交联壳聚糖树脂对Ni(II)的吸附行为研究

研究了甲醛、环氧氯丙烷交联壳聚糖树脂(AECTS)对Ni(II)的吸附行为和吸附Ni(II)对树脂结构及性能的影响.用FTIR,WAXD,TGA和DSC对吸附产物进行了结构表征,并深入分析了AECTS与Ni(II)之间的作用机理.结果表明:AECTS主要以配位形式吸附Ni(II);AECTS吸附Ni(II)后,结晶度下降、总体上热稳定性变差;Ni(II)对AECTS的主链分解具有明显的催化功能,而空气气氛中对AECTS在500℃附近的分解表现出火焰缓蚀作用.AECTS对Ni(II)的吸附行为符合Langmuir模型,属于单分子层吸附,所有吸附位对Ni(II)的作用近似相同;与壳聚糖(CTS)比较,造成AECTS对Ni(II)吸附量增大的主要原因是AECTS结晶度下降和孔隙率增加,二者导致在交联处理前Ni(II)难于接近的吸附位点“活性”相对增大,使其更容易与Ni(II)相结合;不同介质对AECTS吸附Ni(II)的影响大小顺序为HCl>CdCl2>MgCl2>NaCl,前两者使吸附量减小,MgCl2使吸附量稍有增加,NaCl对吸附量基本没有影响.     

因子分析－导数分光光度法同时测定混合物中多组分的研究

采用目标因子分析技术与导数光度法相结合，同时测定镍、铜、锌。用ＰＡＲ作显色剂，三种离子在一阶导数光谱最大吸收波长处的摩尔吸光系数分别为３．８×１０￣５，２．７×１０￣５和５．５×１０￣５Ｌ·ｍｏｌ￣（－１）·ｃｍ￣（－１）比基本光谱最大吸收波长处的摩尔吸光系数分别提高５．８、７．１和５．７倍。用于人工合成样的分析，结果良好。     

Oxidative conversion of methane and methanol on M/Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/cordierite structured metal oxide catalysts (m = Ni,Cu, Zn)

A study was carried out on the properties of Ni/Al₂O₃ and Cu-ZnO/Al₂O₃ composites supported on ceramic honeycomb monoliths made from synthetic cordierite in the carbon dioxide conversion of methane and the partial oxidation of methanol. The structured nickel-alumina catalysts are significantly more efficient than the conventional granulated catalysts. The improved working stability of these catalysts was achieved by adjusting the acid-base properties of the surface by introducing sodium and potassium oxides, which leads to inhibition of surface carbonization. The hydrogen yield was close to 90% in the partial oxidation of methanol with a stoichiometric reagent ratio in the presence of the Cu-ZnO/Al₂O₃/cordierite catalyst. A synergistic effect was found, reducing the selectivity of CO formation in the presence of the Cu-ZnO catalyst relative to samples derived from the individual components Cu and ZnO. __________ Translated from Teoreticheskaya i éksperimental’naya Khimiya, Vol. 43, No. 5, pp. 299–306, September–October, 2007.     

2—乙基己基膦酸单2—乙基己基酯与钴,镍,铜,锌固体萃合物的研究

酸性磷(瞵)酸酯是一类重要的萃取剂,它们对金属离子的萃取性能和机理研究巳有报导,但大多限于溶液体系。酸性磷酸酯金属萃合物的研究也有报导,但对固态烷基膦酸单烷基酯金属萃合物方面的报导较少。本文报导2-乙基已基膦酸2-乙基已基酯(简称HEH(EH)P或HA)金属(M=Co、Ni、Cu、Zn)固体萃合物的磁性,电子光谱和红外光谱,结合热分析结果对萃合物的成键特性和可能构型进行了讨论。     

Ni亚微米管装填Co金属丝同心复合结构有序阵列的模板合成及其磁性质

An ordered array of Ni submicrotubes with up to 35 μm in length has been successfully prepared by electrodeposition in the pores of alumina membrane modified with methyl-γ-diethylenetriaminopropyl-dimethoxysilane as pore-wall-modifying agent. Furthermore, using the array of Ni submicrotubes with an alumina membrane support as a “second-order-template”, the concentric composite structure of Co wires filling Ni submicrotubes was prepared by electrodeposition method. Magnetization measurements on the array of the Ni submicrotubes and the concentric composite structure of Co wires filling Ni submicrotubes revealed different uniaxial magnetic anisotropy.     

高压消解-火焰原子吸收光谱法测定大米中痕量铅铬镉镍和钴

采用高压溶样弹，将样品用硝酸－过氧化氢溶解后，用FAAS法对大米中铅、铬、镉、镍和钴测定，回收率为96％－103％，RSD分别为2.7%、3.1%、4.3%、3.9%和1.8%。应用于出口大米检测，取得满意的结果。     

乙腈液相选择性加氢中Ni-B非晶态合金和Raney Ni催化性能的比较

以乙腈液相选择性加氢为目标反应，分别考察了超细Ni-B非晶态合金和Rancy Ni的催化性能，发现两者的质量比活性相似，但单位活性比表面积上前者的活性及对乙胺的选择性显著高于后者，乙胺的最高得率前者为67．6％后者为40％。通过催化剂的系统表征，结合考察乙腈加氢反应的动力学，从几何效应和电子效应两方面阐述了Ni-B非晶态合金催化性能与催化剂结构和表面电子态的关系。     

铁（Ⅱ、Ⅲ）、钴（Ⅱ）、镍（Ⅱ）、铜（Ⅱ）－MBTAE配合物的反相高效液相色谱分离和测定

本文报道了以２－（６－甲基－２－苯并噻唑偶氮）－５－二乙氨基酚（ＭＢＴＡＥ）作柱前衍生化试剂，在ＳｐｈｅｒｉｓｏｒｂＣ＿８柱上，以甲醇：水＝８０：２０（Ｖ／Ｖ），含２ｍｍｏｌ／ＬＬｉ＿２ＳＯ＿４和１０ｍｍｏｌ／ＬｐＨ５．０醋酸盐缓冲溶液作流动相，反相高效液相色谱分离和测定了Ｆｅ￣（２＋）、Ｃｏ￣（２＋）、Ｎｉ￣（２＋）和Ｃｕ￣（２＋）。各金属离子的检出限（Ｓ／Ｎ＝３）分别为（ｐｇ）：Ｆｅ￣（２＋）６．４０，Ｃｏ￣（２－）１．３８，Ｎｉ￣（２＋）４．４７，Ｃｕ￣（２＋）７．２８。方法用于欧洲标准局，黑麦草标样的分析，所得结果与标准值相符。     

Capillary electrophoresis chemiluminescence assay of naphthol isomers in human urine and river water using Ni(IV) complex‐luminol system

A capillary electrophoresis method involving online indirect chemiluminescence (CL) detection was used to determine naphthol (NAP) isomers. The method was based on the quenching effect of 1‐ and 2‐NAP on a new CL reaction of luminol with Ni(IV) complex in an alkaline medium. Separation was conducted with a 25.0 mM sodium borate buffer containing 0.8 mmol/L luminol. Under optimized conditions, 1‐ and 2‐NAP were baseline separated and detected in less than 8 min. The limits of detection of 1‐ and 2‐NAP were 3.1 and 2.7 μg/L, respectively (S/N = 3), with a linear range of 4.0–80.0 μg/L (r > 0.995). Analysis of real samples demonstrated that the spiked recoveries were in the range of 89.2–107.5% (n = 3). The proposed method was successfully used to determine 1‐ and 2‐NAP contents in three environmental water samples and 14 human urine samples. No derivatization or tedious pretreatment was required in the analysis. The proposed method is a potential approach for routine tests of naphthol isomers in a facile CE–CL system.     

Nickel electrodes as a cheap and versatile platform for studying structure and function of immobilized redox proteins

Practical use of many bioelectronic and bioanalytical devices is limited by the need of expensive materials and time consuming fabrication. Here we demonstrate the use of nickel electrodes as a simple and cheap solid support material for bioelectronic applications. The naturally nanostructured electrodes showed a surprisingly high electromagnetic surface enhancement upon light illumination such that immobilization and electron transfer reactions of the model redox proteins cytochrome b₅ (Cyt b₅) and cytochrome c (Cyt c) could be followed via surface enhanced resonance Raman spectroscopy. It could be shown that the nickel surface, when used as received, promotes a very efficient binding of the proteins upon preservation of their native structure. The immobilized redox proteins could efficiently exchange electrons with the electrode and could even act as an electron relay between the electrode and solubilized myoglobin. Our results open up new possibility for nickel electrodes as an exceptional good support for bioelectronic devices and biosensors on the one hand and for surface enhanced spectroscopic investigations on the other hand.