Compton suppression gamma-spectroscopy provides an efficient method for measuring the concentration of226Ra,228Ra, and210Pb in ocean sediments. The background reduction realized from the suppressed mode of operation provides an “active shield”
to allow for the low-level counting required for these measurements. We have used the method to study the possible accumulation
of radium from produced waters in sediments from Gulf of Mexico sites of varied distances from drill platforms. In addition,210Pb levels were determined to evaluate the use of our spectrometer for this purpose. Baseline undisturbed concentrations have
been obtained from the study of subsurface core material which predates drilling activities. Correlations of radium isotope
concentrations with iron and barium provide information concerning the possible relationships between radium levels and drilling
activity (excess barium) and natural variations in sediment texture (iron).
Neutron activation analysis and Ge(Li) spectroscopy was used to determine 32 elements in seven U.S.G.S. standard rocks of
a wide range of composition. Short half-life nuclides (10 sec-10 min) were used to measure Sc, Hf, Dy, Mg, Al, Ca, Ti, V (and
Na) in an automated rabbit Ge(Li) detector system. The elements K, Cu, Zn, Ga, Sr, Ba, La, Eu, Sm (and Mn) were determined
by dissolution of the irradiated sample followed by removal of24Na on hydrated antimony pentoxide (HAP). Long-lived nuclides were used to measure Sc, Cr, Fe, Co, Zr, Rb, Sb, Cs, Ba, Ce,
Eu, Yb, Tb, Lu, Hf, Ta and Th after decay of24Na. The method involves little radiochemistry and the separation is selective for24Na under the experimental conditions used. Elemental concentrations determined agree well with previously published data.
Authors:M. de la Rubia, R. Alonso, J. de Frutos, and A. López-Garcia
The objective of this study is to determine the influence of partial substitutions of Ti4+ by isovalent Hf4+ in the perovskite-type crystalline structure of PbTiO3. Different samples over the whole composition range (0 ≤ x≤1) in the PbTi1-xHfxO3 family have been prepared. Phase transitions have been determined by thermal analysis (differential scanning calorimeter:
DSC) and complex impedance spectroscopy (IS) over a wide temperature range. As a consequence of the cation replacement the
changes that take place in the different phase transition temperature are reported. By both techniques, thermal analysis and
electrical characterization, it is shown that for all compositions prepared there is only one phase transition in a temperature
range between 230 and 460 °C. With these results and the previously known crystalline structure of pure PbTiO3 and PbHfO3 perovskites, the phase diagram of the PbTi1-xHfxO3 family is presented including a morphotropic phase transition at x ~ 0.5.
Authors:Y. Tsujimi, M. Kobayashi, H. Furuta, and T. Yagi
The ultra-slow modes with a relaxation time much longer than 1 ns are discovered by a time-resolved spectroscopy in uniaxial ferroelectric (NH2CH2COOH)3H2SO4 (TGS) and in glass-former HOCH2(CHOH)4CH2OH (D-sorbitol). A mode discovered in TGS is a thermal relaxational mode and is proved to be the physical origin of the central peak found by Brillouin scattering. Two modes are discovered in D-sorbitol. One is a thermal relaxational mode. The other is a mode characterized by the Kohlraush-Williams-Watts function with a relaxation time
R. A remarkable result is that
R indicates a critical behavior not at the liquid-glass transition temperature Tg =–7°C but at the ergodic to nonergodic transition temperature Tc=33°C.
Confinement of the glass-forming regions in the nanometer range influences the α-relaxation which is associated with the glass transition. These effects were investigated for semicrystalline poly(ethylene terephthalate) by dielectric spectroscopy and differential scanning calorimetry. The results are discussed within the concept of cooperative length, i.e. the characteristic length of the cooperative process of glass transition. Both experiments showed a dependence of the glass transition on the mean thickness of the amorphous layers. For the dielectric relaxation, the loss maximum was found to shift to higher temperatures with decreasing thickness of the amorphous layers, but no differences were observed in the curve shape for the differently crystallized samples. For the calorimetric measurements, in contrast, there was no correlation for the glass transition temperature, whereas the curve shape did correlate with the layer thickness of the mobile amorphous fraction. From the structure parameters, a characteristic length of approximately (2.5±1) nm was estimated for the unconfined glass relaxation (transition).
Authors:A. Porto, W. Magalhães, C. Carvalho, and J. Machado
Positron Lifetime Spectroscopy (LS) measurements were performed in a series of binary molecular solid solutions of the general formula M1–xGxL3, where L(ligand)=acetylacetone, dipivaloylmethane, or N-benzoyl-N-phenylhydroxylamine, M=Al(III), Ga(III) or In(III), as matrix, and G=Cr(III), Mn(III), Fe(III), Co(III), Ru(III), Rh(III) and Ir(III), as guest molecules, and the corresponding mechanical mixtures. For the solid solutions, the o-Ps yield values (I3) decrease very rapidly with the increase of the guest mole fraction, showing a high efficient Ps inhibition process, while for the corresponding mechanical mixtures, these values decrease linearly with the increase of the guest molecule concentration, indicating the presence of two distinct phases. These results confirm our previous proposal that the LS technique is able to characterize solid solutions formed by one matrix, in whichI3 values are high, and one guest, in which theI3 values are very low.
Semiconductor particle detectors are ideal for alpha spectroscopy due to their compact size, low noise, and high resolution.
This paper describes the construction and testing of an automatic sample changer for use with such a detector. The changer
was constructed from locally available services and materials. It holds up to 24 samples of alpha emitting material deposited
on 22 mm stainless steel counting planchets. The vacuum chamber can be evacuated to less than 10 μm mercury in 10 to 15 minutes.
Once the chamber has been evacuated and detector bias has been applied, any sample in the chamber may be selected for analysis,
either automatically or manually. Continuous automatic analysis of up to 24 samples is possible. Variation in efficiency from
position to position was found to be 3.25% at the detector-sample spacing of 4.8 mm, and 2.31% at 27 mm. Shielding between
the adjacent samples not under analysis and the detector was acceptable.
Authors:G. Troyer, E. Nordquist, D. Legare, K. Hillesand, S. Kessler, J. Nelson, R. Richard, S. Goodwin, and E. Killian
The cleanup of high-level defense nuclear waste at the Hanford Site presents many challenges. These include removing and disposing
of components from buried active waste tanks to allow new equipment insertion or hazards mitigation. This paper discusses
a unique automated system that provides for retrieval, high-pressure washing, inventory measurement, and containment for disposal.
Key to the inventory measurement is a three-detector high-purity germanium high-performance gamma-spectroscopy system capable
of recovering data at up to 90-percent saturation (200,000 counts/s). Data recovery is based on a unique embedded electronic
pulser and special software to report the inventory. Each detector has different shielding specified through simulation using
the Monte Carlo computer code for N-particle transport modeling. This shielding provides performance over a dynamic range
of eight orders of magnitude. This paper covers system description, calibration issues, and operation.
Authors:Em. Cincu, I. Manea, V. Manu, D. Barbos, O. Sima, I. Gustavsson, P. Vermaercke, N. Vajda, Zs. Molnar, and H. Polkowska-Motrenko
Samples of high alloy Stainless Steel SS 1 were analyzed by instrumental neutron activation analysis (INAA) at 5 research
institutes in 4 European countries within the frame of an Inter-Laboratory Comparison (ILC) exercise aiming at checking if
the results were independent of the standardization methods, and if INAA was accurate enough to contribute to certification.
The mean element concentration values yielded by INAA were also compared with mean values obtained by atomic emission spectroscopy
techniques at other laboratories that took part in the International Proficiency Testing organized by KIMAB Institute of Sweden,
producer of the SS 1. The performances of the nuclear and atomic techniques were compared in terms of the z-score values calculated for 11 element concentrations evaluated by the two analytical ways. Finally, consideration is given
to the ways in which highest accuracy and precision can be ensured for certifying stainless steels as CRMs.
Authors:A. Hensel, J. Dobbertin, J. E. K. Schawe, A. Boller, and C. Schick
The results from temperature modulated DSC in the glass transition region of amorphous and semicrystalline polymers are described with the linear response approach. The real and the imaginary part of the complex heat capacity are discussed. The findings are compared with those of dielectric spectroscopy. The frequency dependent glass transition temperature can be fitted with a VFT-equation. The transition frequencies are decreased by 0.5 to 1 orders of magnitude compared to dielectric measurements. Cooling rates from standard DSC are transformed into frequencies. The glass transition temperatures are also approximated by the VFT-fit from the temperature modulated measurements. The differences in the shape of the curves from amorphous and semicrystalline samples are discussed.