Multielemental determination in some water samples by neutron activation method

A method was developed for the determination of element concentrations in structured water samples (water with high oligoelements content). Sixteen elements (As, Br, Ca, Ce, Co, Cr, Eu, Fe, K, La, Lu, Na, Sb, Sc, Sm, Zn) were determined in 4 structured water samples and one taken from the water tap. The samples were preconcentrated evaporating 1 1 at atmospheric pressure and obtaining 100–500 mg of dry residue. Measurement accuracy by -spectroscopy was 3–30% and it can be improved by increasing the measurement time. The method allows simultaneous multielement analysis of various water sources and may successfully be used in environmental pollution control.     

Synthetic multielement standard samples for serial neutron activation analysis of biological materials

New synthetic standard samples (SSB-1 and SSB-2), produced on the basis of phenol-formaldehyde resin in the shape of tablets are suggested. The samples are intended for INAA of biological materials. SSB-1 and SSB-2 samples contain Se, Cr, Au, Sb, Ag, Rb, Fe, Zn, Co and Ca, Ba, Hg, Sn, Br, Cs, Ni, Sc and Na. The concentrations of these elements are chosen so that the maximum statistical error of -quantum registration by the semiconductor detector should not exceed 3% when irradiating samples in a neutron flux of 10¹³ n·cm^–2·s^–1.     

Element content and element correlations in Chinese human liver

The amounts of the 19 elements As, Br, Ca, Cd, Ce, Co, Cr, Cs, Fe, K, La, Mo, Na, Rb, Sb, Sc, Se, Sm, and Zn in 92 lyophilized autopsy human liver samples from normal subjects have been analyzed by instrumental neutron-activation analysis (INAA). For intercomparison and quality control ten samples were independently analyzed in two institutes, the Institute of High Energy Physics in China and the Joef Stefan Institute in Slovenia. Most of the element contents determined by the two institutes were in quite good agreement, even though different experimental conditions were applied, indicating the reliability of the analytical results. Analysis of the chemical species of mercury present in the ten liver samples was also performed in Slovenia. Possible differences between the element content of male and female liver samples were studied by means of Students t-test, but significant differences were found only for Ce, Co, Fe, La, Mo, and Zn. The results obtained were also compared with those reported from other areas of the world; no appreciable differences were observed. Correlation among the various elements in the human liver samples was studied using multivariate statistics. It was found that there was relatively close correlation between some elements, for example As–Fe, Ca–Fe, Cd–Co, Cd–Zn, Mo–Zn, Co–Se, Cs–Rb, Br–Rb, Sc–Sm, La–Sm, La–Ce, etc.; these correlations could be rationally explained by the similarity of the electronic structures of the elements and/or their physiological functions in the human body.     

Determination of macro and trace elements in canned marine products by inductively coupled plasma—optical emission spectrometry (ICP-OES) and ICP—mass spectrometry (ICP-MS)

This study determined the concentration of eight macroelements (Na, K, Mg, P, S, Ca, Fe, Zn) and nineteen trace elements (Li, Be, Cr, Mn, Co, Ni, V, Cu, Ga, Se, Rb, Sr, In, Sn, Cs, Ba, Tl, Bi, U) in commonly consumed canned marine products from South Korea. The samples were wet-digested using nitric acid and hydrogen peroxide by a microwave system and analyzed for macroelements using inductively coupled plasma—optical emission spectrometry (ICP-OES) and for trace elements by inductively coupled plasma—mass spectrometry (ICP-MS). The analytical methods were validated by the correlation coefficients, limits of detection and quantification, correlation variance, spiking recovery tests, and analyzing a NIST 1566?b oyster tissue certified reference material. The concentrations of macro and trace elements varied among the canned marine products. The macroelements were present in the order of Na?>?K?>?P?>?S> Mg?>?Ca?>?Fe?>?Zn. In general, the concentrations of macro and trace elements were within the specified limits of Food and Nutrition Board, Joint Food and Agriculture Organization/World Health Organization Expert Committee on Food Additives, and Ministry of Food and Drug Safety, Korea. The results suggest that the analyzed canned marine products are safe in terms of the analyzed elements and their consumption therefore does not cause any threat to human health.     

Macro- and micro- elements in some herbal drug raw materials and their water extracts consumed in Poland

The concentrations of seven macro- and microelements (K, Mg, Ca, Na, Fe, Zn, Mn) in 59 herbs (herbs, leaves, flowers, fruits, roots), which are commercially available and frequently used in Poland for medical purposes as well as in their water extracts (infusions and decoctions), were determined after microwave mineralization. The data obtained show that all herbal raw materials analysed contain macroelements in the range of mg g⁻¹ on d.w. whereas microelements in the range of mg kg⁻¹ on d.w. and that elemental concentrations varied widely. On the basis of a comparison of concentrations of elements in herbal raw materials examined and water extracts prepared from them, the extraction efficiency was expressed as a percent of the total content of each element present in the infusion or decoction. The percentages of macro- and micro- elements leaching from different morphological parts of plants into water extracts varied across a wide range of values, from 1% in the case of Na to 56% in the case of K. Real daily intake of the macro- and microelements elements through one cup of infusions or decoctions were shown that water extracts from herbal raw materials are not an important source of bioelements in human diet.      

Assessment of elemental contamination in the bottom sediments from a dam reservoir using a sequential extraction technique and chemometric analysis

The concentration of elements in sediments is an important aspect of the quality of water ecosystems. The element concentrations in bottom sediments from Goczalkowice Reservoir, Poland, were investigated to determine the levels, accumulation and distribution of elements; to understand the contamination and potential toxicity of elements; and to trace the possible source of pollution. Sediments were collected from 8 sampling points. The functional speciation, mobility and bioavailability of elements were evaluated by means of modified Tessier sequential extraction. The element contents were measured by optical emission spectrometry with inductively coupled plasma. The experimental results were analyzed using chemometric methods such as principal component analysis and cluster analysis to elucidate the metal distributions, correlations and associations. The highest concentrations of most elements were found at the center of the reservoir. The distribution of metals in the individual fractions was varied. To assess the extent of anthropogenic impact indices, contamination factor, degree of contamination, metal pollution index and risk assessment code were applied. The calculated factors showed the highest contamination factor and the ability of chromium to be released from sediments. The degree of contamination showed that the area is characterized by a very high contamination. Strontium and manganese showed high potential ecological risk for sediments.      

Radionuclide contents in environmental samples as related to the Chernobyl accident

Many kinds of environmental samples including total diet samples, were collected in the Chernobyl (Ukraine) vicinity and in Ibaraki prefecture (Japan). Six radionuclides and twelve stable elements were analyzed. After samples were dry-ashed, radioactivities of¹³⁷Cs,¹³⁴Cs,⁴⁰K,⁶⁰Co and⁵⁴Mn were determined by -ray spectroscopy with a germanium detector. Strontium-90 was determined by low-background -spectrometry. Stable elements were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). Comparison of the levels of radionuclides between the Ukraine and Ibaraki showed the former were several times to a few tens of thousands of times higher than the latter, depending on the samples.     

Crystal Chemistry of Dichalcogenides MX2

Crystal-chemical analysis of the structures of metal (other than REE) dichalcogenides of composition X:M = 2:1 has been carried out. It is shown that there are two types of structure depending on the formal degree of metal oxidation. The first group are compounds M(X₂) containing metals in the oxidation state 2+ and covalently bonded pairs of chalcogen elements; the main structural types here are cubic (pyrite) and orthorhombic (marcasite) FeS₂. The second group involves the compounds MX₂ with metals in the formal oxidation state 4+ and chalcogenide ions X ₂ ^- ; the main structural types in this group are CdI₂, CdCl₂, MoS₂. The bond lengths M–X, X–X, and X...X are analyzed; it is shown that the high polarizability of the chalcogenide ions is reflected in shortened X...X distances. In the covalently bonded pairs X–X, the bond lengths change within the following limits: 2.03-2.30, 2.35-2.55, and 2.70-2.83 for X...X ion contacts, the minimal values are 3.07, 3.10, and 3.20 (X = S, Se, and Te, respectively).     

Determination of particle-bound trace metals in high purity hydrogen chloride

Summary Two analytical procedures for the determination of particle-bound trace metals in high purity hydrogen chloride are described. Polycarbonate membrane filters with a pore diameter of 0.05 m were used for sampling. Membrane filtration with subsequent instrumental neutron activation analysis (using irradiation with a thermal neutron flux of 10¹³ n cm^–2 s^–1 and irradiation and measurement times of either 20 min) has made it possible to determine the elements Br, Mg, Mn, Na, Sb, Sn, Te, Ti and Zn. For a gas sample volume of 500 l the detection limits determined are in the range of 0.86 ng l^–1 for Zn to 0.30 pg l^–1 for Mn.The elements Cr, Cu, Fe, Mn and Ni were determined by membrane filtration with subsequent graphite tube furnace atomic absorption spectrometry. In this case the detection limits achieved are (for a gas sample volume of 500 l and 4 ml digestion solution) between 8.4 pg l^–1 for Fe and 2.1 pg l^–1 for Cu. The analytical procedures were applied for the characterisation of high purity hydrogen chloride, which is used in the manufacture of highly integrated semiconductor components, by trace analysis, both directly on the gas cylinder and at the 'point of use after passing through the supply system. A review of the status of element determination in high purity process gases is given.

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Bestimmung von partikelgebundenen Metallspuren in hochreinem Chlorwasserstoff

     

Preparation of L-asparagine complex of technetium-99m

Attempts have been made to employ magnesium oxide as the preconcentration agent for determination of trace metal sin seawater by neutron activation analysis. Hydrous magnesium oxide can efficienthy adsorb most cationic transition metals and rare earths in a simple water system. The adsorption behavior is believed to depend mainly from the association of the cationic species of the metals with MgO ₂ ^2– adsorbent. In seawater matrix some of the metal ions such as Hg²⁺, Ni²⁺, etc. may become inefficiently adsorbed owing to the formation of highly stable metal-chloro complexes with chloride ion. Usually the adsorption efficiencies of the metals can be recovered to be as high as the case in the simple water system if an acidified seawater (to pH1) is subjected to the adsorption experiment. In practice, a large volume of seawater (5 1) is stirred with a small amount of hydrous MgO (1 g). Thereafter, the trace metals adsorbed MgO is separated and taken to be neutron activated. The abundant sodium ion and ubiquitous bromide ion can be obviated by the adsorption process, thereby beneficial to the -spectrometry of the metals enriched on MgO.     

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。     

溴与其他卤族元素及卤水溴、氯含量与矿化度的相关关系

研究了地下卤水、土壤、食品和人体组织中Br与其他卤族元素,以及卤水Br、Cl含量与矿化度的相关关系.结果表明,Br与Cl及Br与Ⅰ呈显著正相关关系,其他卤族元素间无显著相关性;Br与矿化度及Cl与矿化度高度相关.利用建立的各类卤水的回归模型,评估了“浓缩均衡矿物滴”(CMD)的盐卤属性.     

ICP-MS Multi-Elemental Analysis of the Human Meninges Collected from Sudden Death Victims in South-Eastern Poland

Metals perform many important physiological functions in the human body. The distribution of elements in different tissues is not uniform. Moreover, some structures can be the site of an accumulation of essential or toxic metals, leading to multi-directional intracellular damage. In the nervous system, these disorders are especially dangerous. Metals dyshomeostasis has been linked to a variety of neurological disorders which end up leading to permanent injuries. The multi-elemental composition of the human brain is still the subject of numerous investigations and debates. In this study, for the first time, the meninges, i.e., the dura mater and the arachnoid, were examined for their elemental composition by means of inductively coupled plasma mass spectrometry (ICP-MS). Tissue samples were collected post mortem from those who died suddenly as a result of suicide (n = 20) or as a result of injuries after an accident (n = 20). The interactions between 51 elements in both groups showed mainly weak positive correlations, which dominated the arachnoid mater compared to the dura mater. The study showed differences in the distribution of some elements within the meninges in the studied groups. The significant differences concerned mainly metals from the lanthanide family (Ln), macroelements (Na, K, Ca, Mg), a few micronutrients (Co), and toxic cadmium (Cd). The performed evaluation of the elemental distribution in the human meninges sheds new light on the trace metals metabolism in the central nervous system, although we do not yet fully understand the role of the human meninges.     

火焰原子吸收光谱法测定四大怀药中10种元素

对四大怀药(即怀山药、怀地黄、怀菊花及怀牛膝)中的8项微量元素(铜、铁、锌、锰、镍、钴、铬和铅)、2种常量元素钾及钙,用火焰原子吸收光谱法做了测定。比较了水煎酸化和硝酸-高氯酸(4+1)混合酸直接消解两种溶样方法,结果表明:用后一种溶样方法可使上述10种元素从药材中更完全地提取。在所述的最优分析条件下,上述10种元素的质量浓度与其相应吸光度在一定范围内呈线性关系。对方法的回收率和精密度做了试验,测得回收率在97.0%～105.0%之间,相对标准偏差(n=5)均小于5%。     

137Cs,trace and toxic elements distribution in Austrian mushrooms

Various mushroom species have been analyzed for their elemental composition (i.e., Al, B, Ba, Ca, Cd, Cr, Cu, Fe, K, Mg, Mn, Na, P, Sr and Zn) by means of ICP-AES. The accuracy of the measurements was confirmed by analyzing a series of the same samples by short time activation analysis. The data were evaluated statistically including the values of¹³⁷Cs. The results denote that the distribution of these elements and their correlation of these elements and their correlation coefficients are highly distinctive for each mushroom species. K, Na and P were found to correlate negatively with¹³⁷Cs in most species. Suillus grevillei and Cantharellus cibarius show high Be values (0.27 and 0.30 g g^–1, respectively), while Pb was high in Suillus grevillei (16.3 g g^–1) and Amanita rubescens (9.3 g g^–1). Higher levels of Cd were found in Rozites caperata and Russula vesca with a mean of 9.2 and 16.1 g g^–1, respectively. Cluster analysis was applied to classify these samples according to their botanical species using their elemental composition. The concentrations of Al, Cr, Mn, Na and¹³⁷Cs have no influence on the classification of these samples.     

TSPIXE analysis of Mg/Ca ratios in ostracode shells

The m-PIXE setup of Fudan University has been used to study the trace elements of ostracode shells. Program TSPIXE was used to calculate their trace element concentrations.Stenocypris derupta Vavra, Dolerocypria mukaishimensis okubo andTanella opima Chen, three kinds of ostracodes were analyzed. In this study, we concentrate on the relationships between molar ratios of Mg/Ca and temperature, and between molar ratios of Mg/Ca and salinity of the host water. We have found that the molar ratios of Mg/Ca of ostracize shells are positively correlated with the temperature of the host water, but negatively correlated with its salinity.     

微波辅助消解-电感耦合等离子体原子发射光谱法(ICP-AES)测定几种血藤中17种元素

建立电感耦合等离子体原子发射光谱法(ICP-AES)测定血藤类中药中K,Ca,Mg,P,Sr,Fe,Mn,Zn,Cu,Co,Cr,Al,Ba,Ni,As,Pb和Cd 17种常量和微量元素含量的分析方法。样品用微波辅助消解,ICP-AES法检测几种血藤中17种元素的含量,方法的检出限为0.000 03~0.009 81μg/mL,加标回收率88.37%~110.00%,相对标准偏差(RSD)均小于5.0%,方法可快速、灵敏、准确测定血藤类中药中多种常量、微量元素的含量。血藤样品中除含有人体必需的常量元素K,Ca,Mg外,还含有Fe,Zn,Mn,Cr,Co等必需的微量元素和其它元素P,Ni,Ba,Al,Sr,Pb,Cd,Ba等。     

Multi-element analysis of environmental samples by cold and thermal guided neutron induced prompt gamma-ray measurement

Non-destructive multi-element determination in environmental samples by neutron-induced prompt -ray analysis (PGA) has been investigated. Comparative standardization for the elements including H, B, C, N, Na, Mg, Al, Si, P, S, Cl, K, Ca, Ti, Mn, Fe, Co, Cd, Sm, Gd, Hg by PGA has been carried out using the cold and thermal guided neutron beams of JRR-3M reactor and then several environmental reference materials have been analyzed. Accuracy and precision of better than 20% were found for these elemental analyses except for H, C, N and Cl in biological samples. Detection limits in various environmental matrices were 25 to 820 ng/g for B, Cd, Sm and Gd, 1.1 to 820 g/g for H, Na, S, Cl, K, Ti, Mn, Co and Hg, and 0.031 to 10% for C, N, Mg, Al, Si, P, Ca and Fe. The present method is being applied to environmental studies of post war Persian Gulf together with INAA and ICP-MS.     

Electronic structure,energy of hydration,and stability of metal aquo ions

The stability of metal aquo ions with respect to redox reactions is determined by the ionization energies of the atoms and the Gibbs energies of hydration for the ions(–_hG⁰). We present critically selected values of –_hG⁰ for 55 metal ions, determined from electrochemical, thermochemical, and spectra data. We consider the factors determining the values of –_hG⁰ (charges, ionic radii, electronic structure, and relativistic effects). For isoelectronic ions, we observe correlations between the ratios of the Gibbs energies of hydration for these ions with different charges and the ratios of their ionic radii. Based on the use of these correlations, we find –_hG⁰ for a number of aquo ions not observed experimentally and we estimate the unknown oxidation-reduction potentials for the pairs of ions M³⁺/M²⁺. We formulate the principles for stabilization of unstable oxidation states of the metals by including the corresponding ions in complexes with certain classes of ligands.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 30, No. 1, pp. 1–11, January–February, 1994.     

Interelement correlations in plants

Summary The concentration of 25 elements in 4 plant species (Citrus aurantia, Brassica oleracea, Lycopersicon esculentum and Pinus strobus) were linearly correlated. For some element pairs (Ce-Fe, Ce-Ni, Ce-Sb, Ce-Sc, Ce-Zn, Fe-Sb, Fe-Sc, Fe-U, Fe-Zn, K-Cd, La-U, Ni-Sb, Sc-U and Sc-Zn) a high positive correlation coefficient (r = +1) was found. The element pairs Ca-Mg, Hg-U, Ni-Sr and Sr-Zn show a significant negative correlation (r = – 1). Plants seem to possess some constant interelement relations, independent of plant species.

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Interelement-Korrelationen in Pflanzen