Authors:Yong Chung, Young Chung, Kyung Cho, and Joung Lee
Trace and toxic elements in Certified Reference Material (CRM) made of Korean rice at the Korea Research Institute of Standards and Science have been analyzed by Instrumental Neutron Activation Analysis (INAA). Data intercomparison from the measurement with those of Atomic Absorption Spectrometry (AAS) and Induced Coupled Plasma Spectrometry (ICPS) has been studied. The powdered samples were sterilized at 1.5·106 rad in the bottles using a60Co source after sieving and spiking to specific elements such as As, Cd, Cr, Cu and Hg and then the homogeneity of samples was assessed. Rice flour (SRM 1568a) and standard solutions made by the National Institute of Standards Technology (NIST) were used to construct the calibration curves for the INAA and the chemical methods, respectively. The uncertainties and concentration of constituent elements were determined and the possibility of their use for analytical quality control was considered.
Authors:P. Oropesa, A. Hernández, and R. Gutiérrez
The establishment of a quality management system is the best way to comply with international requirements concerning the achievement of confident and traceable analytical results. Some important points dealing with the technical factors of quality management in gamma-ray spectrometry of environmental samples are discussed. The experience obtained from analytical procedure validation is presented. Results of the application of standardized procedures to the analysis of ALMERA intercomparison samples, as well as the outcome of the utilization of certified reference materials for the quality control of measurement are presented. In fact, the implantation of simple technical principles reports reliable results and allows to elevate the quality of the measurements at a cost relatively low according to the real possibilities of the small laboratories, even in developing countries.
Radiochemical neutron activation method is presented for the determination of iridium in geological materials. The procedure consisted of thermal neutron irradiation of an 500 mg sample followed by sinterization with sodium peroxide, precipitation with tellurium and high resolution gamma-spectrometry with a hyper-pure Ge-detector. The procedure was evaluated by the analysis of the certified reference materials SARM-7 and W-1. The detection limit for the analytical conditions employed was 0.004 ng·g–1 Ir. The procedure was applied to the reference materials TDB-1 and WGB-1, which present provisional values for Ir concentration, and GXR-3, GXR-5 and GXR-6, which do not present any reported data for Ir contents.
A new, very accurate (definitive) method for the determination of trace amounts of cobalt in biological materials has been devised. The method is based on combination of neutron irradiation with quantitative and selective post-irradiation separation of cobalt from all accompanying radionuclides followed by measurement by -ray spectrometry. Column chromatography in which owing to addition of Co carrier the course of separation can be followed visually is the key element of the separation scheme. Several criteria have been formulated which must be simultaneously fulfilled in order to acknowledge the result as obtained by a definitive method. The high accuracy of the method has been demonstrated by the analysis of several certified reference materials of widely different Co contents.
A method for the determination of trace amounts of Mo, Cd, Co and Cr in biological materials by neutron activation analysis with radiochemical separation is presented. The method is based on the ion-exchange scheme developed by SAMSAHL, where Co and Cr are trapped on BioRad Chelex-100 and Cd and Mo on BioRad AG2X8. The elements Mo, Cd and Co can be determined without systematic errors. For the element chromium the situation is less clear, partially due to lack of sufficient certified reference materials for Cr. The method has been used in the characterization of candidate reference materials. Detection limits in these materials range from 1.5 g/kg for Co to 10 g/kg for Cr. Actual levels as low as 8 g/kg for Cd and 7 g/kg for Co were measured.
Authors:A. Senhou, A. Chouak, R. Cherkaoui, M. Lferde, A. Elyahyaoui, T. El Khoukhi, M. Bounakhla, K. Embarche, X. Bertho, A. Gaudry, S. Ayrault, and D. Piccot
In this paper the performances and the limitations of three multi-elementary analysis techniques are compared applied to a study of air pollution biomonitoring in Morocco. These techniques are: (1) 14 MeV neutron activation analysis (14 MeV-NAA), (2) thermal neutron activation analysis using the k0 quasi-absolute method (k0-NAA) and (3) energy dispersive X-ray fluorescence analysis (ED-XRF). The experimental procedures and the control of the analytical results using certified reference materials are described and discussed. The three methods were confronted for the analysis of lichens, mosses and tree-barks. The complementarity of these methods enabled us to determine 43 elements in different samples. The most suitable method for each element was selected according to the sensitivity and selectivity necessitating the minimum corrections of the matrix effects and/or the interfering reactions.
As part of an ongoing Great Lakes deposition study, we have determined a series of heavy metals in air filter samples collected near Lake Ontario. To decrease our detection limits for key elements used in our receptor modeling, we have employed instrumental epithermal neutron activation analysis (NAA) and Compton suppression techniques. Our detection limits were much better than those with thermal NAA, typically, 0.3 ng for Sb, 0.7 ng for As, 8 ng for Cd, 0.2 ng for In, 14 ng for I, 5 ng for Mo and 2 ng for U. Silicon, which is usually not reported in conventional NAA results for air filters, was routinely determined at the 60 g level. Accuracy was corroborated by analyzing the certified reference material concurrently.
Authors:B. Smodiš, R. Jaćimović, G. Medin, and S. Jovanović
The k0-standardization method of INAA (instrumental neutron activation analysis) was applied to three reference materials: NIST (National Institute for Standards and Technology, Washington, D.C., USA) SRM (Standard Reference Material) 1646 Estuarine Sediment, NIST SRM 2704 Buffalo River Sediment and IAEA (International Atomic Energy Agency) CRM (Certified Reference Material) SL-1 Lake Sediment. Among the 50 elements sought yielding long-lived radioisotopes after (n, ) activation, for 32 elements numerical values were obtained, and for the remaining 18, only detection limits were estimated. When comparing the results obtained in this work to certified, recommended or other literature values, good agreement was found, proving that the same analytical procedure can be applied with confidence for analysis of environmental sediment samples.
A new approach for the determination of elemental uranium in uranium bearing ore, using high resolution -ray spectrometry, was applied. Using a variant of the enrichment technique an agreement of better than 1% has been obtained between -ray measurement results and a certified value obtained by other analytical methods. For the calibration of the -ray spectrometer uranium reference samples have been used which are made available jointly in Europe and the USA as Certified Reference Materials for Gamma-Ray Spectrometry (EC NRM 171 and NBS SRM 969, respectively). The measured ore has been put in a special designed container which ensured in all directions seen from the radiation window an uniform degree of infinite thickness of about 95%. The results can be taken as an example for the applicability of -ray spectrometry when high accuracy is required and under conditions were homogeneously distributed elemental uranium is embedded in larger amount of matrix material.
Authors:R. Dybczyński, M. Wasek, and H. Maleszewska
A highly accurate and precise procedure deserving the name of definitive method has been devised for the determination of copper in biological materials. The method is based on combination of neutron activation and very selective and quantitative post-irradiation separation of copper from other radionuclides by extraction chromatography, using columns with LIX 70 on Bio-Beads SM-1, followed by gamma-ray spectrometric measurement. All potential sources of errors were carefully examined and eliminated or appropriate corrections were introduced into the procedure. The method contains several warning mechanisms safeguarding against making gross errors. Limit of detection for rather short irradiation time (tir
1 h) (which enables radiochemical work without sophisticated shielding) amounts to 15 g/kg. Results for copper concentration in several NBS, IAEA and other certified reference materials are presented and a new recommended value for IAEA's Milk Powder (A-11) is proposed.