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Abstract  

The preparation of a set of standards for the calibration of the analysis of deuterium using the2H/3He, p/4He reaction is described. Important considerations in the selection of a suitable standard are that it should be stable under irradiation and be simple to prepare with ready control of the amount of analyte. These requirements were met by Ca/OH/2 which was prepared by the replacement of hydrogen with its isotope in known proportions in the reaction of CaO with water.

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Abstract  

DSC analysis of wax/polymer blends is carried out between 270 and 420 K. Calibration for melting point and enthalpy is normally carried out using indium (melting point 430 K), which is unsatisfactory for these materials. IUPAC organic standards covering this range tend to sublime and their onset temperatures are variable. Pure alkanes have similar thermal characteristics to wax/polymer blends and some have been well characterised by adiabatic calorimetry. They are being investigated as alternative secondary calibration standards to give more accurate thermal characterisation of wax/polymer blends. Also,n-triacontane can be used to check DSC resolution.

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Abstract

The identification of the calorimetric curves corresponding to liquid mixtures for different injection flows, given by a flow microcalorimeter, permits to classify in a kinetic way the studied mixtures. For this purpose, it is determined the establishment time constant of the mixture (τmix) that allows us to estimate the length occupied by the dissipation (through the parameter λmix) and thus to justify the sensitivity variation obtained in different chemical calibrations.

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Abstract  

A simple experimental method for the efficiency calibration of germanium detectors especially for environmental samples is presented, using only the natural radionuclides in the sample. The method is based on the fact that for the energy range above 300 keV the full-energy-peak efficiency of a Ge detector can be described in a first order approximation by a linear interpolation curve in the log-log display with errors lying normally under 5%. Photons with different energies which are emitted from one radionuclide yield count rates which are correlated to the corresponding efficiencies. From this correlation one coefficient of the interpolation curve — a first order polynomial — can be calculated. The second coefficient can be obtained by the count rate of40K, resulting from KCl, which is mixed homogeneously with the sample. Expecially for environmental samples with large volumes, this method is very useful, because it takes into account the self-absorption of photons in the sample.

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Abstract  

Instruments that measurein situ radiation from natural or radiochemically-contaminated earth formations must be calibrated in appropriate facilities to provide quantitative assessments of concentrations of radionuclides. For instruments that are inserted into boreholes, these calibration facilities are typically special models having holes for probe insertion and having sufficient size to appear radiometrically infinite in extent. The U.S. Department of Energy (DOE) has such models at Hanford, Washington, and Grand Junction, Colorado. They are concrete cylinders having a central borehole and containing known, enhanced amounts of K, U, and Th for spectral gamma-ray measurements. Additional models contain U for calibrating neutron probes for fissile materials and total-count gamma-ray probes. Models for calibrating neutron probes for moisture measurements in unsaturated formations exist for steel-cased boreholes at Hanford and for uncased boreholes at the DOE's Nevada Test Site. Large surface pads are available at Grand Junction for portable, vehicle-mounted, or airplane-mounted spectral gamma-ray detectors.

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Abstract  

The unusual mechanical properties (i.e. shape memory effect and superelasticity) of shape memory alloys (SMA) rely on the thermoelastic martensitic transformation (TMT) which is a first-order solid-solid, non-diffusive phase transition, athermal in character. Differential scanning calorimetry (DSC) is often used as a convenient method of investigating the thermal properties ofSMAs. The common practice of standard temperature calibration, required for a correct instrument performance, is here critically discussed in relation to the study of both the direct exothermic transformation on cooling, and the reverse endothermic transformation on heating in a NiTiSMA. The DSC results show that, with the standard temperature calibration, the instrument is calibrated on heating but un-calibrated on cooling. A general method is advanced to overcome this problem, intrinsically related to the dynamic character of DSC.

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Performance validation of step-isothermal calorimeters

Application of a test and reference reaction

Journal of Thermal Analysis and Calorimetry
Authors: B Finnin, M O'Neill, S Gaisford, A Beezer, J Hadgraft, and P Sears

Abstract  

Isothermal calorimetry is becoming indispensable as a tool for the study of a wide variety of systems. As with all scientific instruments it is essential that robust calibration routines be developed in order to validate the data obtained. Chemical test reactions offer many advantages over (the traditionally used) joule effect heating methods, not least because they have the potential to validate instrument performance (i.e. they can be used to assess all aspects of calorimeter operation). In this work the results of a validation exercise, conducted by Thermal Hazard Technology as part of an installation routine, using the base catalysed hydrolysis of methyl paraben are discussed. In the case described, a systematic misreporting of the reported temperature of a calorimeter was identified, caused by an upgrade to the calorimeter's firmware, a discrepancy which may not have been noted using traditional electrical calibration methods and one which highlights the importance of both manufacturers and end-users adopting chemical test reactions into their test and validation routines.

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Abstract  

A method for the absolute calibrations of -rays spectrometers for voluminous samples using natural radionuclides is suggested. The method is based on relative calibration with a solution of 232Th salts and absolute calibration with K2CO3 or KCl.

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Abstract  

Metrologically based measuring procedures and evaluation methods are recommended as guidance for practical temperature, heat and heat flow rate calibration of DSC instruments which are largely independent of instrumental, test and sample parameters. The relevant terms are defined, the measuring procedures and evaluation methods described, calibration materials and their characteristic data stated and guidance for the sample handling provided. Reference is made to three extended papers on calibration. The recommendations were developed by the working group ‘Calibration of Scanning Calorimeters’ of the German Society of Thermal Analysis (GEFTA).

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Abstract  

Personnel from the Pennsylvania State University's Breazeale Nuclear Reactor assisted NRC (Nuclear Research Corporation) personnel in calibrating a new MSL/16N Nitrogen-16 Monitor. This paper describes the neutron flux calibration procedures utilized and the results obtained for the production of a nitrogen-16 source of known activity for a BGO detector calibration.

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