Authors:J. Kučera, V. Sychra, J. Horáková, and L. Soukal
A set of certified Reference Materials was prepared consisting of four natural agricultural soils with normal (n) and elevated (e) levels of element contents: CRM 7001 Light Sandy Soil (n), CRM 7002 Light Sandy Soil (e), CRM 7003 Silty Clay Loam (n), and CRM 7004 Loam (e). In these materials, certified and/or information values of the total contents of the elements As, Ba, Be, Cd, Co, Cr, Cu, Hg, Mn, Ni, Pb, V and Zn, and their fractions extractable by aqua regia, boiling and cold 2M nitric acid were derived from an interlaboratory comparison in which 28 laboratories participated. Highly precise and accurate procedures of instrumental neutron activation analysis (INAA) were employed for homogeneity testing and also for certification of the total element contents. For comparation purposes, NIST SRM-2704 Buffalo River Sediment was analyzed by INAA, as well. The INAA results obtained compared very well with the certified and/or information values for four soil CRMs and also with NIST values for SRM-2704. From this agreement, a very high reliability of the new soil CRMs can be inferred.
Recently, the interest in quantitative determination of rare earth elements has grown considerably, especially in connection
with the space programs. There has also been a need for quantitative methods for rare earth element determination in different
matrices at the National Bureau of Standards. We have therefore applied some of our earlier qualitative investigations with
di(2-ethylhexyl) orthophosphoric acid (HDEHP) to separations of these elements for their subsequent quantitative determination.
The rare earth elements in NBS Standard Reference Material 480, Trace Elements in Glass, a sodium glass to which 61 trace
elements, including the thirteen naturally occurring rare earths, were added, have been determined by neutron activation analysis
with a chemical separation using a column (11 cm×40 cm) of “Corvic” powder [poly(vinyl chloride-vinyl acetate)] loaded with
HDEHP and operated at a constant temperature. Since our earlier solvent extraction studies with HDEHP had shown perchloric
acid to be the most favorable of three acids (HCl, HNO3, HClO4) for rare earth separation, we established the best operating conditions (e. g. time, flow, acid concentration, etc.) using
this acid. A detailed description of the separations procedure and the quantitative results will be discussed.
The elements As, Cd, Cu, Hg, Mo, Sb, and Se were determined in the biological reference materials (RMs) Bowen's Kale, NIST SRM-1577 Bovine Liver, NIST SRM-1549 Milk Powder, and Versieck's 2nd Generation Biological RM Human Serum using two newly developed radiochemical neutron activation analysis (RNAA) procedures. The first is based on sample decomposition in a mixutre of H2SO4+HNO3+H2O2 and simultaneous extraction of the elements As, Cd–In, Cu, Mo, and Sb by 0.025M Zn(DDC)2 in chloroform from 2–4M H2SO4 in the presence of 0.01M KI. The second consists of sample decomposition in HNO3 in teflon bombs heated at 150°C, Hg extraction by 0.01M Ni(DDC)2 in chloroform from about 1M HNO3, and Se precipitation by ascorbic acid from about 1M HClO4. The RNAA procedures were also used for intercomparison analyses of A and P NIST Leaf Materials (NIST candidate SRM-1515 Apple Leaves and NIST SRM-1547 Peach Leaves, respectively), and CZIM Bovine Liver 12-02-01 RM. Very good agreement of results with certified and/or literature values proved the high accuracy of these determinations by the proposed RNAA procedures, even at the sub-ng/g levels.
An edited transcript of the plenary discussion is given on the subject of “Representative Sampling and the Proper Use of Reference
Materials” which was held at the International Conference: Modern Trends in Activation Analysis on September, 15, 1976 in
Munich, Federal Republic of Germany.
A new assembly dedicated for the low-level ψ-ray spectrometric measurements of environmental samples have been installed recently
at the International Atomic Energy Agency's Laboratories, Seibersdorf. Calibration of the detection efficiency was performed
by a set of 14 IAEA Certified Reference Materials, a standardized solution of134Cs, solutions of 2 pure potassium salts, and 2 mixed radionuclide gamma reference standard solutions. These materials, in
1.3 liter Marinelli beakers, were measured by a large HPGe detector. The high precision and accuracy of the calibration procedure
is shown by the high significance achieved in the linear fits of the efficiency results, which are traceable to certified
and standard reference materials. Small biases between some calibrands were detected. A new corrected result is the 1.37±0.05
Bq/kg activity concentration of137Cs in IAEA-A-14 Milk Powder.
Authors:T. Miura, H. Matsue, T. Kuroiwa, and K. Chiba
Prompt gamma activation analysis using a focused thermal neutron guided beam at JAEA JRR-3M was applied to the determination
of B in ceramic certified reference materials (BAM CRM S-003 Silicon Carbide Powder and NMIJ CRM 8004-a Silicon Nitride Powder).
Cl and Si were used as internal standards to obtain linear calibration curves of B. The analytical result of B in BAM CRM
S-003 was in good agreement with the certified value. The relative expanded measurement uncertainties (k = 2) were 4.8% for BAM CRM S-003 and 4.9% for NMIJ CRM 8004-a.
Authors:A. Kimura, Y. Toh, M. Oshima, and Y. Hatsukawa
Recycling steel products demands a new technique for determining tramp elements in steel. Tramp elements, As and Sb, in some
iron certified reference materials were determined by neutron activation analysis with multiple gamma-ray detection method
and reported in MTAA11. In MTAA12, the authors reported the lower limit of determination values (LDL) and the dispersion of
this method. The values of the LDLs for As and Sb in high purity iron were 0.002 and 0.0009 μg·g−1. The dispersion is small enough to satisfy the demand from materials science.
The NIST program for environmental Standard Reference Materials (SRM) includes materials covering a range of matrices, mass
fraction values and analytes. For many SRMs, mass fraction data are accumulated, incidentally, over time, as these are used
routinely for quality assurance purposes. Although these are not formal stability studies, data generated may be useful in
assessing stability. To evaluate the potential for assessing material stability from incidental use of SRMs, results of neutron
activation analysis performed from 1992 through 2008 were compiled for SRM 1547 Peach Leaves and SRM 1566a Oyster Tissue.
Results indicate that incidental use of SRMs yields useful information on SRM stability.
Authors:N. Chutke, M. Ambulkar, R. Weginwar, and A. Garg
A radiochemical solvent extraction procedure has been developed for the determination of As(III) using76As tracer. It is based on the complexation of As(III) with toluene-3,4-dithiol (TDT) at pH 2 and subsequent extraction in benzene. The effect of various parameters such as pH, time of equilibration, nature of solvent, quantitative character and interferences have been studied. The method has been further developed into substoichiometric isotope dilution analysis for the determination of As at < 1 g level and employed for the analysis of several environmental and biological standard Reference Materials from NIST (USA), IAEA (Vienna) and NIES (Japan).
A Synthetic Reference Material (SyRM) composed with accurately known amounts of 12 elements has been prepared. The elemental composition of the SyRM is closely similar to that of marine macro-algac sample. The elemental composition of the SyRM was regulated by the starting materials used for the synthesis. The SyRM was used as a comparative standard for non-destructive alpha-particle activation analysis of marine macro-alga samples. P, Cl, K and Ca were determined simultaneously without correction for alpha range due to difference in the elemental composition between the analytical samples and the comparative standard.