Authors:Katarzyna Drozdzewska, V. Kestens, A. Held, G. Roebben, and T. Linsinger
The application of differential scanning calorimetry (DSC) for purity determination is well documented in literature and is
used amongst others in the analysis of pure organic crystalline compounds. The aim of this work is to examine whether the
DSC method for purity determination consistently produces values for the purity of polycyclic aromatic hydrocarbons (PAHs)
which are sufficiently accurate as required for the certification of reference materials. For this purpose, 34 different existing
PAH certified reference materials were tested. The DSC results are shown to be consistent with the results obtained by other
methods assessing the organic impurities content in PAHs, like gas chromatography (GC), high performance liquid chromatography
(HPLC) and mass spectrometry. Significant differences between the measured values and the certified purity values were observed
only in a limited number of cases.
An analytical procedure was developed to determine the concentration of some elements regarded as trace impurities in nuclear fuel using inductively coupled plasma mass spectrometry (ICPMS) associated to the matrix matching method. The assessment of this approach was carried out using a set of certified reference materials produced by the New Brunswick Laboratory (NBL). Eighteen out of the twenty-four elements in the reference materials could be easily determined. It was found that the mean values for reproducibility and accuracy were 5.0% and 15.0%. The remaining six elements provided mean values of 11.0% and 37.0%, respectively. They could not be adequately determined due to the effects of analyte signal suppression and spectral interference.
Authors:Z. Varga, G. Surányi, N. Vajda, and Z. Stefánka
A rapid and simple sample preparation method for plutonium determination in environmental samples by inductively coupled plasma
sector field mass spectrometry (ICP-SFMS) and alpha-spectrometry is described. The developed procedure involves a selective
CaF2 co-precipitation for preconcentration followed by extraction chromatographic separation. The proposed method effectively
eliminates the possible interferences in mass spectrometric analysis and also removes interfering radionuclides that may disturb
alpha-spectrometric measurement. For 239Pu, 240Pu and 241Pu limits of detection of 9.0 fg·g−1 (0.021 mBq), 1.7 fg·g−1 (0.014 mBq) and 3.1 fg·g−1 (11.9 mBq) were achieved by ICP-SFMS, respectively, and 0.02 mBq by alpha-spectrometry. Results of certified reference materials
agreed well with the recommended values.
Simple and rapid
analytical procedures for the AAS (Atomic Absorption Spectrometry)
determination of Zn, Cd, Ni, Mo and Pb in biological, geological and soil
samples are described. Special attention was paid to sample preparation,
which is the step, most vulnerable to contaminants. Optimal conditions are
presented for the wet digestion of plant matrices, products and waste for the
coal treatment and soil matrices with different acids including: nitric,
perchloric, hydrochloric, hydrofluoric, sulfuric and hydrogen peroxide along
with optimal temperature programmes for subsequent electrothermal (ET)-AAS and
flame (F)-AAS determination of Zn, Cd, Ni, Mo and Pb. Results of the analysis
of all samples are discussed. The proposed method allows obviating the organic matrix (soil and plant)
destruction stage, shortening the analyte dissolution time, reducing cost, and
minimizing hazards of loss and contamination. The validity and versatility of the methods developed were verified by
the analysis of certified reference materials.
Authors:M. Oladipo, J. Lori, J. Bonire, and O. Ajayi
Instrumental neutron activation analysis (INAA) technique has been employed viak0 approximation method to determine elemental composition of five shaving powders commonly marketed in Nigeria. Fe displayed the highest concentrations in the range 1000–2000 g·g–1. Na and Zn concentrations were established in the range 200–400 g·g–1. Heavy elements like Ga, La, Cr, Co, Ag, Ce and Nd concentrations were noted in the lower range of 1–10 g·g–1 Br, As, Sb, Sm, Eu, W, Cs, Tb, Yb, Hf, Ta, Th and U concentrations were established in even lower traces in the <1 g·g–1 range. Results obtained for a certified reference material, CANMET BL-1 and CERT (in house) Kaolin standard compared favourably with the literature values thus establishing the results presented for the shaving powders.
Authors:S. Sahoo, H. Yonehara, K. Kurotaki, K. Shiraishi, V. Ramzaev, and A. Barkovski
The present paper describes the inductively coupled plasma mass spectrometric (ICP-MS) determination of rare earth elements (REEs), thorium and uranium in forest, pasture, field and kitchen garden soils from a Russian territory and in certified reference materials (JLK-1, JSD-2 and BCR-1). In addition to concentration data, strontium isotopic composition of the soil samples were measured by thermal ionization mass spectrometry. The measurements contributed to the understanding of the background levels of these elements in an area contaminated due to Chernobyl accident. There was not a significant variation in the concentration of REEs at different depth levels in forest soil samples, however, the ratio of Th/U varied from 3.32 to 3.60. Though concentration of U and Th varied to some extent, the ratio did not show much variation. The value of 87Sr/86Sr ratio, was in the top layer soil sample relatively higher than in the lower layers.
Authors:M. Carmo Freitas, L. Moens, P. De Paepe, and J. Seabra E Barros
A 7 kg stone of a Carrara marble was reduced to grains smaller than 100 m, mixed and homogeneized in order to prepare a marble reference material. The homogeneity was tested for 16 elements by instrumental neutron activation analysis (INAA). Through a one-way analysis of variance based on several analyses of each of 15 bottles and within the same bottle, it was concluded that the inter-bottle heterogeneity is not greater than the intra-bottle heterogeneity. Results on the concentration of major and trace elements in the marble reference material, obtained by different laboratories and different techniques, are given. The limestone certified reference material KALKSTEIN KH was used to evaluate measurement accuracy, to intercalibrate laboratories, and to provide compatibility of measurement data.
The assessment of environmental pollution of the coastal areas of the Malaysian Peninsula was done by analyzing the contents of the heavy and trace elements in the bivalves blood clams (Anadara granosa) and green mussels (Perna viridis) and sediments at twenty-two sampling stations to look for prevailing trends. Heavy and trace elements analyzed in this study were As, Cd, Cr, Cu, Pb, Se and Zn. Two techniques, namely the neutron activation analysis (NAA) and atomic absorption spectrophotometry (AAS) were used in the quantitative determination of the heavy metals while Marine Sediment Reference Material (BCSS) and Lobster Hepatopancreas (TORT-1) provided the certified reference materials in the quality assurance control. The potential use of these bivalves as suitable bio-indicators was evaluated from correlation tests based on the concentrations of heavy and trace elements in the sediment-metals system to those in the bivalves.
Authors:Kh. Rezaee, M. Abdi, E. Saion, K. Naghavi, and M. Shafaei
In order to complete having data base of elemental assessment of the east coast of Peninsular Malaysia marine sediments along
the South China Sea coasts, trace elements are analyzed and their distribution in marine sediments is undertaken. The present
study is done parallel with pervious study on elemental assessment of heavy metals, rare earth elements and actinides in the
marine sediments of the east coast of Peninsular Malaysia. Thirty surface sediment samples were collected in this area, including
regions of Kelantan, Terengganu, Pahang, Rompin and Johor Baharu. Multielemental analysis was carried out by instrumental
neutron activation analysis and inductively coupled plasma atomic emission spectroscopy. In both cases methodology validation
was performed by certified reference material analyses. For the surface elemental distributions the enrichment factor values,
average Igeo and mCd values indicate that the trace elements of the surface sediments are uncontaminated in all sampling stations that are consistent
with previous studies results of heavy metals, rare earth elements and actinides.
The accuracy and precision of the results obtained for total mercury in various environmental and biological samples and certified
reference materials (CRMs) by various analytical methods, including k0-instrumental neutron activation analysis (k0-INAA), radiochemical neutron activation analysis (RNAA) and cold vapour atomic absorption (and atomic fluorescence) spectrometry
(CVAAS/AFS) used in routine analysis in our laboratory, were investigated. Three natural matrix reference materials (RMs)
from the International Atomic Energy Agency (IAEA), five CRMs from the Institute for Reference Materials and Measurements
(IRMM), six CRMs from the National Institute of Standards and Technology (NIST) and one from the Jožef Stefan Institute (IJS)
were analyzed. The results obtained show good agreement between certified or assigned values, and between the methods used,
except for some data obtained by k0-INAA in biological samples. This can be explained by losses during irradiation in semi-open systems (irradiation in plastic
ampoules) and/or spectral interferences.