Determination of arsenic and antimony in niobium by radiochemical neutron activation—γ-spectrometry

A method for the determination of arsenic and antimony in niobium, with simultaneous determinations of Au, Cu and Mo, is described. The samples are irradiated for 12 h in a thermal neutron flux of 8 × 10¹³ n cm^-2 s^-1 and then dissolved in hydrofluoric —nitric acid. After addition of various masking agents, and reduction with potassium iodide, As(III) and Sb(III) are extracted with diethylammoniumdiethyldithiocarbamate in chloroform. Before reduction, Au, Cu and Mo can be extracted as dithiocarbamates and determined. For samples of about 100 mg, the limits of detection are 10 pg g^-1 for As, 20 pg g^-1 for Sb, 0.8 pg g^-1 for Au, 10 pg g^-1 for Cu and 25 ng g^-1 for Mo. Results are given for niobium samples of different grades of purity.     

Determination of phosphorus in steels by radiochemical neutron activation analysis

The viability of radiochemical neutron activation analysis as a method for certification of phosphorus in steels was tested by analysis of SRM low alloy steels. Preliminary results are generally in agreement with certified values. The limit of detection, as defined by Currie¹, was determined to be 5 μg/kg.     

Simultaneous determination of arsenic and antimony in environmental samples by radiochemical neutron activation analysis

A radiochemical separation procedure using an inorganic exchanger, tin dioxide (TDO), for the separation of arsenic from antimony is reported here. This separation avoids the interference of 564 keV gamma-ray of¹²²Sb in the measurement of the 559 keV gamma-ray of⁷⁶As in neutron activation analysis. Environmental samples, after neutron irradiation and digestion, are taken up in 1M HCl–0.1M HF and passed through a TDO column which selectively retains arsenic. The effluent from the TDO column, after proper conditioning, is passed through an anion exchange column for quantitative retention of antimony. The procedure has been utilized for arsenic and antimony determination in NBS Orchard Leaves and NBS Albacore Tuna.     

Determination of impurities in tantalum by a radiochemical neutron activation analysis

A radiochemical separation method using Dowex 1×8 (200–400 mesh) has been applied to two tantalum metals of 99.9% purity. While tantalum was still retained on the resin, the elements Na, K, Cr, Mn, Fe, Co and Zn were separated with 2M HF and subsequently the elements Sc, As, Zr, Mo, Eu, W and Hf with a mixture of 0.5M HF and 3M HCl. The separation yields for all impurities was 98–100%. Elemental contents were calculated by a single comparator method using two monitors.     

Determination of gold in biological materials by radiochemical neutron activation analysis

A radiochemical neutron activation analysis procedure was developed for the determination of trace amounts of gold in biological materials. The procedure was realized with irradiation of reference and test samples in a nuclear reactor, selective and quantitative separation of gold using inorganic MnO₂ Resin and gamma-ray spectrometric measurement of ¹⁹⁸Au. The method is characterized by a low limit of detection of gold at ng g^?1 level. Results shows that the method can be applied to the determination of trace amounts of gold in tissues for medical research.     

Determination of rare-earth elements in steels by radiochemical neutron activation analysis

For the separation of rare-earth elements from steel, with a cation exchange resin, separation experiments were performed on NIST reference materials of SRM-363 and SRM-364. Iron, Na, Cr, Mn, Co, Cu, As, Mo, Sb and W were separated in 2M hydrochloric acid, five rare-earth elements, La, Ce, Pr, Nd and Sm and three other elements, Hf, Zr and Ba were separated using 8M nitric acid. Each element was determined by a single comparator method using two monitors, gold and cobalt.     

Determination of cadmium using radiochemical neutron activation analysis

A method has been developed for the determination of cadmium in samples of food and biological materials using neutron activation analysis with radiochemical separation. The irradiated sample is digested in presence of cadmium carrier, with a nitric-perchloric mixture, evaporated to dryness, dissolved in 6M HCl and placed onto an ion exchange column loaded with Dowex 1-X8 resin in chloride form and conditioned with HCl 6M. The cadmium is retained in the resin. After a washing procedure with several portions of HCl of decreasing concentration, the cadmium is eluted with an ammonia-ammonium chloride buffer. The activity of ^115mIn which is in equilibrium with ¹¹⁵Cd, is measured using a NaI(Tl) well type detector. The method has been evaluated by analyzing certified reference materials with cadmium concentrations covering a range of 0.020 to 200 mg^.kg^-1. The agreement of the results with the certified values is within 95%, which gives an indication of the sensitivity and accuracy of the proposed method.     

Determination of trace impurities in tin by neutron activation analysis

Two methods are described to determine indium and managenese in high-purity tin. In the first method indium and manganese are separated from the tin and antimony matrix activities on Dowex 1X8 anion exchanger. Tin and antimony are adsorbed in 10M HF while indium and manganese are eluted. In the second method the incident γ-ray intensity due to the tin matrix is reduced by placing a lead absorber between the sample and the detector. The reproducibility and the sensitivity of both methods are of the order of 10 ppb for manganese and of 1 ppb for indium for 1 g samples and a neutron flux of 10¹¹ n·cm⁻²·sec⁻¹. Aspirant of the N. F. W. O.     

Determination of trace impurities in tin by neutron activation analysis

A method was developed for the determination of 15 trace elements in tin. High-purity tin samples (99.9999% and 99.999%) as well as tin of technical quality were analysed. Reactor neutron activation of the tin samples was followed by distillation of the matrix activities from a HBr−H₂SO₄ medium and Ge(Li) gamma-ray spectrometry of the distillation residue. The sensitivity of the method is generally high. For the high-purity samples the detection limits vary from 0.02 ppb (scandium) to 200 ppb (iron) for irradiation of 1 g of tin for 1 week at a thermal flux of 5·10¹²n·cm⁻². ·sec⁻¹. To decontaminate the surface of the tin samples, pre- and post-irradiation etching procedures were applied. The efficiency of these etching techniques was studied.     

Determination of trace impurities in tin by neutron activation analysis

Arsenic, selenium and antimony were determined in four different tin samples. After distillation from HBr?H₂SO₄ medium arsenic and selenium were precipitated with thioacetamide, and antimony was subsequently separated by deposition on iron powder. The separated samples were counted on a high-resolution Ge(Li) γ-spectrometer. The sensitivity of the method is highly satisfactory.     

Determination of selenium in human diets by radiochemical neutron activation analysis.

A post-irradiation radiochemical separation technique was tested for the determination of selenium levels in diet samples, collected by using a duplicate portion technique, from both rural and urban population groups in Turkey. The technique involved sample irradiation, acid digestion, selective distillation, precipitation and filtration steps. During the separations it was possible to determine the yield of each sample using a stable selenium carrier. An average chemical yield of 71 +/- 3% was obtained for the radiochemical neutron activation analysis. For samples from urban and rural regions, the average selenium concentrations obtained were 0.14 +/- 0.04 and 0.07 +/- 0.02 mg kg-1, respectively. It was also possible to determine daily dietary selenium intakes, which were found to be 81 +/- 41 micrograms and 23 +/- 11 micrograms for the urban and rural groups, respectively. Although daily selenium intakes were found for a small number of subjects in this study, the separation technique developed can be used for determination of the selenium status in larger population groups.     

Determination of U and Th in tungsten by radiochemical neutron activation analysis

A radiochemical separation method using an anion exchange resin has been applied to 4N grade tungsten for determining U, Th and 4 other elements. While tungsten remained in the resin, Na, K and As were separated with 0.05M HCl and 1M HF and then U, Th and Cr were eluted with 1M HCl and 1M HF. The separation yield of neptunium (U) was influenced largely by the amount of thorium, but this influence could be neglected as the concentration of the thorium was below 0.5g/ml. The content of these elements were calculated by a single comparator method using monitors, gold and cobalt. The detection limits of U and Th are 4.0 and 1.2 ppb, respectively.     

Determination of impurities in niobium metal by a radiochemical neutron activation analysis

A radiochemical separation method using an anion exchange resin has been applied to 3N grade Nb for determining nine impurity elements. Five elements (Cr, Fe, Co, Zn and Se) were separated in 2M HF, three elements (Mo, W and Hf) in 32M HF, Nb in 0.5M HF/3M HCl, and Ta in 1M NH₄F/4M NH₄CCl. The contents of the elements were calculated by a single comparator method using two monitors of Au and Co. The main impurity was revealed to be Ta with a content of over 160 ppm.     

Determination of trace quantities of tin by neutron activation analysis

A neutron activation method of general applicability has been developed for determining traces of tin in a variety of samples. The samples and comparative standards, sealed into ampoules, are irradiated intermittently for 3 days at a neutron flux of ca, 3 · 10¹¹ n/cm²/sec, followed by carrier radiochemical separations mainly consisting of solvent extraction steps. As little as 0.1 μg Sn can be easily determined by comparing the induced β-activity of ¹²¹Sn (27.5 h) with that of a standard, The method is rapid and has a reasonably high chemical yield of about 50%. Results are quoted for the tin contents of a number of materials including silicate rocks, sea waters, biological materials and steels.     

Determination of copper in high-purity tin by reactor neutron activation analysis

For the determination of very low concentrations of copper in tin, an analytical method involving reactor neutron activation was developed whereby the copper activity was separated from the tin matrix by extraction of the Cu(I) cuproin complex in n-amyl alcohol. A new decontamination technique was sought in order to remove the copper contamination present on the tin surface. Pre-irradiation removal of the tin surface combined with post-irradiation etching appeared to be the most efficient.     

Determination of traces of phosphorus in gallium arsenide by radiochemical neutron activation analysis

A radiochemical separation procedure has been developed to determine traces of phosphorus in gallium arsenide. In this procedure the indicator nuclide³²P is separated from all other long-lived activation products in high purity. The resulting eluate is sufficiently pure to allow -counting. Because of the high -energy of³²P (1710 keV) the activity can be measured via the Cerenkov effect, whereas most radionuclides, because they have essentially lower -energies, are discriminated by this technique, so that the selectivity of the measurement of³²P is improved considerably. A detection limit of 1 ng/g was achieved when using samples of 50 mg, a thermal neutron flux of _th=1·10¹³n·cm^–2·s^–1, an irradiation time of 36 hours and a measuring time of 1 hour.     

Determination of iodine in human brain by epithermal and radiochemical neutron activation analysis

Despite the role of iodine for proper development of the brain and the functions of the element, the accurate data on its concentration in brain tissue are largely lacking, the main reason being analytical difficulties associated with determination of the element especially at low levels. In this work, samples from human brain regions from Hungarian patients were analyzed using epithermal and radiochemical neutron activation analysis (ENAA and RNAA, respectively). The RNAA procedure is based on alkaline-oxidative fusion followed by extraction of elemental iodine in chloroform. The results were checked by the analysis of biological standard reference materials, namely bovine liver, bone meal and diet, and by comparison with previous results obtained by a different RNAA procedure.     

Determination of iodine in Asian diets by epithermal and radiochemical neutron activation analysis

Samples of diets from China, Japan, Korea, India, Pakistan and Philippines were analyzed using epithermal and radiochemical neutron activation analysis (ENAA and RNAA, respectively) within the framework of the IAEA project “Reference Asian Man”. The RNAA procedure was based on alkaline-oxidative fusion followed by extraction of elemental iodine in chloroform. The analytical methods employed are discussed in terms of detection limits and uncertainties of the results obtained. For quality control purposes a number of NIST biological reference materials, namely diets and foods were analyzed. Results for the diet samples indicate that achieving the WHO recommended daily allowance for iodine may be a problem in most of the above given countries. This revised version was published online in August 2006 with corrections to the Cover Date.     

Determination of antimony in nail and hair by thermal neutron activation analysis

The concentration of antimony in nail and hair was determined by thermal neutron activation analysis. Samples were collected from the workers of an antimony refinery, inhabitants near the refinery, and residents in control area. They were irradiated by Kyoto University 5 000 kW Reactor for 1 h, and cooled for 30 to 100 days. After cooling, the concentration of Sb in nail and hair was estimated by measuring the intensity of gamma-ray from 124Sb of the samples, then the samples were washed by 0.1% aqueous solution of nonionic surface active agent in an ultrasonic cleaner. The gamma-ray spectrometry was done again (after washing). The concentration of Sb in nail before washing was 730 ppm for the workers, 2.46 ppm for habitants near the refinery, and 0.19 ppm for the control; after washing, it became 230 ppm for the workers, 0.63 ppm for habitants, and 0.09 ppm for the control. The concentration of Sb in hair before and after washing was 222 ppm and 196 ppm for the workers, and 0.21 ppm and 0.15 ppm for the control, respectively.