熔融制样-X射线荧光测定钨钼锡矿中的主次成分

采用熔融制样-X射线荧光光谱法测定矿物中的Cu、Pb、Zn、Mo、W、Al、Fe、Si、K、Na、Ti、Ca、Sn等13种主次量元素,采用混合均匀的三混熔剂,以硝酸锂为氧化剂、溴化锂为脱膜剂,进行实验条件优化选择。在650℃下对样品进行预氧化,在1100℃下高温熔融,熔融时间为300 s,最后制成均匀透明,表面光滑无气孔的熔片,以部分国家一级标准物质和自制的钨钼锡标准样品,熔融制片进行测定,线性拟合建立标准曲线,并通过测定谱线选择、基体校正,使钨钼锡的测定范围扩宽,从微量到主量均能进行测定,并且适用于多种不同矿石的测定。样品的组成和含量变化会对分析线强度造成吸收、增强以及谱线重叠的影响,采用经验系数和理论α系数结合来校正其产生的基体效应。相同条件下熔融10个标准样品进行测定,其相对标准偏差(RSD)均小于5%,表明方法的准确度、精密度均满足国家相关质量标准的要求。选用一些含量不同的标准样品进行测定,最终的测定结果与标准值相符,表明方法可用于钨钼锡矿的测定。     

血清铁、锌、钙、镁、磷与妊娠的关系探讨

为探讨血清铁、锌、钙、镁、磷在孕妇体内的水平，做好围产期孕妇的保健工作，提高孕产妇的健康水平和新生儿健康素质，抽取125例孕中期妇女空腹静脉血，采用透射比浊法测定了其血清铁、锌、钙、镁、磷的含量。结果表明，铁、锌、钙、镁、磷的异常在孕妇中有一定的发生率，其中尤以钙与锌的缺乏最为多见。提示应定期检测孕妇血清铁、锌、钙、镁、磷水平，并采取相府的防治措施．以提高孕产妇及新生儿的健康水平。     

Distribution of trace and minor elements in hungarian spice paprika plants

Detailed investigations were carried out to study the distribution of trace and minor elements in different parts (fruit, seed and rib, peduncle, stem, leaf, root) of ripe Hungarian spice paprika plants. Two varieties of paprika plants were analyzed for their Cl, Co, Fe, K, Mg, Mn, Na, Rb, Sc, V and Zn content by non-destructive neutron activation analysis. The results showed that the iron contents of the samples were much higher than those of the other trace elements. For the trace elements Co, Fe, Mn, Sc, V and Zn a considerable enrichment was observed in the leaf, while the Rb and K, Na, Mg showed accumulation mainly in the peduncle. In the other parts (fruit, seed and rib, stem) of the paprika plants no significant enrichment of trace elements was found. Since some of the elements investigated may have been partially eluted during the cleaning of the roots with distilled water and, on the other hand, if the cleaning was not intensive enough, some soil particles could be retained on the samples, the data obtained for the roots should be considered with precaution.     

Character of the reaction of di- and polynucleotides with some pesticides

Lontrel, Sencor, Roundup, Kusagard, Tachigaren, Tilt, and Sethoxydim, as well as the bidentate Cu, Co, Ni, Mo, and Fe complexes of the herbicide Lontrel form molecular complexes with adenine heterocyclic compounds containing di- and polynucleotides. Sencor forms the strongest complexes, and Tilt has the lowest complexing constant. Lontrel, Sencor, Basagran, and Roundup totally destroy the cooperative character of the double helix of native DNA. The overall effect of the pesticides on nucleotides is determined both by the complexing constant with the purine base and by the capacity of the molecule of the pesticide to reach the reaction side located in the depth of the twisted double helix of DNA and RNA.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 9, pp. 1984–1989, September, 1989.     

电感耦合等离子体发射光谱法(ICP-AES)测定黑豆和红小豆中15种元素

采用ICP—AES法同时测定黑豆和红小豆中Na,Sn,Ca,Zn,Cu,Mg,Al,Fe,P,K,Si,Se,Ba,Mn,M015种元素含量,并对各元素进行了加标回收实验,黑豆和红小豆中各元素的平均回收率在93．11％～102．15％,相对标准偏（RSD）在0．83％0～2．8％,检出限介于0．11～14．09Fg／L。建立了简便、快速、准确和稳定的测定黑豆和红小豆中元素的测定方法。结果显示在黑豆和红小豆中K,Ca,P,Mg,Mn,Fe,Zn等常量元素和微量元素含量较高。红小豆中Ca,Mg,Fe,Zn等营养元素的含量较黑豆中的高。     

Elemental Characterization of Ciders and Other Low-Percentage Alcoholic Beverages Available on the Polish Market

Seventy-three samples of alcoholic beverages and juices that were purchased on the Polish market and home-made were analyzed for their elemental profiles. The levels of 23 metals were determined by ICP-MS (Ag, Ba, Bi, Cd, Co, Cr, Li, Mn, Ni, Pb, Sr and Tl), ICP-OES (Al, B, Ca, Cu, Fe, K, Mg, Na, Ti and Zn) and CVAAS (Hg) techniques in twenty-five samples of ciders widely available on the Polish market; six samples of home-made ciders; two samples of juices used in the production of these ciders; and forty samples of low-percentage, flavored alcoholic beverages based on beer. The gathered analytical data confirmed that the final elemental fingerprint of a product is affected by the elemental fingerprint of the ingredients used (apple variety) as well as the technology and equipment used by the producer, and in the case of commercial ciders, also the impact of type of the packaging used was proven. These factors are specific to each producer and the influence of the mentioned above parameters was revealed as a result of the performed analysis. Additionally, the inclusion of the home-made ciders in the data set helped us to understand the potential origin of some elements, from the raw materials to the final products. The applied statistical tests revealed (Kruskal–Wallis and ANOVA) the existence of statistically significant differences in the concentration of the following metals: Ag, Al, B, Bi, Co, Cr, Cu, Fe, K, Li, Mg, Na, Ni, Ti and Zn in terms of the type of cider origin (commercial and home-made). In turn, for different packaging (can or bottle) within one brand of commercial cider, the existence of statistically significant differences for Cu, Mn and Na was proved. The concentrations of all determined elements in the commercial cider from the Polish market and home-made cider samples can be considered as nontoxic, because the measured levels of elements indicated in the regulations were lower than the allowable limits. Moreover, the obtained results can be treated as preliminary for the potential authentication of products in order to distinguish the home-made (fake) from the authentic products, especially for premium-class alcoholic beverages.     

Determination of impurities in nuclear fuel element components by neutron activation analysis

Neutron activation analysis methods for the determination of impurities in zirconium cladding material and uranium oxide are described. Detection limits for the elements Al, Cd, Cr, Co, Cu, Hf, Fe, Mn, Ni, W and U in zirconium are below that required by the ASTM B 352-79 standard. The method has been tested on the NIST SRM 360a Zircaloy-2 from which the elements Na, Mg, Al, Ca, V, Cr, Fe, Co, Ni, Cu, Eu and U have been detected. The values for Cr, Fe, Ni and Cu are compared with the certified values. A method for the pre-irradiation separation of the elements Mg, Na, Al, K, Sc, Ca, V, Mn, Cr, Fe, Co, Cu, Zn, Rb, Zr, Cd, Cs, REE and Hf from uranium has been developed. A neutron activation analysis method for the determination of those elements in uranium is described. The method is tested by the analysis of the IAEA reference sample SR-54/64. The elements Al, Mn, V, Cu, Cr, Co, Ni and Fe have been detected and the results compared with the certified values.     

Trace element determination in tomato puree using particle induced X-ray emission and Rutherford backscattering

Particle induced X-ray emission (PIXE) and Rutherford backscattering spectrometry (RBS) were used to determine the concentrations of trace elements in samples of 12 tomato puree brands sold in the Mexican market. While RBS offered information about the main elements present in the matrix, PIXE gave results on trace elements. As a whole, data for 17 elements (C, N, O, Na, Mg, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, and Zn) were obtained. To evaluate the results, a comparison with brands from USA, Japan, Colombia, and Chile was carried out, using tomato purees produced following the domestic technology recipe. Additionally, the results were considered in the light of the Codex Alimentarius and the Mexican standard. It was found that all of the brands fall within the limits established by these standards, being of the same order of magnitude as the foreign brands. This revised version was published online in July 2006 with corrections to the Cover Date.     

微波消解－ICP-OES测定钛渣中常量或微量杂质

钛渣样品采取高压密闭微波加热方式以HF、HNO3进行消解,采用电感耦合等离子体原子发射光谱法(ICP-OES)直接同时测定常量、微量杂质铁、铅、砷、铬、铜、磷、锰、钒、镁、钙。考察了消解条件、基体钛以及共存元素之间的干扰影响、等离子体参数等测定条件,通过优选元素分析谱线、以及采用基体匹配与同步背景校正相结合的方式消除光谱干扰和基体效应。测定50、60、70、80、90等不同品位钛渣中杂质元素的结果表明:方法检测范围涵盖了0.005%～10.0%的钙、镁、铁,以及0.005%～2.0%的铅、砷、铬、铜、磷、锰、钒,校准曲线相关系数大于0.999 2;背景等效浓度0.002%～0.0015%,检测限0.0009～0.0038%;含量不小于1.0%的RSD低于0.677%,在0.010%～0.10%含量范围内RSD低于3.85%;回收率为90.0%～108.0%。以本法对70、80、90 3个高钛渣标准样品的定值分析结果与传统化学方法对照一致。     

白族长寿地区硬果仁中19种元素的测定分析

用电感耦合等离子体发射光谱法（ICP－AES）,对云南省白族长寿区的葵花子仁、麻子仁和核桃仁中的Ca、Mg、P、S、Na、AI、B、Fe、Zn、Cu、Mo、Sr、Mn、Cr、Se、Ge、Cd、Pb、As等19种元素进行了测定分析。结果表明,3种硬果仁中含有丰富的人体必需的Ca、Mg、P、S、Na、Fe、Zn、Mn、Se、Cu、Cr、Sr、Mo等有益元素,且P、Mg、S、Ca、Na、Zn、Mn、Fe、Se的含量较高。这些生命元素在3种硬果仁中的含量存在差异。有害元素Cd、Pb均未检出,核桃仁中As含量较高。硬果仁中富含这些生命元素是该地区老人健康长寿的一个重要原因。     

Effect of Cr(VI) anions on adsorption and desorption behavior of Cu(II) in the colloidal systems of two authentic variable charge soils

Heavy metals in wastes exist as multiple pollutants. The study of the interactions between multiple pollutants and soils should be of significance in practice. In the present study, the effect of chromate on adsorption and desorption behavior of Cu(II) in two variable charge soils was investigated, with the emphasis on the adsorption and desorption equilibria of Cu(II). The results showed that chromate can affect adsorption and desorption of Cu(II) in the colloidal systems of two variable charge soils. The extent of the effect was related to the initial concentrations of chromate and Cu(II), the system pH, and the nature of the soils. The presence of chromate led to an increase in the adsorption of Cu(II). For example, in the presence of 0.5, 0.8, 1.0, and 1.5 mmol L(-1) of chromate, for the rhodic ferralsol the adsorption of Cu(II) increased by 15.3, 18.0, 19.0, and 20.2%, respectively. For the hyperrhodic ferrasol, the corresponding figures were 11.9, 17.0, 20.3, and 26.1%, respectively. The presence of chromate also caused an increase in the desorption of Cu(II). For instance, in the presence of 0.5, 1.0, and 1.5 mmol L(-1) of chromate, the desorption for the rhodic ferralsol increased by 16.9, 27.5, and 34.1%, respectively. For the hyperrhodic ferralsol, the corresponding figures were 18.1, 35.6, and 51.4%, respectively. The increments of the adsorption and desorption increased with the increase in equilibrium concentration of Cu(II) in the solution. For instance, when the equilibrium concentrations were 0.5, 1.0, 1.5, and 2.0 mmol L(-1), the increments for the rhodic ferralsol were 2.5, 3.2, 3.3, and 3.0 mmol kg(-1), respectively. For the hyperrhodic ferralsol, the corresponding figures were 2.9, 3.5, 4.0, and 4.2 mmol kg(-1), respectively. The effect of chromate for the hyperrhodic ferralsol was greater than that for the rhodic ferralsol. This is caused by the difference in the content of iron oxides for the two soils. The increments of the adsorption and the desorption of Cu(II) increased with the rise in pH, reaching a maximum value, and then decreased. It can be assumed that the increment of the adsorption was caused by the change in surface charge of the soils induced by the adsorption of chromate and the cooperative adsorption of chromate adsorbed and Cu(II). The increase of electrostatically adsorbed Cu(II) was responsible for the increase in the desorption of Cu(II).     

Egyptian and foreign cigarettes

Neutron activation analysis has been employed to determine the concentration of 27 elements in an Egyptian cigarette filter before and after smoking. The filter of three foreign cigarette brands are also analyzed and compared to the Egyptian brand. The elements determined are Al, As, Ba, Br, Ce, Cl, Co, Cr, Cs, Eu, Fe, Hf, K, La, Mg, Mn, Na, Ni, Rb, Sb, Sc, Se, Sr, Th, Ti, V and Zn. It is observed that the concentration of the measured elements in the Egyptian brand are within the concentration range of foreign brands, and that the concentration of As, Br, Cl, K, Na and Se in the filters are increased after smoking regardless the brand examined.     

Arrangement of ad-atoms of various kinds on substrates: Part II. Iridium and rhodium

The number of iridium sites and that of rhodium sites occupied by a foreign atom was determined with the aid of the pulse technique. In the case of iridium the foreign atoms included are Cu, Ag, Cd, Hg, In, Tl, Pb, Se, Te, As and Bi. The approximate value is 1 for the first two, 2 for the next five and 2.5–2.7 for the others. In the case of rhodium substrate, the foreign atoms included are Cu, Ag, Cd, Hg, In, Tl, Ge, Pb, As, Sb, Se, Te, and Bi. The approximate value is 1 for the first two, 2 for the next six, 2.4–2.6 for the next four and 3.0 for the last one. Silver and copper ad-atoms are closely packed both on the iridium and rhodium surface, but the ad-atoms of the other elements are arranged on the surfaces leaving empty sites for geometrical reasons, even when the monolayer is apparently complete.     

Utilization of instrumental neutron activation analysis (INAA) for geochemical behaviour study of major and trace elements in Bouregreg river basin (Morocco)

The Bouregreg river basin is located in the Moroccan Central Massif which consists mainly of Palaeozoic formations that were subject to the Hercynian orogeny. This study documents the background geochemistry and hydrochemistry of the Bouregreg river basin, focusing on the distribution of major and trace elements. Rock samples were collected at nine locations along the Bouregreg River and its tributaries in the winter of 2005. Major (Al, Fe, Mn, Na, K and Ti) and trace (Rb, Cs, Sr, Sc, Ba, Cr, V, Co, Ni, Zn, As, Sb, La, Ce, Nd, Sm, Tb, Dy, Yb, Lu, Hf, Ta, Mo, Th and U) elements were analysed using instrumental neutron activation analysis. Data show that most of the geochemistry and hydrochemistry are related to regional and local geology. The geochemical heritage of geological environment in the Bouregreg river basin is very important, that results from the more compatible behaviour and the inertia of some elements during the weathering (3d transition elements (Co, Ni, Cr,…), interne transition elements f (lanthanides, Zr, Hf, Nb, Ta,…)). The geochemical homogeneity of the basin shows also heritage during the crustal accretion (magmatism-metamorphism-sedimentation) and the typology of this continental area is the same that the upper continental crust. Some anomalously high heavy metal analyses, particularly for As and Sb, may be related to anthropogenic activities.     

我国胶体与界面化学的发展

胶体与界面化学在能源、材料、生物、化学制造和环境科学等领域具有广泛的应用,并渗透到国民经济的各个主要领域中。所涉及到其中的一些重大科学问题,如土壤改良、功能与复合材料、三次采油、人造血浆、药物缓释与定向、润滑和油漆涂料等,与国家安全、能源开发、环境保护和人民生活等方面密切相关,发展胶体与界面化学学科对社会与经济的可持续发展具有重要的意义。本文综述了我国胶体与界面化学学科30年来的研究进展,尤其是近10年所取得的成就,主要包括新型两亲分子有序组合体的设计与构建、界面化学与有序分子膜、胶体与界面化学在微纳米功能材料合成中的应用新进展、胶体与界面化学在生物医药中的研究新进展,以及胶体与界面化学的研究新方法,并对该学科的发展前景与趋势进行了分析。     

Electronic structures and chemical bonding in 4d transition metal monohalides

Bond distances, vibrational frequencies, dipole moments, dissociation energies, electron affinities, and ionization potentials of MX (XM = Y-Cd, X = F, Cl, Br, I) molecules in neutral, positively, and negatively charged ions were studied by density functional method, B3LYP. The bonding patterns were analyzed and compared with both the available data and across the series. It was found that besides ionic component, covalent bonds are formed between the 4d transition metal s, d orbitals, and the p orbital of halogen. For both neutral and charged molecules, the fluorides have the shortest bond distance, iodides the longest. Although the opposite situation is observed for vibrational frequency, that is, fluorides have the largest value, iodides the smallest. For neutral and anionic species, the dissociation energy tends to decrease with the increasing atomic number from Y to Cd, suggesting the decreasing or weakening of the bond strength. For cationic species, the trend is observed from Y to Ag.     

128例脑性瘫痪血钙、锌、铁、铜、镁元素分析

为探讨小儿脑性瘫痪(CP)体内微量元素的变化,测定了128例脑性瘫痪患者血钙、锌、铁、铜、镁含量,随机选择128例正常儿童进行对照分析。结果表明,两组病例血锌、铜、镁均在正常范围,脑瘫组血钙56例、铁45例低于正常参考值,健康组血钙16例、铁11例低于正常参考值。经统计学处理,两组病例中血钙、铁、铜、镁含量具有显著性差异(P<0.05),血锌无显著性差异(P>0.05)。提示脑瘫儿童血钙、铁、铜、镁含量均低于正常儿童,补充钙、铁、镁等可能有利于脑瘫康复。     

Status of trace and toxic elements pollution in creek ecosystem using TXRF method

The economic development worldwide has brought in its wake many changes in the environment. Marine ecosystem which forms a part of this environment has been subjected to impact of industrialisation and urbanization. The study has been carried out in the creek ecosystem of Mumbai receiving the effluents from industrial and urban settlements. The trace elements such as P, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Pb, As, Rb and Sr were analysed in the creek water collected from the side receiving industrial effluent and discharges from the urban settlements using total reflection X-ray fluorescence spectrometry. On comparing the concentration of the trace element from the mid stream water of the creek with the water samples collected from the industrial and city effluent receiving side, it was found that the concentration of P, Ca, Mn, Fe, Co, Cu, Zn, Pb and As were found higher in the industrial side of the creek whereas V, Cr and Ni concentration were found higher in the samples collected from the side receiving city effluent.     

An indirect study of air pollution by neutron activation analysis of snow

Al, As, Br, Cd, Ce, Cl, Co, Cs, Cu, Fe, Hg, K, La, Mg, Mn, Mo, Na, Sb, Sc, Sr, Ti, V and Zn were determined in the soluble and insoluble fractions of snow which was collected at 6 differents sites in the Montreal area. From these data the variability coefficients and the enrichment factors were calculated and the probable sources of each element are discussed. The overall concentrations found in the snow were compared with the concentrations of these elements in the air sampled in the same area by high volume samplers. From these, the snow-out ratios for Cr, Cu, Fe, Mn, V and Zn and their mean were calculated. They are equal to 3338, 3389, 2322, 526, 563, 2603 and 2913 m³/kg respectively.     

The capability of neutron activation for trace element analysis in sea water and sediment samples of the Northern Adriatic Sea

In a framework of a more intensive study of the oceanographic phenomenology of the Northern Adriatic Sea, recently undertaken by the O. G. S. of Trieste, the present paper provides some insight into the determination of trace elements in sea water and bottom sediment matrices. Sampling procedure using continuous pumping and filtering and neutron activation analytical techniques are presented and the obtained results briefly discussed. Accounting for the physiography of the basin, for the oceanographic processes and for the different freshwater input, several samples were collected of filtered water in order to set up their properties. Results were obtained throughout the settlement only for long-lived radionuclides based on routine neutron activation: Cr, Ag, Co, Cs, Rb, Sb, Sc, Sr, Zn, U. For each of them, the concentration range was determined and discussed. Results indicate that the Cs, Rb, Sr and U concentration range is readily comparable with that assessed at open seas. On the contrary, for the other elements such as Cr, Ag, Co, Sc, Sb and Zn concentrations are noticeably higher than those found at open seas, mainly as far as samples collected near the sea bottom are concerned. The concentration increase is surely related to the burden of pollutants suffered by rivers. Moreover, the positive concentration gradient experienced toward the bottom, is fully in agreement with the estuarine character of the investigated area and in accordance with the strong decomposition of organic matter taking place in the bottom layer of the basin. Finally, the complexity of the sedimentary pattern in the Northern Adriatic renders it difficult to properly define the element concentration in bottom sediment. Only four samples were chosen as representative of the different sediments and analysed. Long-lived elements obtained are: Ce, Co, Cs, Cr, Rb, Sc, Tb, Yb. Their concentration was found to be related to the geochemical features of the activated matrix.