New NIST sediment SRM for inorganic analysis

NIST maintains a portfolio of more than 1300 standard reference materials (SRM), more than a third of these relating to measurements in the biological and environmental fields. As part of the continuous renewal and replacement efforts, a set of new marine sediments has been recently developed covering organic and inorganic determinations. This paper describes the steps taken in sample preparation, homogeneity assay, and analytical characterization and certification with specific emphasis on SRM 2702 inorganics in marine sediment. Neutron activation analysis showed the SRM to be highly homogeneous, opening the possibility for use with solid sampling techniques. The certificate provides certified mass fraction values for 25 elements, reference values for eight elements, and information values for 11 elements, covering most of the priority pollutants with small uncertainties of only several percent relative. The values were obtained by combining results from different laboratories and techniques using a Bayesian statistical model. An intercomparison carried out in field laboratories with the material before certification illustrates a high commutability of this SRM.Electronic Supplementary Material Supplementary material is available in the online version of this article at     

中药微量元素的主成分分析

基于主成分分析的方法,研究了中药的相似性。主成分综合得分越近,中药就越相似。     

苏州荠苧总黄酮与微量元素含量的测定

采用分光光度法测定了苏州荠芋的总黄酮含量；采用了等离子发射光谱法测定了其元素含量。结果表明，苏州荠芋总黄酮的含量分别为55．31mg/g(7月采收)、65．00mg/g(8月采收)；含K、Ca、Mg等多种常量元素；含Cu、Fe、Mn、Zn、Cr、Co等多种人体必需的微量元素，其中Fe含量最高；而有害重金属元素Hg未检出，Pb和AS的含量均较低(小于药典规定量)。可见8月采收的苏荠芋总黄酮含量较高，苏州荠芋含多种人体必需的微量元素，有害重金属含量低，具有较大的开发价值。     

Fractionation and Bioaccessibility of Manganese,Copper, Zinc,Cadmium, and Lead in Commercial Vegetable and Rice Baby Foods Using Inductively Coupled Plasma - Mass Spectrometry (ICP-MS) with Central Composite Design (CCD)

Abstract

Herein the bioaccessibility of Mn, Cu, Zn, Cd, and Pb, selected from essential and toxic elements, was determined in commercially sold vegetable purees intended for infant and toddler consumption. Chemical fractionation studies using water, acetone, diethyl ether, chloroform:methanol, and n-hexane were employed to predict the importance of the protein and lipid parts of a matrix to assess the bioaccessibility data. In addition, in-vitro gastrointestinal digestion was performed to determine the bioaccessibility of the elements using a five level, three factor central composite design (CCD) to maximize the elemental solubility. The total elemental concentrations in all of the fractions were determined by inductively coupled plasma – mass spectrometry (ICP-MS). Based on the consumption of one jar of vegetable/rice-based baby food, Zn was 1.3% of the recommended dietary allowance and Mn was 4.2% of the adequate intake level, while Cu was almost 100% of the adequate intake level. Additionally, Pb was always below the detection limit and Cd was sometimes under the detection limit for the percent bioaccessibility. However, in some samples, Cd was as high as 80% of the tolerable weekly intake level depending on the body weight.     

A Closed-Form Relation for Dimension-Dependent Two-Electron Matrix Elements of the Interelectronic Distance

The evaluation of matrix elements of two electron atoms is fundamental for the study of the electronic properties of those systems. We add to this knowledge by presenting an explicit expression for the matrix elements of the inverse of the interelectronic distance of two-electron atoms in any spatial dimension D. The basis functions used are the D-dependent hydrogenic wavefunctions {1s ²,2p ²,3d ²,4f ²,5g ²,...,21y ²,...}, extending and including, in this way, the results of the previous basis set {1s ²,2p ²,3d ²,4f ²}. The methodology used does not employ Fourier integral transforms as in previous works but hypergeometric transformation formulas.     

Stabilization of p-block organoelement terminal hydroxides, thiols, and selenols requires newer synthetic strategies

Metal hydroxides represent a very interesting and highly useful class of compounds that have been known to chemists for a very long time. While alkali and alkaline earth metal hydroxides (s‐block) are commonplace chemicals in terms of their abundance and their use in a chemical laboratory as bases, the interest in Brønsted acidic molecular terminal hydroxides of p‐block elements, such as aluminum and silicon, has been of recent origin, with respect to the variety of applications these compounds can offer both in materials science and catalysis. Moreover, these systems are environmentally friendly, relative to the metal halides, owing to their ‐OH functionality (resembling that of water). Design and conceptualization of the corresponding terminal thiols, selenols, and tellurols (M? SH, M? SeH, and M? TeH) offer even more challenging problems to synthetic inorganic chemists. This concept summarizes some of the recent strategies developed to stabilize these otherwise very unstable species. The successful preparation of a number of silicon trihydroxides a few years back resulted in the generation of several model compounds for metal–silicates. The recent synthesis of unusual aluminum compounds such as RAl(OH)₂, RAl(SH)₂, and RAl(SeH)₂ with terminal EH (E=O, Se, or Se) groups is likely to change the ways in which some of the well‐known catalytic conversions are being carried out. The need for very flexible and innovative synthetic strategies to achieve these unusual compounds is emphasized in this concept.     

血清必需元素测定中样品预处理方法的探讨

对血清必需元素测定的样品预处理方法进行了研究，用火焰原子吸收法测定了经不同处理的血清样品中的锌，铜，铁，钙，镁含量，结果显示，预处理方法不同，其测定结果有较大差异，变异系数，镁为７．９４％，锌，铜，铁，钙在１５．１９％～５３．５３％之间，并对各样品作了精密度和准确度实验。     

二(2,4,4-三甲基戊基)膦酸萃取分离稀土元素(Ⅲ)的研究

本文研究了二(2,4,4-三甲基戊基)磷酸(Cyanex 272)的煤油溶液在不同介质(HCI,HNO_3)中对三价混合稀土的萃取分离性能.观测了平衡水相酸度对萃取平衡的影响,由酸度曲线求出相邻元素的平均分离系数,并考察了酸度对反萃取平衡的影响.比较了HCI和HNO_3介质中,Cyanex 272对混合稀土(Ⅲ)的萃取性能.     

食道癌患者血清铜／锌比值及血清硒含量的测定及临床意义

报道了３５例食道癌患者血清铜／锌比值及血清硒水平，结果发现食道癌患者血清铜／锌比值增加，血清硒水平下降，具有显著性差异（Ｐ〈０．００１）；同时提示随着食道癌分期增加，铜／锌比值进一步增加，血硒水平进一步下降，但无统计学差异。上述结果对临床诊断及观察病情变化有一定意义。     

Efficient oxidation of benzylic alcohols with [hydroxy(tosyloxy)iodo]benzene under microwave irradiation

An efficient method for the oxidation of benzylic alcohols with [hydroxy(tosyloxy)iodo]benzene under solvent-free microwave irradiation conditions is described.