started manually. The principle of the EJ3 is to produce an exact measure of power (mW) into the senor. Note: The Joule Effect Zone will automatically set the sensitivity coefficients to zero. With older versions of software. Q=RI2 t. but it is designed to be connected to an additional serial port (or USB) for automated software control. t. the joule effect calibration was activated by a dongle and gave an extra zone in the acquisition software. The Calvet principle uses this heat quantity in the apparatus to generate a proportional difference when a change in heat-flow occurs between a sample and reference chamber within the same furnace. With SetSoft (16bit) the EJ calibration option has to be added via a floppy disk and is a separate application module. Page 7 of 8 .

m. over time. Page 8 of 8 . Generally. Heat Flow [mW]. for a change in temperature. has to be established from a known mass of sample with a known specific heat capacity in order to calibrate the Heat Flow measurement. t.T + A2. Hence. Cp. expressed by: Cp = J. will also be proportional to the mass. Q. dQ = m.K In the case of the Calvet principle. Specific Heat Capacity is the energy that raises the temperature of one kilogram by one kelvin. (W) = J.Calisto – Calibration Procedure The Calvet configuration of the thermopile element is to detect heat flow between a reference and sample by electrically balancing two thermopiles that will produce a voltage difference if any heat flow is detected. Power is already given by the Joule Effect calibration.T3 + A4. This equation converts the raw heat-flow signal (µV) to power (mW) at that given temperature. This is a direct measure of heat quantity (Q).Cp For a single thermocouple type DSC.K-1] The Heat Quantity.K-1 The Energy is thus calculated from: J = Cp.Kg.T2 + A3. Q is equivalent to [J.T4 with units of µV/mW. So. Q = m. of the sample and its specific heat capacity. T.Kg-1.Cp dT dt dt Or.s-1 (Heat Flow measured in milliWatts) After using the Joule Effect calibration a set of sensitivity coefficients are generated that follow the form: S(T)= A0 + A1.

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