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Abstract  

A new application of neutron transmutation doping is described. The method is useful to prepare graded zinc contents in highly pure copper materials. The research reactor BER II at the Hahn-Meitner-Institute, Berlin served as a neutron source. The zinc content produced in the samples was analyzed by determining the 65Zn-activity via gamma-spectrometry. Simultaneously irradiated flux monitors were used to determine the neutron flux density. Since cylindrical sample geometries are favorable for a reference material application in optical emission (OE) spectroscopy, the spatial distribution of the induced activity in a cylinder with a diameter of 8 mm and a length of 35 mm was investigated.

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The centification of standard reference materials is of fundamental importance for environmental scientists to proceed with their own quality control programs or calibration procedures. As part of the National Institute of Standard and Technology (NIST) program, we participated in the certification of a hazardous waste material. Our efforts concentrated on judiciously using thermal and epithermal neutron activation analysis in conjunction with Compton suppression techniques. We have demonstrated that besides lowering the detection limit for several elements usually not reported by conventional NAA, Compton suppression is ideally suited to substantially reduce certain spectrla interferences. A detailed comprehensive study was undertaken using this method to highlight which isotopes can be most favorably used.

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Instrumental neutron activation analysis was applied to the determination of the elements Na, K, Br, As, Rb, Zn, Co, Fe and Sc in Brazilian rice samples and in biological standards. Hg and Se concentrations were determined by using a simple radiochemical separation. The chemical procedure was carried out by means of distillation of Hg and Se in HBr medium and subsequent precipitation of selenium by sodium metabisulfite and mercury by thioacetamide. The accuracy of the instrumental and radiochemical methods was evaluated by means of analysis of the Reference Materials NBS-Bovine Liver, Bowen's Kale and NBS-Rice Flour.

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The paper describes a destructive neutron activation procedure especially set up for the determination of low levels of iridium. Only a few steps are required after irradiation, namely sample dissolution, noble metals adsorption on an ion-exchange column, removal of interfering radionuclides and counting. Successively iridium is removed from the column and the chemical yield evaluated. The method has been used for the determination of iridium in a large variety of standard reference materials, including materials of geological, biological and technological origin, with iridium levels ranging from about 0.005 to 18 ng/g. Results, given as the average of three or more independent analyses, and relative standard deviations, are reported and discussed. Average precision is about 8%, and the sensitivity is 0.004 ng.

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The instrumental neutron activation analysis technique (INAA) was used for homogeneity tests and certification analyses of the coal fly ash reference material ECO prepared at the Institute of Radioecology and Applied Nuclear Techniques (IRANT), Koice, Czechoslovakia. The relative standard deviations due to inhomogeneity were found to be <3% for 19 elements including for sample weights about 50 mg. The results of determination of the elements Al, As, Ba, Ca, Ce, Co, Cr, Cs, Dy, Eu, Fe, Ga, Hf, In, K, La, Mn, Mo, Na, Nd, Ni, Rb, Sb, Sc, Sm, Sr, Ta, Th, Ti, U, V, W, and Zn, were compared with the IRANT certified or information values. Inference was made on the reliability of the IRANT specified values for the element contents.

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Abstract  

Homogeneity study is one of the steps in reference material, RM, characterization. Due to its inherent characteristics, Instrumental Neutron Activation Analysis, INAA, is an analytical technique of choice for homogeneity testing. An interesting possibility is the use of complementary gamma ray photopeaks to confirm INAA homogeneity test results. In this study, the use of the complementary gamma ray photopeaks of 110mAg, 82Br, 60Co, 134Cs, 152Eu, 59Fe, 140La, 233Pa (for Th determination), 46Sc and 75Se radionuclides was investigated in the between bottle homogeneity study of a mussel candidate RM under preparation at IPEN–CNEN/SP. Although some photopeaks led to biased element content results, the use of complementary gamma ray photopeaks proved to be helpful in supporting homogeneity study conclusions for the new RM under characterization.

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The k 0 parametric neutron activation analysis has been applied since 1995 in the Radiochemical Sector/CDTN, Belo Horizonte, Brazil. Several certified reference materials were studied with the aim of analysing biological samples. This work is related to an IAEA co-ordinated research project whose goal is to make a survey of the exposures to metals related to occupational diseases. It has been conducted by CDTN and government departments of health. The hair samples as bioindicators were donated by galvanising factory workers in Belo Horizonte. This city and surrounding area are important industrial centres and that industry is responsible for the majority of patients who look for medical assistance because of metal contamination. The Al, Co, Cu, Cr, La, Mn, Sb and V concentrations determined in the workers' samples suggest endogenous contamination.

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Abstract  

A fast (14-MeV) neutron activation analysis procedure was employed to directly measure mass fractions of oxygen in coal samples. The procedure demonstrated sufficient precision and accuracy to determine a relative change of about 5% or more, in the oxygen mass fraction of about 12%. The procedure was applied to test samples of the newly developed SRM 1632c Trace Elements in Coal (Bituminous). The samples had been stored at three conditions: in liquid nitrogen vapor and at room temperature in the original containers packaged under argon, and for accelerated aging at 50 °C open to air. Following six months storage increments, duplicate samples of each of twelve bottles of the SRM were measured for each storage condition. In addition each sample was processed through ten separate analytical runs yielding a total of some 720 measurements per storage duration. Oxygen was determined by comparison to a primary standard potassium dichromate and the accuracy of the method was assessed through the analysis of replicate samples of three reference materials that are certified for oxygen content. The initial 6-months test period indicated uptake of oxygen in the open-air storage.

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This paper presents the results of the proficiency test exercise conducted in Pakistan for the determination of trace elements in mushroom reference material. Thirteen laboratories from different organizations of the country submitted trace elemental data on Al, As, Br, Ca, Cd, Ce, Cl, Co, Cr, Cs, Cu, Fe, Hg, K, Li, Mg, Mn, Na, P, Pb, Rb Sc, Si, Sm, Sr, Th, Zn. Results for Al, As, Br, Ca, Cd, Cl, Co, Cr, Cs, Cu, Fe, K, Mg, Mn, Na, Rb Sc, and Zn, in the mushroom material were reported by two or more participating laboratories and could be subjected to statistical evaluation. The original data of these trace elements was subjected to a computer program “Histo Version 2.1” provided by IAEA. The four outlier tests, i.e., Dixon, Grubbs, skewness and kurtosis were applied to the data sets. Consensus (overall) mean values, absolute standard deviation, relative standard deviation, standard error, median and range of values for these elements have been reported at a significance level of 0.05.

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Abstract  

The characterized concentrations of 24 impurity elements in New Brunswick Laboratory (NBL) Certified Reference Material (CRM) 124 were reevaluated. A provisional certificate of analysis was issued in September 1983 based upon the “as prepared” values (gravimetric mixing). The provisional certificate does not state uncertainties for the characterized values, or estimate the degree of homogeneity. Since release of the provisional certificate of analysis various laboratories have reported analytical results for CRM 124. Based upon the reported data a re-evaluation of the characterized values with an estimate of their uncertainties was performed in this work. An assessment of the degree of homogeneity was included. The overall difference between the re-evaluated values for the 24 impurity elements and the “as prepared” values from the provisional certificate of analysis is negligible compared to the uncertainties. Therefore, NBL will establish the “as prepared” values as the certified values and use the derived uncertainties from this work for the uncertainties of the certified values. The traceability of the “as prepared” values was established by the gravimetric mixing procedure employed during the preparation of the CRM. NBL further recommends a minimum sample size of 1 g of the CRM material to ensure homogeneity. Samples should be dried by heating up to 110 °C for one hour before use.

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