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Abstract  

Degradation of polymeric materials used in nuclear power plants (NPP), especially polymeric cable insulation materials, in the course of their service can be monitored by measuring their properties by DSC, mainly oxidative induction time — OIT. The studied materials were in-laboratory aged by applying main stressors that act in NPP — ionising radiation and temperature. The dependence of OIT on radiation and thermal degradation of polymeric material was determined. The OIT values have been compared to elongation at break as a property that directly reflects the functionality of the studied material. The comparison of monitored OIT of real cable samples taken from NPP with dependencies on how the OIT values change with the elongation at break, makes possible to establish the extent of cable degradation. This method can be considered as a suitable and effective technique for lifetime assessment not only of cable insulations but also of many other plastics.

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Abstract  

Kinetic evaluation of thermogravimetry data was used to understand the ageing behavior of beeswax used as an artists’ paint medium on ancient mummy shrouds and Fayum portraits. Individual components of beeswax were subjected to dynamic thermogravimetry to assess their evaporation rates, and three methods of kinetic analysis were evaluated for accuracy. The results showed that although it is impossible to accurately predict the volatility at room temperature for individual components of beeswax due mostly to their high molecular mass, relative trends and ranking of the volatility of the compounds can be obtained which may explain compositional changes over time.

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Journal of Thermal Analysis and Calorimetry
Authors:
E. T. Stepkowska
,
J. M. Blanes
,
A. Justo
,
M. A. Aviles
, and
J. L. Perez-Rodriguez

Summary Two hydrated and aged cement pastes from India (NCB), w/c=0.4, of a similar chemical composition but of a different specific surface and different strength (OPC, C-33 and C-43), hydrated at w/c=0.4 for 1 month, were studied by XRD after 1 year and 5-6 year ageing on contact with air. They were tested by static heating (SH) in fresh state, and by DTA/DTG/TG, IR and mass spectrometry (MS), after ageing, presented elsewhere. The main XRD peaks of (i) portlandite were decreasing with T and disappearing about 450°C, (ii) calcite peak at room T was small and broad, it increased gradually, especially after portlandite disappearance; above 600°C it was lowered and it was lost above 700°C. Important variation in the d(001) of portlandite with ageing was observed, exceeding the standard value of d(001)=4.895 Å (72-0156). It was higher in the paste C-33 (4.925-4.936 Å), containing more carbonates, than in the paste C-43 (4.916-4.927 Å). Small variations only were found in the value of d(101), i.e. 2.627-2.635 Å (nominally 2.622 Å), whereas the d(104) of calcite could be used as internal standard and other calcium carbonates (vaterite and aragonite) showed a small variation only. The increase ind(hkl) with temperature was straight linear (in portlandite ?d(001)=0.095 Å, at 30-400°C) and the thermal expansion coefficient estimated thereform was high (4.75-4.95·10-5 K-1). Close to the T of decomposition the ?d/?T became steeper. The thermal variation of d(104)=3.035 Å of calcite (?d=0.015 Å at 30-400°C) was smaller than that ofd(101) of portlandite (?d=0.025 Å at 30-400°C) and was similar in C-33 and C-43. The thermal expansion coefficient was 1.54 10-5 K-1, thus higher than the reported aa=0.65·10-5 K-1.

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A series of aged granulated blast furnace slags were investigated by DTA. Devitrification characteristics were found to change as a function of age, and regular trends could be established. XRD showed the devitrification process to result predominantly in melilite formation and minor amounts of merwinite, depending on slag age.

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Abstract  

Radiocarbon ages of 17 ancient Japanese documents of known age and 3 unknown samples were measured by AMS. Radiocarbon dating on the known documents concluded that the Japanese paper is a suitable sample for radiocarbon dating because of small discrepancy between the calibrated radiocarbon age and the historical age due to the characteristics of Japanese paper. From the dating of the paper samples of unknown age, the wood-block prints, it was clarified that they had been produced between the 11th century and the first half of the 12th century as the historical information suggested.

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Journal of Radioanalytical and Nuclear Chemistry
Authors:
Yan Chen
,
Zhi-yuan Chang
,
Yong-gang Zhao
,
Ji-long Zhang
,
Jing-huai Li
, and
Fu-jun Shu

Abstract  

An isotope dilution multicollector inductive coupled plasma mass spectrometry (ID-MC-ICP-MS) method for determining age of trace Pu through measuring 241Pu/241Am, 240Pu/236U ratio was established. At the same time, other two methods-α-spectrometry combined with MC-ICP-MS and liquid scintillator combined with α-spectrometry through measuring 241Pu/241Am ratio to determine the age of trace Pu were also studied. The techniques were explored for the age determination of nanogram grade Pu sample on the basis of Pu/Am, Pu/U separation. The ages of two Pu samples—one with known and the other with unknown age—were determined by the three methods. The determined ages by the three methods were all in agreement with the reference value. The established methods for determining the age of trace Pu could be adopted in the verification activities of nuclear safeguards and nuclear arms control.

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Abstract  

Rib bone samples of human accident victims were analyzed for thorium. The analysis was carried out using neutron activation technique to determine Th-232. The age of the victims ranged between 6 years and 65 years. The thorium concentration was found to increase with age. The measured concentration ranged from 0.20 ng/g fresh weight at age 6 years to 1.84 ng/g at age 65 years. The arithmetic mean and geometric mean concentrations were found to be 0.54±0.38 ng/g and 0.46x/÷1.8 ng/g (by excluding the outlier high value of 65-year-old individual). These values are much lower in comparison to those reported by earlier workers. Assuming the total skeletal weight as 14.3% of the body weight and taking the average Indian's body weights as 14.5, 38 and 50 kg at ages 5, 15 and >18 years, the estimate of total skeletal thorium was made.A plot of the total skeletal thorium with age groupings 0–10, 10–20... 50–60 years could be fitted into a linear relation with age. However, the deviation of data in 40–50 and 50–60-year age groups was such that the data could also be fitted into a sub-linearly increasing curve. Both the fittings, however, show a considerably lower rate of uptake in bone than that expected from substitution of Indian (Bombay) intake data into the ICRP model of Th metabolism.

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Abstract  

The hyphenated thermal analysis-mass spectrometry technique (TA-MS) was applied for the investigation of the thermal behavior of reference and aged parchment samples. The kinetic parameters of the process were calculated independently from all recorded TA and MS signals. The kinetic analysis showed the distinct dependence of the activation energy on the reaction progress. Such behavior is characteristic for the multistage mechanism of the reaction. The comparison of the kinetic parameters calculated from the different signals i.e. TG, DSC, MS for H2O, NO and CO2, however, indicated that they were differently dependent on the aging of the sample. For the parchment samples, the aging almost does not change the kinetics of the decomposition calculated from the DSC data: the influence of aging seems to be too negligible to be detected by these techniques. On the other hand, the much more sensitive mass spectrometric technique applied to the kinetic analysis allowed monitoring of visible changes in the thermal behavior of the parchment samples due to the aging process. The influence of aging was especially visible when the MS signals of water and nitric oxide were applied for the determination of the kinetic parameters. The applied method of the kinetic analysis allowed also the prediction of the thermal behaviour of reference and aged parchment samples under isothermal and modulated temperature conditions. Presented results have confirmed the usefulness of thermoanalytical methods for investigating behaviour of such complicated systems as leather or parchment.

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Abstract  

The age of plutonium is defined as the time since the last separation of the plutonium isotopes from their daughter nuclides. In this paper, a method for age determination based on analysis of 241Pu/241Am and 240Pu/236Pu using ICP-SFMS is described. Separation of Pu and Am was performed using a solid phase extraction procedure including UTEVA, TEVA, TRU and Ln-resins. The procedure provided separation factors adequate for this purpose. Age determinations were performed on two plutonium reference solutions from the Institute for Reference Materials and Measurements, IRMM081 (239Pu) and IRMM083 (240Pu), on sediment from the Marshall Islands (reference material IAEA367) and on soil from the Trinity test site (Trinitite). The measured ages based on the 241Am/241Pu ratio corresponded well with the time since the last parent-daughter separations of all the materials. The ages derived from the 236U/240Pu ratio were in agreement for the IRMM materials, but for IAEA367 the determination of 236U was interfered by tailing from 238U, and for Trinitite the determined age was biased due to formation of 236U in the detonation of the “Gadget”.

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Abstract  

Reactor thermal neutron irradiation of biological matrices induces high levels of intense gamma-ray or bremsstrahlung radiation from82Br,42K,24Na, and32P, that interfere with the determination of As, Cd, Cu, and Mo by INAA. Central nervous system (CNS) issue samples from subjects with Alzheimer's disease (AD), amyotrophic lateral sclerosis (ALS), and controls were analyzed using a simple RNAA procedure involving a rapid two-step solvent extraction procedure to determine these four elements. Significant increases (p0.05) in concentrations of Cd and Mo were observed for brain of AD subjects compared to controls, but significant imbalances were not observed for ALS subjects. Concentration data for these elements in selected international reference standards are also presented.

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