DSC measurements in open pans are often disturbed by mass losses such as sublimation during melting or release of water during
chemical reactions. By simultaneous DSC and TG measurements the DSC signal can be corrected. For this purpose, a temperature
dependent calibration function has to be determined by which the SDTA signal from the TGA/SDTA851e measuring cell can be converted into a heat flow curve (DSC).
By this procedure, accurate heat of melting can be determined despite ongoing sublimation in open pans. This method is illustrated
with reference of the melting of anthracene.
Additionally, condensation reactions were investigated and analyzed by DSC/TG even under ambient pressure, knowing the heat
of evaporation. Using phenol formaldehyde resins the influence of the presence or the release of volatile reaction products
on the reaction rate and kinetic parameters were studied.
In general, the method can be used to correct DSC curves for thermal effects related to mass change.
The Analytical Development Section of Savannah River Technology Center (SRTC) was requested by the Facilities Disposition Projects (FDP) to determine the holdup of enriched uranium in the 321-M facility as part of an overall deactivation project of the facility. The 321-M facility was used to fabricate enriched uranium fuel assemblies, lithium-aluminum target tubes, neptunium assemblies, and miscellaneous components for the production reactors. The results of the holdup assays are essential for determining compliance with the Waste Acceptance Criteria, Material Control & Accountability, and to meet criticality safety controls. This report covers calibration of the detectors in order to support holdup measurements in the C and D out-gassing ovens. These ovens were used to remove gas entrained in billet assembly material prior to the billets being extruded into rods by the extrusion press. A portable high purity germanium detection system was used to determine highly enriched uranium (HEU) holdup and to determine holdup of 235U, 237Np, and 241Am that were observed in these components. The detector system was run by an EG&G Dart system that contains the high voltage power supply and signal processing electronics. A personal computer with Gamma-Vision software was used to control the Dart MCA and provide space to store and manipulate multiple 4096-channel -ray spectra. The measured 237Np and 241Am contents were especially important in these components because their presence is unusual and unexpected in 321-M. It was important to obtain a measured value of these two components to disposition the out-gassing ovens and to determine whether a separate waste stream was necessary for release of these contaminated components to the E-Area Solid Waste Vault. This report presents determination of the calibration constants from first principles for determination of 241Am and 237Np using this detection system and compares the values obtained for 237Np with the calibration factors obtained with a subsequent measurement using a point source of radioactive equilibrium 237Np/233Pa.
The self-attenuation correction factor is used to relate the efficiency for a sample with a given matrix to the efficiency for an ideal sample with identical geometry but negligible photon attenuation. A certain linear relation for the efficiency for a given sample as a function of the efficiencies for a number of subsamples into which the original sample can be decomposed is established and experimentally validated. This relation can be used also in the case when the sample and the subsamples have different matrices. In this way the efficiency for volume samples with arbitrary compositions and densities can be constructed on the basis of the efficiencies (independently measured) for a number of basic geometries. Also a possibility to check the consistency of efficiency calibrations carried out with different standard sources (with different matrices) is provided.
Authors:K. Abel, A. Schilk, D. Brown, M. Knopf, R. Thompson, and R. Perkins
A large area beta scintillation detector has been developed which is currently capable of determining Sr-90/Y-90 contamination in surficial soils. The detector system employs scintillating fiber optic arrays, with active dimensions approximately 15 cm wide by 100 cm long, both ends of which are coupled to multiple photomultiplier tubes (PMTs). Electronic processing includes coincidence requirements to optimize sensitivity and selectivity for the 2.28 MeV (maximum) beta particle from Y-90. Low energy beta particles and gamma rays are discriminated against using double ended and multi-layer coincidence requirements. The detector system is personal-computer-software controlled and data restored in a format compatible with standard database software for ease of final data reduction. Experimental calibration studies have shown a linear response for Sr-90/Y-90 soil concentrations from 12 to over 500 pCi/g and a discrimination factor of 50 to 1 versus Cs-137.
Two compounds are described with interesting properties for use in DSC. The first compound is adamantane (C10H16), with a reversible solid-solid transition at 208.62 K , suitable for DSC calibration at this low temperature . The second compound is 4,4'-azoxyanisole (C14H14N2O3), with a liquid crystal range between 390 and 407 K . This compound shows two transitions on heating, with a large heat effect at 390 K and a small heat effect at 407 K. For this reason, this substance is well suitable for testing the sensitivity and the resolution of DSC instruments . For both compounds not only the heating, but also the cooling behaviour is investigated.
In order to calibrate a gamma-ray spectrometer for radioactivity measurements in environmental samples, it is essential to
use standard radioactive sources in the appropriate geometrical configuration. However, the lack of standard sample due to
any reason would necessitate the use of reference materials as reliable alternative. They often appear in many matrices and
densities. Accordingly, special attention should be drawn towards optimizing the calibration. This work studies the errors
encountered because of the attenuation process due to the density difference of the samples (including reference samples)
aliquots with identical matrix contents. The highest effect was noticed in the lower energy regions. This study suggests that
even for the reference samples with the same matrix, it is necessary to set a recommended density for the measurement process
to avoid the errors due to the attenuation. If this is not practically possible it is recommended that attenuation correction
due to matrix contents followed by another correction due to density correction would be a reliable approach to reach an optimum
Authors:R. McDonald, A. Smith, D. Hurley, E. Norman, and M. Schoonover
Following many years of productive research, the 184-inch Cyclotron, the SuperHILAC, and the BEVALAC accelerators at the Berkeley
Laboratory were closed, leaving thousands of concrete shielding blocks available for reuse, recycling, or disposal. The process
history of these blocks precludes free release pending radiological characterization. This paper describes a procedure whereby
a high efficiency shielded germanium spectrometer is used to rapidly characterize natural and man-made activity within the
blocks. The spectrometer is moved up to the block and 5 minutes of data are collected at the point on the block that registers
highest on a micro-R meter. Sensitivity is better than 1 pCi/g (0.037 Bq/g) for Co-60 and Eu-152, the prominent man-made activities
observed. One-time calibration of the detector system is obtained from a sample of concrete, drilled with a hammer drill,
counted in our low-background facility, and compared to crushed rock with known U, Th, and K activity. A simple relationship
exists between the counts/minute observed in a characteristic gamma-ray peak and the activity in the block.
Authors:L. Bennett, D. Sims, W. Andrews, and K. Nielsen
A computer program entitled SCAAP (Set-up, Calibration, Acquisition and Analysis Program) has been designed to make gamma-ray spectroscopy easily useable by staff in laboratories at the Slowpoke-2 Facility at RMC and in support of the Canadian Forces Nuclear Emergency Response Teams (NERTs). The former group utilises gamma-ray spectroscopy for neutron activation analysis (NAA), while the latter may need to have inhalation dose rates calculated. The intent of this program, written using Microsoft Visual Basic, is to provide a simplified interface between the operator and the spectroscopy equipment and to provide the calculations necessary to produce results quickly. There are five sections (Setup, Calibrate, Acquire, Analyse and NAA) of which the first four are linked. In these sections, a checklist of procedures is presented and automated for the user to set up and calibrate the equipment and then to analyse spectra to provide various dose rates. In the unlinked section, NAA, gamma-ray spectra are analysed to provide elemental concentrations in samples.
Authors:R. Jakopič, A. Verbruggen, R. Eykens, F. Kehoe, H. Kühn, Y. Kushigeta, U. Jacobsson, J. Bauwens, S. Richter, R. Wellum, and Y. Aregbe
In nuclear safeguards, precise and accurate isotopic analyses are needed for two major elements from the nuclear fuel cycle:
uranium and plutonium. This can be achieved by Isotope Dilution Mass Spectrometry (IDMS), which is one of the most reliable
analytical techniques for the determination of plutonium amount content to a high level of accuracy. In order to achieve reliable
isotope measurements isotopic reference materials with certified amount of plutonium and isotopic composition are required.
At the Institute for Reference Materials and Measurements (IRMM) various plutonium spike reference materials for isotopes
239Pu, 240Pu, 242Pu and 244Pu are available. This enabled the setup of an inter-calibration campaign inter-linking selected plutonium spikes on a metrological
basis applying state-of-the-art measurement procedures. The aim of this campaign is threefold: firstly to perform measurements
on selected plutonium spike isotopic reference materials for quality control purposes, secondly to verify the amount content
and the isotopic composition of the recently produced IRMM-1027m large sized dried (LSD) spikes and thirdly to demonstrate
IRMM’s measurement capabilities for plutonium analysis via external quality tools. The obtained results using various spike
isotopic reference materials will be presented and discussed in this paper. The measurement uncertainties of the IDMS results
were calculated according to the guide to the expression of uncertainty in measurement (GUM).
The LabSOCS software performs mathematical efficiency calibration of Ge detectors. Extensive tests have been conducted comparing the LabSOCS efficiency calibration with those from traditional radioactive sources for typical laboratory geometries. For this study, 4 NIST-traceable standards containing 13 different energy lines were counted in 7 different geometries that are typical of laboratory samples. The results from the first 13 detectors produced using this process show that efficiency calibrations generated with LabSOCS have an accuracy of 5.1% SD at low energies and 4.2% SD at high energies.