Multielemental Analysis of Agroindustrial By-Products Employed in Animal Feeding by INAA

Instrumental neutron activation analysis (INAA) with gamma-ray spectrometry was applied to determine As, Ca, Cd, Cl, Co, Cu, Cr, Fe, Hg, K, Mg, Mn, Mo, Na, Sb, Se and Zn in the Brazilian agroindustrial by-products. These materials are widely used in ruminant feeding. The results obtained were compared with requirement and maximum tolerable concentrations. The general conclusions from the data obtained were: (1) many by-products presented concentrations of some essential elements lower than the requirement concentrations, while in some concentrations of Cr, Fe, Mg and Se exceeded by a little the maximum tolerable concentrations, (2) the elements As, Cd, Hg and Sb, generally considered toxic, showed concentrations lower than maximum tolerable values.     

Trace element analysis of turkey vulture (Cathartes aura) feathers

Ten feather samples, including primary and secondary flight and tail feathers, were analysed for the trace element composition of vane and rachis structures using instrumental neutron activation analysis (INAA), inductively coupled plasma-mass spectrometry (ICP-MS), and cold vapour atomic absorption spectroscopy (CVAAS). Five environmentally significant elements, Cr, As, Se, Sb and Hg, were analysed by INAA and ICP-MS/CVAAS. A further seventeen elements were analysed by ICP-MS. The majority data obtained by INAA and ICP-MS/CVAAS were not statistically significantly different (p = 0.05), although the removal of isobaric interferences using dynamic reaction cell technology was essential to produce ICP-MS data that were consistent with INAA for Cr, As and Se. Significantly higher trace element concentrations were observed for vane relative to rachis for all elements, except Cu and Hg. These elements displayed vane/rachis ratios of 0.7 ± 0.2 and 1.0 ± 0.2, respectively. In general, vane and rachis subgroups afforded data that were consistent with a normal distribution, with RSDs in the range (12–83) % for INAA analyses. A total of 18 outliers were noted amongst the various feather, structure, element combinations, with 14 outliers being observed in the vane and/or rachis structures of the same tail feather. Given the significant differences in vane and rachis concentrations observed for many elements, the large RSDs reported for elements and the potential for outliers, the determination of environmental trace element burden using feathers is significantly enhanced by the analysis of multiple feathers using INAA.     

Multielement analysis of Chinese Biological Standard Reference Material by monostandard instrumental neutron activation analysis

A procedure for monostandard INAA of 21 elements (Hg, As, Br, Cr, Sb, Se, Ba, Zn, Ca, Ce, Co, Cs, Eu, Fe, Hf, K, La, Rb, Sc, Sr, Ta) in Chinese Biological Standard Reference Material (peach leaves) is described. The accuracy of the procedure was checked by analyzing the U.S. NBS Standard Reference Materials SRM-1571 and SRM-1632a.     

Multi-element determination in earthworms with instrumental neutron activation analysis and inductively coupled plasma mass spectrometry: A comparison

Earthworms were collected from agricultural fields in Admont, Graz, Piber and Gumpenstein, Austria. Six earthworm samples were investigated with INAA and with ICP-MS in parallel for the element concentrations of As, Ba, Cd, Co, Cr, Cu, Fe, Hg, Pb, Rb, Sb, Se and Zn. With both techniques 14 elements were analysed in a wide concentration range (ng/g to mg/g) GF-AAS and HG-AAS were used for verification of some element concentrations. A comparison of analytical results between INAA and ICP-MS was discussed. In general, good agreement between ICP-MS and INAA was obtained, the relative difference values of most of the elements are within ±20% range, however, a methodical error for the determination of Hg by ICP-MS was found.     

Determination of As,Cd, Cr,Cu, Hg,Sb and Se concentrations by radiochemical neutron activation analysis in different Brazilian regional diets

The present paper describes radiochemical separation procedures developed for the determination of seven elements: As, Cd, Cr, Cu, Hg, Sb and Se in different Brazilian regional diets. In the case of the elements As, Hg, Sb and Se, the procedure was based on retention in inorganic exchanger TDO (tin dioxide) and determination of Hg by extraction with Ni(DDC)₂. For determination of Cd, Cr, Cu and Se the procedure chosen was based on retention in inorganic exchanger HMD (hydrated managese dioxide) and extraction of Cu and Cd as diethyldithiocarbamate compounds. The accuracy and precision of the methods studied were tested by means of analyses of different reference materials. Due to the lack of data on trace element levels in Brazilian foodstuffs and diets, these methods were applied to determination of these elements in different Brazilian regional diets. These diets were supplied by the Food and Experimental Nutrition Department of the Faculty of Pharmaceutical Science, University of São Paulo. The daily dietary intake values for these diets are presented for As, Cd, Cr, Cu, Hg, Sb and Se.     

微波消解-ICP-OES法测定汽车涂料中8种重金属

建立微波消解-电感耦合等离子体发射光谱(ICP-OES)测定汽车涂料中Pb,Cr,Se,Ba,Sb,As,Cd,Hg含量的方法。以HNO_3-H_2O_2(体积比为4∶1)混合酸消解样品,各元素分析谱线:Pb 220.353 nm,Cr 267.716 nm,Se196.090 nm,Ba 233.527 nm,Sb 217.581 nm,As 189.042 nm,Cd 228.802 nm,Hg 184.950 nm。8种元素测定结果的相对标准偏差为2.02%~12.94%(n=6);对白色、蓝色、红色汽车漆样品进行加标回收试验,Pb,Cr,Se,Ba,As,Cd,Hg,的加标回收率为81.26%~99.79%,Sb的回收率为62.43%~87.61%。该方法快速、简便,精密度、准确度较高,可用于汽车涂料中重金属含量的监控。     

An innovative Compton suppression spectrometer and its capability of evaluation in multi-elemental neutron activation analysis

A new Compton suppression system was established. A low energy HPGe detector (LO-AX) is used as the analyzing detector. It is completely shielded by a 50%n-type HPGe and two NaI(TI) detectors. Experiments show that a substantial Compton suppression effect is also achieved in the low energy region down to 15 keV. The capability of applying this system in INAA was evaluated for 13 elements (As, Cd, Co, Cr, Hg, Mo, Ni, Sb, Se, Sr, Th, U and Zn) in biological and environmental samples. The benefits and problems of using this Compton suppression spectrometer in INAA are examined for each element.     

Neutron activation analysis of IAEA proposed certified reference material IAEA-407 (North Sea Fish Homogenate)

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.     

Mineral profile of Ghanaian dried tobacco leaves and local snuff: A comparative study

The concentration of thirty-four elements each in Ghanaian dried tobacco leaves and snuff (powdered tobacco) have been determined using instrumental neutron activation analysis (INAA). The concentration of Hg, Cr, As and Cd in both set of samples were found to be in excess of WHO limits for drinking water, thus indicating potential toxicity of the samples. Cr, Cd, Sb and Cu were two to eight times high, whilst As and Hg were comparable in powdered tobacco and tobacco leaves. The aim of the study was to determine the pattern of elemental concentrations and the toxicological strengths in both tobacco leaves and tobacco powder. The results indicated that the toxicity of the snuff was higher than the tobacco. This indicated strongly that from the medical point of view, the level of toxic accumulation in users might be potentially high in the tobacco powder compared to the leaves. Thus, education of the Ghanaian public on the threshold value of toxic elements contained in both set of samples was suggested to safeguard users against these addictives.     

INAA of essential micronutrients in <Emphasis Type="Italic">Terminalia arjuna</Emphasis> bark powder: a versatile heart tonic

Five bark powder samples of Arjuna (Terminalia arjuna) having different origins including two commercial brands were analyzed for 8 minor (Al, Na, K, Mg, Ca, P, Cl, Fe) and 19 trace (As, Ba, Br, Co, Cr, Cs, Cu, Eu, Hg, La, Mn, Rb, Sb, Sc, Sm, Sr, Th, V, Zn) elements by INAA. Also concentrations of Ni, Cd and Pb were determined by AAS and of Sn by ICP-MS. Arjuna bark powder is enriched in Ca (34.1 ± 10.6 mg/g), Mg (5.41 ± 1.93 mg/g), K (5.87 ± 2.18 mg/g), Cl (4.0 ± 2.2 mg/g) and Fe (2.99 ± 1.77 mg/g) with significant amounts of Cr (6.9 ± 4.0 μg/g), Mn (75.5 ± 24.8 μg/g), Sr (114 ± 69 μg/g) and Zn (11.9 ± 8.9 μg/g). Several toxic elements such as As (78.6 ± 19.9 ng/g), Cd (5.60 ± 9.04 μg/g), Hg (69 ± 41 ng/g) and Pb (5.0 ± 3.5 μg/g) were also detected.     

Interlaboratory study of trace and other elements in the iaea powdered human hair reference material,HH-1

A powdered intercomparison material for trace element studies was prepared from human scalp hair and distributed to more than 100 laboratories of which 66 reported results for altogether more than 40 elements. By statistical evaluation of these data certified concentration values were derived for 20 elements, namely As, Au, Br, Ca, Cd, Cl, Co, Cr, Cu, Fe, Hg, Mg, Mn, Na, Pb, S, Sb, Se, Sr and Zn. The data also made it possible to compare different methods of analysis and to judge the value of different levels of experience on the part of the analyst concerned; these comparisons are presented here with special reference to the elements As, Cd, Hg, Pb and Sb.     

Determination of trace elements in food by neutron activation analysis

Neutron activation analysis (NAA) methods have been developed for the determination of major, minor and trace elements in duplicate diets and individual food items. These include a cyclic instrumental NAA (CINAA) method for measuring Se content through its short-lived nuclide^77mSe; epithermal INAA (EINAA) for I and As; conventional INAA for Br, Ca, Cl, Co, Cr, Fe, K, Mg, Mn, Na, Rb, Sb, Sc, Sn and Zn; combination of EINAA and INAA for Al; radiochemical NAA (RNAA) for As, Au, Co, Cu, Fe, Hg, Mo, Sb, Se and Zn; and preconcentration NAA (PNAA) for U and Th. Accuracy of measurements have been evaluated by analyzing a number of biological and diet reference materials. Multielement concentrations of diets and foods have been measured by these methods.     

Neutron activation as a routine method for the determination of trace elements in water

By freeze-drying the following elements can be determined in natural water except sea water: Au, Ba, Br, Ca, Ce, Co, Cr, Eu, Fe, K, La, Mo, Na, Sb, Sc, Se, U, Zn. Some problems may arise with respect to As and Hg. Cu, Cd and Ni can only be determined if present in high concentrations. Separation by adsorption on charcoal in presence of complexing agents gives yields between 75 and 100% for the following elements in sea water: Ag, Au, Cd, Ce, Co, Cr, Eu, Fe, Hg, La, Mo, Sc, Se, U, Zn (As 67%, Sb 56%). Activation or use of labelled ions and study of exchange give information about mobility of trace elements in suspended matter.     

Determination of trace elements in petroleum by neutron activation analysis

Instrumental neutron activation analysis (INAA) and Ge(Li) spectrometry have been used to determine Sc, Cr, Fe, Co, Ni, Zn, As, Se, Sb, Eu, Au, Hg, and U in crude petroleum. The technique involves no chemical separations and no pre-concentration of the samples by ashing is necessary, thus avoiding contamination or loss of volatile elements. The estimated detection limits in ppb for the elements are Sc (0.1), Cr (0.16), Fe (400.0), Co (0.6), Ni (1.1), Zn (200.0), As (6.0), Se (23.0), Sb (1.0), Eu (0.58), Au (0.11), Hg (4.3), U (1.5). Precision values ranged from 0.1% to 15% (relative standard deviation). Interferences in the Co and Fe determinations due to fast neutron reactions (n, p) and (n, α) on Ni isotopes are small and are easily corrected. Losses of As, Se, and Hg due to escape of volatile gases during irradiation are negligible     

Availability of essential trace elements in medicinal herbs used for diabetes mellitus and their possible correlations

Four plant parts (leaves, roots, fruits and seeds) of twenty samples of sixteen antidiabetic herbs including three commercially marketed capsules have been analyzed for 6 minor (Na, K, Ca, Cl, Mg, and P) and 21 trace (As, Ba, Br, Ce, Co, Cr, Cs, Cu, Eu, Fe, Hg, La, Mn, Rb, Sb, Sc, Se, Sm, Th, V and Zn) elements by instrumental neutron activation analysis (INAA). Further, Ni, Cd and Pb contents were determined by AAS. Elemental data were validated by simultaneously analyzing reference material (RM), MPH-2 Mixed Polish Herbs. Several elements such as Cr and V (1–2 μg/g), Rb (10–40 μg/g), Cs (80–300 ng/g), Se (∼100 ng/g) and Zn (25–60 μg/g) play an important role in diabetes mellitus. Interelemental linear correlations have been observed for Cu vs. Zn (r = 0.89) and Rb vs. Cs (r = 0.87). K/P ratio varies in a narrow range with a mean value of 6.2 ± 1.4. Toxic elements As and Hg were found in <1 μg/g whereas Cd and Pb were in ∼5 μg/g and <10 μg/g, respectively.     

A study of trace element distribution in the solvent refined coal (SRC) process using neutron activation analysis

Twenty-two trace elements have been measured by INAA in materials produced in the Solvent Refined Coal (SRC) pilot plant. The elements As, Sb, Se, Hg, Ni, Br, Na, K, Cr, Sc, Fe, Co, Cs, Ce, Rb, Th, Sr, Ba, Tb, Eu, Sm and Lu were measured in coal, SRC, insoluble residues, solvents, and process waters. The liquefaction process produces a fuel lower in toxic trace elements than the parent coal. Elemental balances indicate that except for As, and Hg the SRC and insoluble residues contain more than 80% of the trace elements found in the coal. Evidence is presented indicating significant organic binding of As, Se, Hg, Br, Ni, and Co in the SRC.     

Distribution of some major and trace elements in Danube Delta lacustrine sediments and soil

Sediment cores collected from lakes Mesteru and Furtuna (eastern part), Sontea channel and soil samples collected from Caraorman bar, all located in the Danube Delta, were analyzed for 42 elements (Ag, Al, As, Be, Na, Mg, P, S, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Br, Rb, Sr, Y, Mo, Ag, Cd, In, Sn, Sb, Cs, Ce, Hf, Hg, Tl. Pb, Bi, Th. U) by instrumental neutron activation analysis (INAA), thick target proton induced X-ray emission (TT-PIXE) and inductively coupled plasma-mass spectrometry (ICP-MS). The INAA and TTPIXE yielded total concentrations whereas the ICP-MS data reflected the fractions soluble in 14M HNO₃. The ICP-MS data exhibited surface enrichment relative to the lower part of the sediment core of Cu, Zn, As, Ag, Cd, In, Sn, Sb, Hg, Tl, Pb, and Bi, most prominently by Cd and Hg. Their vertical distribution in the investigated cores generally reflected the pollution history of recent sediments in Danube delta, showing a steady increase until the end of the 1980s followed by a slow decrease after 1990. The vertical profiles of most remaining elements were characterized by a relatively uniform distribution along the cores. In some cases, the concentrations of As, Cd, Cu, Cr, Mn, Ni and Pb exceeded minimum thresholds of safety, as defined by the Romanian regulations. The elemental composition of the sediment below 20 cm depth (total concentrations) was similar to that of the upper continental crust (UCC) for most elements. Values distinctly higher than UCC were observed for As, Sb (factor ~5) and Cr, Ni, Cu (factor 2 to 3). The nitric acid soluble element concentrations in the soil samples in some cases showed increased values at the surface as compared to 30 cm depth, either due to air pollution or to the action of plants. In no case a large contribution to the topsoil from atmospheric deposition was evident, indicating that the surface contamination of the sediments was mainly by riverine transport. This revised version was published online in July 2006 with corrections to the Cover Date.     

Determination of elemental levels in radiopharmaceuticals by instrumental neutron activation analysis

Instrumental neutron activation analysis (INAA) was applied to thedetermination of the concentration levels of Na, Mg, Al, Cl, K, Sc, Ti, V,Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Br, Rb, Sr, Zr, Mo, Ag, Cd, Sb, I, Cs,Ba, La, Ce, Nd, Sm, Eu, Tb, Dy, Yb, Lu, Hf, Ta, Hg, Th and U in three radiopharmaceuticals.The irradiation of the samples was carried out in a 0.5 kW Bariloche RA-6Research Nuclear Reactor and the induced gamma-activity was measured by gamma-spectrometry.INAA proves to be an accurate and precise technique to obtain a quick informationon the concentration levels of several minor and trace components in radiopharmaceuticals.The quantification of heavy toxic elements is required for the registrationof radiopharmaceuticals.     

Preparation of the Bovine Kidney and Bovine Muscle reference materials and the certification of element contents from interlaboratory comparisons

Results obtained in interlaboratory comparisons on candidate reference materials Bovine Kidney and Bovine Muscle, in which more than 32 laboratories participated employing atomic spectrometry, electrochemical, and nuclear analytical techniques, have been evaluated using combined statistical and analytical considerations. Certified and/or information values for the elements Br, Ca, Cd, Co, Cr, Cu, Fe, Hg, K, Mg, Mn, Mo, Na, P, Pb, Rb, Se, and Zn have been established. Information on contents of the elements Al, As, Au, Cs, Li, Ni, Sb, Sn, Sr, and V is also presented.     

Challenges and successes in the use of neutron activation analysis procedures for value assignment of animal serum and bovine liver Standard Reference Materials

Analyses for value assignment in the renewal Standard Reference Materials^® SRM 1598a Animal Serum and SRM 1577c Bovine Liver included extensive characterization by neutron activation analysis (NAA). Conventional instrumental NAA procedures were complemented by pre-irradiation chemical separations for the determination of Al, V, Mn, and Cu, radiochemical separations for the determination of Ag, As, Cd, Cr, Cu, Mo, Sb, and Se, and the use of (anti-) coincidence gamma-ray spectrometry systems for the instrumental determination of Ag, Cr, and Hg. The previous materials, SRMs 1598, 1577, and 1577b, were analyzed together with the new materials for quality control.