H. B. Desai

DETERMINATION OF SCANDIUM, YTTRIUM, SAMARIUM AND LANTHANUM IN STANDARD SILICATE ROCKS, G-1 AND W-1, BY NEUTRON-ACTIVATION ANALYSIS

Abstract Neutron-activation analysis results for four rare earth elements in standard silicate rocks, G-1 and W-1, are reported. An anion-exchange method for the separation of scandium, yttrium, samarium and lanthanum in good radiochemical purity has been developed. The method is based on the chromatographic elution of these elements from a Dowex 1 × 8 (nitrate form) resin column using methanol-nitric acid mixtures. The results obtained by this method are compared with values already available.

A sequential multielement separation scheme for determination of As, Mn, Mo, Cu and Zn in human milk by neutron activation analysis

A simple separation scheme for the analysis of As, Mn, Mo, Cu and Zn using neutron activation is described. It has been checked using three standard reference materials, A-11 milk powder (IAEA) and bovine liver and orchard leaves (USNBS) and found to give acceptable results. This scheme was applied for determination of these trace elements in mature human milk samples. The concentrations of As, Mn, Mo, Cu in samples obtained from two socio-economic groups—low and middle incomes—were not significantly different. However, Zn levels in samples obtained from the poor income group were significantly lower than in those obtained from the other group.

Rare earth impurities in high purity lanthanum oxide determined by neutron activation analysis

Individual rare earth impurities in high purity La2O3 (≧99.9%) have been determined by NAA after pre-separation of the matrix (La). The separation is carried out on an anion exchanger (Dowex 1×8) using different mixtures of methanol/nitric acid as eluants. The rare earth elements from Dy to Lu are eluted quantitatively using a 10% 1M HNO3-90% methanol mixture, while the light rare earths from Ce to Gd are eluted quantitatively using a 10% 0.05M HNO3-90% methanol mixture. La, which is retained on the column, is eluted using 0.1M HNO3. The recoveries of the various rare earth elements have been checked using radiotracers and also by spiking the sample with known amount of elements, and the recoveries are found to be quantitative. Results obtained on a typical high purity lanthanum oxide are reported here.

Daily requirements of Fe, Co and Se during infancy

The daily intakes of trace elements by infants showing optimal pattern of growth are used as the basis to estimate the requirements of Fe, Co and Se during infancy. Since milk is the only food and source of nutrition in the first few months of life, the requirements of these elements are calculated from their average concentrations in human milk and the volume of milk required to supply sufficient amount of energy for maintenance and healthy growth of infants. The concentrations of the three elements in human milk were determined, using the technique of neutron activation followed by radiochemical separation.

Determination of traces of rare earth elements in high-purity uranium by ion-exchange separation and neutron activation γ-spectrometry

Abstract Neutron activation γ-spectrometry is sufficiently sensitive for the determination of traces of rare earth elements but quantitative separation from uranium is essential. The rare earth elements in 0.2 M ammonium carbonate medium are quantitatively retained on Chelex-100, and are quantitatively separated from uranium by recycling the eluate. When 10-g samples are used, neutron activation provides detection limits of 1–20 μg kg −1 . Recoveries of rare earths, checked by spiking with radiotracers, are essentially complete.

Radiochemical neutron activation analysis of individual rare earth elements in monazites from different geological environments

Radiochemical neutron activation analysis /RNAA/ has been applied for the determination of individual rare earth elements /REE/, except Tm, in 8 Indian monazites and one each from Malaysia and Thailand. Because of the very low amounts of heavy rare earths /HREE/ compared to light rare earths /LREE/ in monazite, HREE from Ho onwards have been determined only after the separation of the heavy and light rare earth fractions in the irradiated monazite samples. The results indicate significant variations in REE contents from Eu to Lu among different monazite samples. The chondritic normalized REE patterns of all the samples show a prominent negative Eu anomaly with different slopes at the heavy rare earth end. All the individual REE, except Tm, have been reported for the first time in various Indian monazites.

LOSS OF ELEMENTS IN THE OXYGEN FLASK DECOMPOSITION OF BIOLOGICAL MATERIALS: A STUDY BY NEUTRON ACTIVATION ANALYSIS

Partial loss of elements in the oxygen flask method for the decomposition of biological materials is described. The irradiated sample is placed in a platinum wire gauze or quartz cup and burnt in an oxygen atmosphere in the presence of carrier solutions. The results obtained by radiochemical neutron activation analysis for the elements like Mn, As, Cu, Sb and Zn in different standard reference materials are presented with a discussion of the possible causes for the lower values.

Determination of traces of rare earths in high-purity thorium dioxide by neutron activation analysis

Abstract The use of thorium dioxide as a nuclear fuel requires the determination of individual rare earth impurities at 0.08–1 mg kg−1 levels. Neutron activation is sufficiently sensitive but separation from the matrix is essential. In the proposed method, thorium dioxide (5–20 g) is dissolved in concentrated nitric acid with a little hydrofluoric acid; after evaporation, thorium is complexed with ammonium carbonate and the solution is passed through a small column of Chelex-100 resin which retains the rare earths quantitatively without retaining thorium. The rare earth elements are eluted with dilute nitric acid, concentrated, and irradiated with standards; after irradiation the rare earth are collected on a lanthanum carrier and measured by γ-ray spectrometry. The recoveries of rare earths were checked with tracers and by standard addition to thorium dioxide matrices. The reproducibility for La, Eu and Dy was satisfactory at 0.01, 0.003 and 0.002 mg kg−1, respectively; as was the reproducibility for all rare earths added to thorium dioxide (1–4 μg/5 g). Limits of detection are adequate for certification of nuclear-grade material.

A radiochemical neutron activation analysis method for the determination of tin, arsenic, copper and antimony for the forensic comparison of bullet lead specimens

Trace element characterization of bullet lead by instrumental neutron activation analysis (INAA) is hampered by the high spectral background due to antimony, normally present in high concentration in bullet lead. Tin is indicated to be a very useful element for characterization purposes. Beta-active121Sn is a suitable nuclide for quantitation of tin provided it is separated in high radiochemical purity. A radiochemical procedure capable of determining tin down to 10 ppm in bullet lead, a sequential procedure for its determination along with copper, arsenic and antimony and the application of this procedure for the determination of the contents of these elements in various bullet leads are described. This method has been applied to a “Rhinoceros shoot-out” case, referred to our laboratory.

Use of a carboxylate exchanger in the determination of copper in distilled water by neutron activation analysis

Copper in distilled water is collected on Zeokarb 226(NH4+) and irradiated with thermal neutrons. By comparison of the induced activity of 0.51 MeV photopeak of64Cu with that of a standard, irradiated under comparable conditions, copper at ppb levels is easily determined.