Several instrumental neutron activation analysis techniques (parametric, comparative, and ko-standardization) are evaluated using three reference materials. Each technique is applied to National Institute of Standards and Technology standard reference materials, SRM 1577a (Bovine Liver) and SRM 2704 (Buffalo River Sediment), and the United States Geological Survey standard BHVO-1 (Hawaiian Basalt Rock). Identical (but not optimum) irradiation, decay, and counting schemes are employed with each technique to provide a basis for comparison and to determine sensitivities in a routine irradiation scheme. Fifty-one elements are used in this comparison; however, several elements are not detected in the reference materials due to rigid analytical conditions (e.g., insufficient length of irradiation or activity for radioisotope of interest decaying below the lower limit of detection before counting interval). Most elements are normally distributed around certified or consensus values with a standard deviation of 10%. For some elements, discrepancies are observed and discussed. The accuracy, precision, and sensitivity of each technique are discussed by comparing the analytical results to consensus values for the Hawaiian Basalt Rock to demonstrate the diversity of multielement applications.
Authors:R. Jaćimović, P. Makreski, V. Stibilj, and T. Stafilov
Major and trace element contents in iron ore reference materials were investigated using k0-instrumental neutron activation analysis (k0-INAA). To avoid iron interferences, radiochemical separation was developed (k0-RNAA). The determination of the investigated elements in the inorganic phase from hydrochloric acid solution was performed
after radiochemical separation of iron by diisopropyl ether. It was found that after the Fe elimination, the limit of detection
for some elements was much lower that enables their direct determination. The distribution of 39 elements (with intermediate/medium
and long half-life radionuclides) after Fe removal was investigated.
The National Institute of Standards and Technology (NIST) seaweed Standard Reference Material (SRM4359) was developed through
an intercomparison of 24 experienced laboratories. Several statistical techniques were evaluated for establishing reference
values using the laboratories’ reported values including mean, midmean, median, Type B On Bias (BOB), Graybill-Deal, Mandel-Paule,
Vangel-Rukhin, Cox and Maximum Likelihood. After reviewing the results from all these techniques, the median was chosen as
a suitably robust way to calculate reference values. The uncertainties for the median values were estimated using bootstrap
By the use of non-destructive neutron activation analysis (NAA) twenty-four trace (Ag, As, Br, Cd, Ce, Cr, Co, Cu, Eu, Fe, Hf, I, La, Mn, Ni, Rb, Sb, Sc, Se, Sm, Sr, U, V and Zn) and six minor (Ca, Cl, Mg, K, Na and S) elements were determined in a certified marine tissue standard reference material. Four non-destructive methods including thermal, epi-thermal, prompt-gamma ray and delayed neutron counting activation analyses were performed. Results when compared to the certified values showed the reliability of employing these methods in such standards program.
Authors:M. Wasim, A. Rahman, J. Zaidi, S. Waheed, and S. Ahmad
The proposed reference material from the International Atomic Energy Agency, namely IAEA-407 (Fish Homogenate) was analyzed using instrumental neutron activation analysis (INAA). 15 elements, Al, As, Cl, Co, Cr, Fe, Hg, Mg, Mn, K, Na, Sb, Se, V and Zn, were determined using two irradiations (5 minutes and 5 hours) and four countings. IAEA-MA-A-1/TM (Copepoda Homogenate), NIST-SRM-1566 (Oyster Tissue), NIST-SRM-1572 (Citrus Leaves) and NIST-SRM-1577a (Bovine Liver) were utilized as standards in the quantification step.
Instrumental neutron activation analysis (INAA) was applied to the rapid determination of magnesium in the botanical reference materials Beech Leaves-100 and Spruce Needles-101. The magnesium content was quantitatively determined by measuring the gamma-ray photopeak at 1014 keV of the short-lived radionuclide27Mg (9.46 m). The magnesium concentrations in the two materials were found to be 834.6±50.2 g·g–1 dry weight and 618.6±36.2 g·g–1, respectively. When assaying a 0.1 g sample under the same experimental conditions the limit of detection is 30 g of Mg.
Authors:Zs. Szántó, M. Hult, U. Wätjen, and T. Altzitzoglou
The paper presents the results of radiological investigation of several mushroom samples collected in the fall of 2004 in
different parts of Europe. The work was performed in order to support decision making to develop and produce a certified reference
material for quality assurance of radionuclide measurements in environmental samples. The levels of 137Cs in mushrooms varied widely ranging from 0.6 to 4300 Bq/kg on dry mass basis, while those of natural 40K were relatively constant. In one sample 60Co of unknown origin was detected (25±2 Bq/kg dry mass), while 90Sr concentrations were usually below the detection limit (<150 mBq/kg dry mass).
Two methods have been developed for the determination of platinum group elements (PGEs) and gold in four geological reference materials: one using radiochemical neutron activation analysis and the other using nickel sulphide fire assay, followed by instrumental neutron activation analysis. The results from ten multiplicate measurements have been discussed in terms of precision and accuracy. The average precision for both methods is about 5%. Comparing the reported data with existing values in the literature, the accuracy of the proposed methods is good agreement in most cases. Detection limits in the range 0.001–0.015 ng have been derived for both methods under the operational conditions.
Authors:E. Moreira, M. Vasconcellos, M. Catharino, V. Maihara, and M. Saiki
Instrumental neutron activation analysis (INAA) was used in the homogeneity study of a Perna perna (Linnaeus 1758) mussel reference material. Simultaneous determination of 15 elements in six bottles of the material, from
a total of 171, was performed. The bottles were considered homogeneous for the analyzed elements, at the 95% confidence level,
according to the analysis of variance test performed. Elements were also determined in one bottle with five different sample
masses for minimum sample intake estimation. Results varied from 50 to 350 mg, depending on the element.
A simple radiochemical machine incorporating ion-exchange procedures has been described. The system has been tested repeatedly for the determination of Cd, Co, Cr, Cu, Mn and Mo at ultra trace concentration levels in a variety of biological samples such as reference materials, human blood serum, human milk, hair and certain dietary materials, thereby demonstrating its suitability for practical use. The procedure can also yield results for A, Au and W, without any further chemical manipulations. Results show <1, 0.12, 0.18, 983, 0.61 and 0.91 g/l for Cd, Co, Cr, Cu, Mn and Mo, respectively, in human blood serum. Corresponding concentrations in human milk are <1, 0.25, <1, 186 to 310, 4 to 40 and 5.8 g/l. Among the reference materials, IAEA milk standard A-11 shows 1.85, 5.1, 17, 380, 260 and 101 ng/g for Cd, Co, Cr, Cu, Mn and Mo, respectively. Corresponding concentrations in animal muscle H-4 are 4.1, 5, 10.2, 4000, 455 and 45 ng/g. Importantly, this scheme has been applied to process large number of samples from single investigations such as those arising from dietary studies, obtaining quick and reliable data for routine use.