A sequential multielement separation scheme for determination of As,Mn, Mo,Cu and Zn in human milk by neutron activation analysis

A simple separation scheme for the analysis of As, Mn, Mo, Cu and Zn using neutron activation is described. It has been checked using three standard reference materials, A-11 milk powder (IAEA) and bovine liver and orchard leaves (USNBS) and found to give acceptable results. This scheme was applied for determination of these trace elements in mature human milk samples. The concentrations of As, Mn, Mo, Cu in samples obtained from two socio-economic groups—low and middle incomes—were not significantly different. However, Zn levels in samples obtained from the poor income group were significantly lower than in those obtained from the other group. Work carried out under Research Contract No. 2598/RB of International Atomic Energy, Vienna. Health Physics Division. Analytical Chemistry Division.     

含茂钛低聚物的制备与光谱

文中报道两种新的含茂钛低钛物Cp_2Ti(Cl)-O-[-Ti(Cp)(O_2CCH_4CH-O)-O-]n-H(Ⅰ)与Cp_2Ti(Cl)-O-[-Ti(Cp)(O_2CCH_2CH)-O-]_u-H(Ⅰ)的制备并用元素分析和光谱(IR,1~H NMR,MS)对它们进行了鉴定。     

低碳烃芳构化过程中HZSM－5催化剂结炭规律的研究

用ＧＣ、ＴＰＯ－ＧＣ、ＮＨ＿３－ＴＰＤ和ＴＥＭ等方法，测定了丙烷在ＨＺＳＭ－５沸石上芳构化过程中，催化剂的活性、结炭量、结炭Ｃ／Ｈ比、酸密度等，考察了催化剂的结炭量与其它参数之间的关系。结果表明，在反应温度为８７３Ｋ，进料空速ＷＨＳＶ＝５ｈ￣（－１）时，丙烷在ＨｚＳＭ－５上的结炭首先发生在沸石晶体的外表面的活性中心上（结炭量１．８％之前）；结炭量为１．８～３．４％时，主要在孔道交叉点结炭；结炭量在３．４～５．７％时，孔道已有受限或阻塞现象发生，导致一些富氢的结炭物在孔道内生成。     

Dissolution of ionisable groups and lignocellulosic components during low-temperature kraft pulping of pinus radiata

A wide range of kraft pulps from radiata pine produced by low-temperature kraft pulping in flow-through reactors was assessed for carboxyl and hexenuronic acid (HexA) contents using the conductometric titrations and UV spectrophotometer, respectively. The Kappa number of pulps varied from 20.8 to 84.7 when using a cooking liquor of 1 M effective alkali as Na₂O, 25% sulfidity, and cooking time of 100–250 min. The experimental results showed that the carboxyl groups (including HexA) and HexA groups dissolved and their residual values in the pulp samples correlate linearly with Kappa number and pulp yield. The dissolving rate of all carboxyl groups is much faster than the loss of HexA. The HexA/lignin ratio decreased non-linearly with Kappa number.     

A facile approach to surface graft vinyl acetate onto polyolefin articles

A facile and environment friendly approach was developed to graft vinyl acetate (VAc) onto plastic articles in an aqueous solution using tert‐butyl alcohol (TBA) as a compatiblizer and benzoyl peroxide (BPO) as an initiator. In a novel setup, excessive monomer suspended in a water phase, VAc could be conveniently grafted on the model substrate of low‐density polyethylene (LDPE) film and the graft percentage (GP) could be developed up to 7.3%. Reaction temperature could increase GP significantly, while adding monomer over a critical volume did not influence GP. By adding some paradioxybenzene, i.e. 0.06–0.08% in VAc phase, homopolymer PVAc could be avoided practically, while graft polymerization proceeded favorably in aqueous solutions. It was proved by attenuated total reflection‐infrared (ATR‐IR) spectroscopy that grafted VAc was located mainly at the surface of the LDPE film and hydrophilic nature of both grafted and alcoholyzed films were improved via contact angle measurements. Copyright © 2004 John Wiley & Sons, Ltd.     

四足配体铽配合物-蒙脱土超分子复合发光材料的插层组装、表征和性质研究

用两种方法分别将四足配体铽配合物[TbL（NO3）]^2＋和[TbL]^3＋插层组装到了蒙脱土（MT）层板间，制备出超分子复合发光材料[TbL（NO3）^2＋-MT和[TbL]^3＋-MT。方法一：通过离子交换反应让配离子[TbL（NO3）]^2＋取代钠＋基蒙脱土（Na-MT）中的Na^＋离子，插层组装到蒙脱土层板间。方法二：用配体L与铽基蒙脱土（Tb-MT）反应，使配体插入蒙脱土层板间与Tb^3＋离子配位。用元素分析、XRD，FT-IR,UV-vis和热分析对材料进行了表征，并对其荧光性质进行了研究。结果表明，复合材料保持了蒙脱土良好的层柱结构特征，其层间距d001值与插层配离予的直径吻合较好，配离子以单层形式分布于蒙脱土层板间，复合材料中配合物的热稳定性有明显提高。在紫外光激发下，复合材料发出较强的Tb^3＋特征荧光，其发射光谱与相应配合物的发射光谱很相似；复合材料中配合物的相对荧光强度较相应纯配合物有明显提高。荧光寿命较长；配合物的激发波长向可见光区发生位移，说明插层组装实现了对配合物激发波长的调制作用。     

二(1,8萘啶氮氧化物)合硝酸钍(Ⅳ)和铀酰(Ⅱ)配合物的合成及其性质

制得二(1,8-萘啶氮氧化物)合硝酸钍和铀酰配合物,元素分析确定其组成为Th(C_3H_6N_2O)_2(NO_3)_4和UO_2(C_3H_6N_2O)_2(NO_3)_2。通过红外光谱、荧光光谱、摩尔电导、差热热重分析等方法,研究了配合物的性质。     

The application of C-N.M.R. spectroscopy to the determination of the stereochemistry of Diels-Alder adducts

Long-range (³J) ¹³C-H coupling is a reliable probe to evaluate the stereochemistry of cycloaddition products. The method is best applied to carbonyl containing adducts but not restricted to them. Several structures have been revised and new ones evaluated.     

Large scale Biginelli reaction via water-based biphasic media: a green chemistry strategy

An important stage in process development is kilo scale preparation of the target compound. For this reason, a procedure involving water-based biphasic reaction media has been developed for conducting some exothermic reactions on a large scale. This protocol is illustrated by the energy-efficient and rapid preparation of dihydropyrimidinones by a solvent-free, green chemistry procedure applied to the Biginelli reaction using p-toluenesulfonic acid as catalyst.