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.     

Analysis of FDA in-house food reference materials with anticoincidence INAA

In-house reference material (IRM) cocoa powder (CCP) has been in use at US Food and Drug Administration laboratories for about 15 years. A single lot of commercial material was originally characterized for 32 elements by several laboratories and five techniques. A unique approach for basis weight determination based upon ambient relative humidity was developed for CCP, eliminating the need for dry weight determinations. The CCP Reference Sheet is updated by incorporating new results approximately every 5 years. The last update occurred in 2006. As part of an effort to revalidate and update values for CCP, anticoincidence instrumental neutron activation analysis (INAA) was used to determine mass fractions for 16 of the originally characterized elements, as well as to provide information on 16 other elements. Results were in very good agreement with 2006 Reference Sheet values. A new candidate IRM, fresh-frozen swordfish (FFSF) powder, was produced by adding inorganic As, Cd, Cr, Hg, Pb, Sb, and Se to liquid nitrogen-frozen commercial swordfish filets which were then homogenized. Portions of FFSF were analyzed by INAA to provide mass fraction and homogeneity information for As, Cd, Cr, Hg, Sb, and Se as well as for eight other elements occurring naturally in the material. Non-homogeneities were ≤2.5 % for As, Br, Cd, and Cs, and ≤1.8 % for Cr, Hg, Rb, Sb, and Se. Certified reference materials DORM-3 Fish Protein powder and fresh-frozen SRM 1947 Lake Michigan Fish Tissue were analyzed as controls.     

The distribution of trace elements in normal human liver determined by semi-automated radiochemical neutron activation analysis

The eight segments of five normal human livers are analysed for 25 trace elements by radiochemical NAA. This consits of an automated wet destruction of the samples and two distillations, followed by ion exchange procedures. Ru is used as triple-comparator for the standardisation. Short-lived and matrix-isotopes are standardised by the Bowen's kale powder. The results reveal that the coefficient of variation within the liver is smaller than 10% for the elements Cd, Cl, Cs, Cu, Fe, K, Mg, Mn, Rb, Se and Zn. The highest range observed for the elements As, Br, Co, Cr, Hg, La, Mo, Na and Sb within a liver is smaller than the range observed between the five livers.     

Elemental analysis of some herbal plants used in the treatment of cardiovascular diseases by NAA and AAS

Elemental analysis of some herbal plants used in the ayurveda for curing of cardiovascular diseases has been performed using the techniques of neutron activation analysis and atomic absorption spectroscopy. The concentration of elements Mn, Na, K and Cl has been estimated by NAA using a²⁵²Cf neutron source and a high purity gemanium detector coupled to a multichannel analyzer, while the elements Ca, Cr, Co, Cu, Fe, Pb, Zn, Ni, Cd and Hg were analysed by AAS using a Perkin Elmer 3100 instrument.     

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.     

Distribution of some elements in human hair and internal organs,determined by neutron activation analysis

Twenty four male autopsies were obtained from Shanghai, China. The samples of liver, lung, kidney cortex, brain and scalp hair were collected from the autopsies. The elements As, Br, Ca, Cd, Cl, Co, Cr, Cu, Fe, Hg, Mg, Mn, Na, Rb, S, Se and Zn were determined by neutron activation analysis (NAA). The present study shows the distribution of the elements in different tissues and provides the element level for normal persons in the local area. In general, the results are comparable with those of other countries.     

前列舒通胶囊中26种无机元素的分析

目的：明确造成前列舒通胶囊不同批次间差异的标志性无机元素,并进行安全性评价。方法：采用ICP-MS测定制剂中Al、As、B、Ba、Ca、Cd、Co、Cr、Cu、Fe、K、Mg、Mn、Mo、Na、Ni、Pb、Sb、Se、Sn、Sr、Ti、Tl、V、Zn和Hg元素含量并进行数据分析。运用主成分及综合评分结合聚类分析手段,确定制剂的特征性元素;进行元素含量和相关性分析,明确不同批次各元素的差异及元素之间的关系;以多元素含量为指标,绘制无机元素谱图。结果：19批样品中均未检测出Se、Mo、Sn、Sb、Tl和Hg,且Pb、Cd、As、Cu、Hg均符合限量标准,无机元素含量谱图趋势一致。主成分分析提取了4个主成分,确定元素B、K、Al、V、Cr、Ca、Ti、Na、Co和Mn可作为特征元素。主成分得分图将19批样品分为两类,聚类分析及综合评分结果与其一致,两类样品中各元素含量存在差异性。相关性分析中,明确了B与K、Al、Cr正相关,K与Cr、Co正相关,V与Cr、Mn正相关,Mn与Co正相关,Ca、Ti、Na两两正相关。结论：通过分析前列舒通胶囊中无机元素含量,确定了特征元素,为前列舒通胶囊质量全面控制研究提供科学依据。     

Indication of environmental pollution by means of INAA of the hair of some free living mammals

Hair samples collected from free living mammals common hare (Lepus europaeus Pall.), common vole (Microtus arvallis Pall.) and wood mouse (Apodemus sylvaticus L.) have been subjected to instrumental neutron activation analysis (INAA). up to 18 elements As, Au, Br, Ce, Co, Cr, Cu, Fe, Hg, K, La, Na, Sb, Sc, Se, Sm, Th and Zn have been determined in each hair sample. Animal hair samples from areas polluted by thermal power plants burning coal were taken and compared with hair samples from the animals living in relatively non-polluted control areas. The results show that animal hair samples from areas with higher level of pollution contain usually higher concentrations of toxic and essential elements as As, Co, Cr, Fe and Se. Muride rodents can be used for more detailed monitoring of environmental exposure than hare. Moreover, hair of common vole shows usually higher levels of contamination as compared with wood mouse, which could be explained by different compositions of feed. Animal hair has been shown to be a rather sensitive indicator of environmental exposure and INAA has proved to be a suitable analytical tool for this purpose.     

The certification of the contents of Cd, Co, Cu, Fe, Hg, Ni, Pb, Zn, Sb, Se, Tl and Cr in a city waste incineration ash

Summary The analysis of ashes being of increasing importance, a reference material was prepared from fly ash of a city waste incinerator. The procedures of preparation, homogeneity and stability testing are described as well as the way of certification of elements of major importance: Cd, Co, Cr, Cu, Fe, Hg, Ni, Pb, Zn, Sb, Se and Tl.

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Zertifizierung der Gehalte an Cd, Co, Cu, Fe, Hg, Ni, Pb, Zn, Sb, Se, Tl und Cr in einer Stadtmüll-Verbrennungsasche

Zusammenfassung Da die Analyse von Aschen zunehmend an Bedeutung gewinnt, wurde von der Flugasche einer Stadtmüll-Verbrennungsanlage ein Referenzmaterial hergestellt. Die Methoden der Herstellung sowie der Homogenitätsund Stabilitätsprüfung werden beschrieben und die Art der Zertifizierung der Elemente von hauptsächlicher Bedeutung aufgezeigt (Cd, Co, Cr, Cu, Fe, Hg, Ni, Pb, Zn, Sb, Se, Tl).

     

Multielement neutron activation analysis of biological materials using chemical group separation and Ge(Li) gamma spectrometry

Neutron activation analysis (NAA) for the determination of some trace elements in biological materials is described. The method presented permits the simple and rapid determination of Se, Ag, Au, Sb, Pt (via¹⁹⁹Au), Hg, Co, Ni (via⁵⁸Co), Fe, Zn, Mo, Sn, Cr, Cd, Cu and As after radiochemical separation from Na, K, Cs, Rb and partially Br. For this purpose, postirradiation separation by extraction with mercury or zinc amalgam was used. Separation of gold by extraction with ethyl acetate or by precipitation with dimethylglyoxime was applied for the determination of gold and platinum in biological materials.     

Neutron activation analysis of biological materials by the monostandard method

Instrumental neutron activation analysis by the monostandard method has been applied to the analyses of biological NBS standard reference materials; 1571 Orchard Leaves and 1577 Bovine Liver. Aluminum foils containing 0.100% gold or 2.00% cobalt were used as the monostandards. The gamma-ray spectral data were recorded on punched paper tape and were analyzed by a computer assisted data processing. The following 25 elements were determined: Al, Ca, Cl Cu, Mg, Mn, V (by short period irradiation), As, Ba, Br, Co, Cr, Cs, Eu, Fe, Hg, K, La, Na, Rb, Sb, Sc, Se, Sm and Zn (by long period irradiation). The results were compared with the certified values by NBS and the reported values in literatures to prove the reliability and accuracy of the monostandard method.     

Comparative PGAA and NAA results of geological samples and standards

Concentrations of major and trace elements in volcanic rock and soil samples, including geological standard reference materials, were determined by neutron activation analysis (NAA) and prompt gamma activation analysis (PGAA), both using the k ₀-standardization method. The paper highlights the different experimental procedures, such as sample preparation, data collection and spectrum evaluation. In geological samples, PGAA gives precise results for major elements (Si, Ti, Al, Fe, Mn, Mg, Ca, Na, K and—as a unique method—for H), for some of the light trace elements as B and Cl, as well as for Sc, S, Cr, Co, Ni, Cd, Nd, Sm and Gd. NAA is sensitive for the rare earth elements, and for many major (Ti, Al, Fe, Mn, Mg, Ca, Na, K) and trace elements (e.g.: Sc, V, Cr, Co, Ni, Cu, Zn, As, Se, Rb, Sr, Zr, As, Sb, Ce, Ba, Hf, Ta, W). For most major elements the results obtained by the two methods show good agreement. The comparison of the results obtained for trace elements is not always possible, since PGAA is less sensitive and concentrations are often below its detection limits. Nevertheless, the complementarity of NAA and PGAA allows nearly panoramic analysis of geological materials.     

Accumulation and distribution of elements in rice /seed,brand layer,husk/ by neutron activation analysis

Various rice samples /seed, brand layer, husk/ from Vietnam were analyzed for Se, Hg, Cr, Ni, Sc, Rb, Fe, Zn and Co by neutron activation analysis. The concentration values found /seed/ were the following: Se 0.04–0.07 ppm, Hg 0.02–0.07 ppm, Cr 2.13–8.65 ppm, Ni 1.56–4.95 ppm, Sc 0.02–0.06 ppm, Rb 0.84–2.71 ppm, Fe 26.31–96.07 ppm, Zn 10.65–27.39 ppm and Co 0.02–0.15 ppm. The values were reported in ppm /dry weight/. Statistical analysis /t-test, t=0.05/ showed that the content of elements varies between sorts of rice; the content of Rb, Fe, Ni, Cr of rice husk was significantly higher than in rice seed and brand layer.     

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     

Preparation of the bovine liver 12-02-01 reference material and the certification of element contents from an interlaboratory comparison

Summary The preparation of the bovine liver 12-02-01 reference material, its stabilization and homogeneity testing is presented. Evaluation of an interlaboratory comparison in which 31 laboratories took part using several analytical methods is described. From the results of the intercomparison, the contents of the elements Cd, Cu, Hg, Mn, Pb, Se, and Zn were certified, while for the elements Br, Co, Fe, K, Mo, Na, and Rb, information values were derived. Non-recommended values for the elements Ag, As, Ca, Cl, Cr, Cs, La, Mg, S, Sb, Sn, Sr, and V were also evaluated.Denoted as CZIM-liver in the report [23]     

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.     

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 Hg,Co, Cr,Zn and Fe in various plant leaves using neutron-activation analysis

Neutron-activation analysis /NAA/ was used for the estimation of Hg, Co, Cr, Zn and Fe in leaves of various plants namelySapindus mukorossis, Alstonia scholaris andDiospyros embryopteris located in urban areas of Punjab, Pakistan. Different varities of tissues were found to have different concentration of trace elements when compared among themselves. Significant pollution has been observed.     

Development and certification of the new SRM 695 trace elements in multi-nutrient fertilizer

During the past seven years, several states within the US have enacted regulations that limit the amounts of selected non-nutritive elements in fertilizers. Internationally, several countries, including Japan, China, and Australia, and the European Union also limit the amount of selected elements in fertilizers. The elements of interest include As, Cd, Co, Cr, Cu, Hg, Mo, Ni, Pb, Se, and Zn. Fertilizer manufacturers and state regulatory authorities, faced with meeting and verifying these limits, need to develop analytical methods for determination of the elements of concern and to validate results obtained using these methods. Until now, there were no certified reference materials available with certified mass fraction values for all elements of interest in a blended, multi-nutrient fertilizer matrix. A new standard reference material (SRM) 695 trace elements in multi-nutrient fertilizer, has been developed to help meet these needs. SRM 695 has recently been issued with certified mass fraction values for seventeen elements, reference values for an additional five elements, and information values for two elements. The certificate of analysis includes an addendum listing percentage recovery for eight of these elements, determined using an acid-extraction inductively-coupled plasma optical-emission spectrometry (ICP–OES) method recently developed and tested by members of the Association of American Plant Food Control Officials.     

Some trace elements in the waters,marine organisms and sediments of the Adriatic by neutron activation analysis

A number of investigations of trace elements in the waters, organisms and sediments of the Adriatic, using neutron activation analysis with radiochemical, separations are reported. These include studies of Hg in mussels from the Northern Adriatic, of Hg and Se in edible animals from the Rijeka region, and of seven elements (As, Cd, Cu, Hg, Mn, Se and Zn) in marine invertebrates from the Slovene coast. Additionally, plankton, sediment cores and water samples were taken from a grid of stations covering the whole Adriatic and analyzed for 6 to 11 of the trace elements As, Cd, Co, Cr, Cu, Fe, Hg, Mn, Sb and Zn (Hg only in water). Generally, levels found were not indicative of pollution as compared with oceanic samples, but some evidence of locally increased levels was found, especially for Hg. The levels of eleven trace elements in three marine Intercomparison samples prepared by the IAEA Monaco Laboratory are also presented.