镀锌镍铁合金溶液中硫酸镍的快速测定

镀锌镍铁合金溶液中硫酸镍的测定,过去采用了二酮肟镍重量法,过程冗长,分析费时。本文制定了丁二酮肟光度法,用于镀液中硫酸镍的快速测定。对于镍铁体系中镍的光度法测定,过去采用酒石酸钾钠掩蔽铁,但酒石酸铁络合物的颜色与丁二酮肟镍相近,影响镍的测定。本文选用三乙醇胺掩蔽铁,使铁在碱性溶液中生成无色络合物,有效地消除了铁对测定镍的影响。以往的经验认为,丁二酮肟与镍离子的显色速度     

铁镍镀层中铁镍组成的紫外-可见分光光度分析法

用紫外－可见分光光度法分析了电沉积在导电玻璃上的NiFe合金镀层，三价铁与EDTA和H2O2形成稳定的深紫色三元络合物；在氨性溶液中，当有氧化剂存在时，镍与丁二酮肟形成酒红色的络合物，用吸收光度法可分别在519nm和538nm波长处测定铁、镍的含量，对Fe和Ni的相对标准偏差分别为0．95％和1．2％，适用含量范围分别为1－50mg/L和0．5－20mg/L；对实际样品的测定结果与XPS分析的一致，该法也适用于其他样品中铁、镍含量的测定。     

火焰原子吸收光谱法测定高纯氧化铝和氢氧化铝中痕量镍

选用碳酸钾加硼酸熔融样品，在pH 8～9的微氨性溶液中，镍与丁二酮肟定量生成络合物，用三氯甲烷单取分离基体。有机相经盐酸反萃取，镍返回水相，用原子吸收法测定。测定范围为1×10-4％～3×10-3％。     

2-(2-喹啉偶氮)-5-二乙氨基苯甲酸固相萃取光度法测定环境水样中的镍

用2－（2－喹啉偶氮）－5－二乙氨基苯甲酸（QADEAB）与镍的显色反应及Waters Porapak^R Sep-Park固术萃取小柱对显色络合物的固相萃取，建立了测定水样中μg/L级镍的新方法。水样中的镍在pH=8.0的硼酸－磷酸二氢钾缓冲介质中和Tween 80存在下与QADEAB反应生成2：1稳定有色络合物，该络合物可用Waters Porapak^R Sep-Park固相萃取小柱富集，用乙醇洗脱后用光度法测定，可测定水样中μg/L级的镍。方法用于几种环境水样分析，结果令人满意。     

β—环糊精交联聚合物包结5—Br—PADAP配合物富集铜和镍的研究

β－环糊精交联聚合物包结有机显色剂２－（５－溴－２－吡啶偶氮）－５－二乙氨基苯酚所形成的配合物树脂可与多种金属离子反应生成吸附配合物，本文报道了以这种包结配合物树脂吸附富集铜与镍的有关实验条件，反应机理以及用分光光度法进行测定的研究，结果表明，在ｐＨ＝４～６的弱酸性介质中，包结树脂可以分别从稀溶液中定量吸附铜与镍，富集倍数达到５０倍（铜）与２００倍（镍）。     

用分光光度法测定固相络合物的组成

以镍－丁二酮肟显色体系和钇－８－羟基喹啉显色体系为例，对萘相中络合物的测量原理和测定方法进行探讨，测得镍与丁二酮肟萘相络合物的组成比以及钇与８－羧基喹啉萘相络合物的组成比均为１：２。     

β－环糊精交联聚合物包结5－Br－PADAP配合物富集铜和镍的研究

β－环糊精交联聚合物包结有机显色剂２－（５－溴－２－吡啶偶氮）－５－二乙氨基苯酚所形成的配合物树脂可与多种金属离子反应生成吸附配合物。本文报道了以这种包结配合物树脂吸附富集铜与镍的有关实验条件、反应机理以及用分光光度法进行测定的研究。结果表明，在ｐＨ＝４～６的弱酸性介质中，包结树脂可以分别从稀溶液中定量吸附铜与镍。富集倍数达到５０倍（铜）与２００倍（镍）。     

β—环糊精交联聚合物包结α—吡啶偶氮—β—萘酚络全物树脂吸附…

以环氧氯丙烷为交联剂合成的β－环糊精聚合物树脂在与１－（２－吡啶偶氮－２－萘酚形成的包结络全物能与多种金属离子形成稳定的吸附络合物，本文报道了以这种包结络合物吸附富集铜、镉、镍与锰的实验条件以及用原子吸收分光光度法测定痕量铜、镉、镍与锰的研究，实验中详细地了有关的吸附条件及富集倍数，提出了一种富集与测定痕量金属的新方法。     

2-(2-喹啉偶氮)-1,5-苯二酚固相萃取光度法测定饮用水中铜的研究

根据新试剂2－（2－喹啉偶氮）－1，5－苯二酚（QADHB）与铜的显色反应及Waters Porapak Sep-Park固相萃取小柱对显色络合物的固相萃取，建立了一种测定水样中铜的新方法。在pH=4.0 HAc-NaAc缓冲介质中，溴化十六烷基三甲基铵（CTMAB）存在下，QADHB与铜反应生成2：1稳定络合物，该络合物可用Waters Porapak Sep-Park固相萃取小柱富集，用乙醇洗脱后用光度法测定，可测定水柱中μg/L级的铜。方法用于几种饮用水中铜的分析，结果令人满意。     

丁二酮肟快速光度法测定不锈钢中的镍

建立测定不锈钢中镍的丁二酮肟快速光度法。镍的浓度在0.5-1.1mg/50mL吸光度呈线性关系，测定结果的相对标准差为0.48%-0.96%。该方法简便、快速，节约试剂，测定结果准确。     

Tetraalkoxyaluminates of nickel(II), copper(II), and copper(I)

The syntheses and structural details of tetraisopropoxyaluminates and tetra-tert-butoxyaluminates of nickel(II), copper(I), and copper(II) are reported. Within the nickel series, either Ni[Al(OiPr)4]2.2HOiPr, with nickel(II) in a distorted octahedral oxygen environment, or Ni[Al(OiPr)4]2.py, with nickel(II) in a square-pyramidal O4N coordination sphere, or Ni[(iPrO)(tBuO)3Al]2, with Ni(II) in a quasi-tetrahedral oxygen coordination, has been obtained. Another isolated complex is Ni[(iPrO)3AlOAl(OiPr)3].3py (with nickel(II) being sixfold-coordinated), which may also be described as a "NiO" species trapped by two Al(OiPr)3 Lewis acid-base systems stabilized at nickel by three pyridine donors. Copper(I) compounds have been isolated in three forms: [(iPrO)4Al]Cu.2py, [(tBuO)4Al]Cu.2py, and Cu2[(tBuO)4Al]2. In all of these compounds, the aluminate moiety behaves as a bidentate unit, creating a tetrahedrally distorted N2O2 copper environment in the pyridine adducts. In the base-free copper(I) tert-butoxyaluminate, a dicopper dumbbell [Cu-Cu 2.687(1) A] is present with two oxygen contacts on each of the copper atoms. Copper(II) alkoxyaluminates have been characterized either as Cu[(tBuO)4Al]2, {Cu(iPrO)[(iPrO)4Al]}2, and Cu[(tBuO)3(iPrO)Al]2 (copper being tetracoordinated by oxygen) or as [(iPrO)4Al]2Cu.py (pentacoordinated copper similar to the nickel derivative). Finally, a copper(II) hydroxyaluminate has been isolated, displaying pentacoordinate copper (O4N coordination sphere) by dimerization, with the formula {[(tBuO)4Al]Cu(OH).py}2. The formation of all of these isolated products is not always straightforward because some of these compounds in solution are subject to decomposition or are involved in equilibria. Besides NMR [copper(I) compounds], UV absorptions and magnetic moments are used to characterize the compounds.     

PROPERTIES OF Ni-Cu/SiO_2 BIMETALLIC CATALYSTSPREPARED BY SOLVATED METAL ATOM DISPERSION(SMAD) TECHNIQUE

IntroductionAsoneofthemethodsofpreparationofsupportedmetalcatalysts,solvatedmatalatomdispersion(SMAD)onoxidesupportsattractsmuchattentionnowadays.TIstechniquehasbeendevelopedbyKlabunde'SandOzin'sresearchgroups.Itprovidesanumberofadvantages,ascomparedwitht…     

Elemental analysis of Cu−Ni and Nd−Al alloys and, nickel and iron powders by energy dispersive X-ray fluorescence (EDXRF) technique

Energy dispersive X-ray fluorescence spectroscopy (EDXRF) has been used for elemental analysis of Cu−Ni alloy, neodymium aluminide, and iron and nickel powder. The preparation of Cu−Ni alloy and neodymium aluminide has been carried out by aluminothermic reduction of mixed oxides of copper and nickel and neodymium oxide respectively. Aqueous electrorefining technique has been followed for the preparation of iron and nickel powder using Fe−Ni alloy as anode. The determination of major and trace elements present in the Cu−Ni and, electrolytically refined nickel and iron has been accomplished by EDXRF using Cd¹⁰⁹ radioisotope source. In the case of Nd−Al alloy Am²⁴¹ radioisotope source has been used. The rapid and multielement analysis of the thermit product by EDXRF has aided in the appropriate variation of the charge constituents during the standardization of the optimum charge composition for Cu−Ni alloy. EDXRF analysis of electrolytically refined nickel and iron revealed heavy contamination of iron in nickel as compared to that of nickel in iron. Neodymium content has been found to be 67.68% in Nd−Al alloy.     

从2AlCl3/Et3NHCl离子液体中电沉积制备Ni 和Ni-Al 合金

在含Ni2+的2AlCl3/Et3NHCl离子液体中的铜电极上通过恒电位电沉积制备出金属Ni和Ni-Al合金.采用循环伏安和计时电流方法,揭示铜电极上沉积金属Ni的成核机理,研究了电沉积Ni-Al合金的机理,以及恒电位沉积Ni-Al合金工艺条件对沉积Ni-Al合金表面形貌和电流效率的影响.结果表明:在铜电极上电沉积金属Ni的成核机理为受扩散控制的三维瞬时成核过程.在电量≥3.0 C时,电沉积Ni-Al合金的组成基本不再变化.Ni-Al合金的电沉积机理为,Ni的电沉积受扩散控制,同时进行Al的欠电位沉积,在Ni-Al合金电沉积过程中某些Ni-Al合金相的沉积可能受动力学限制而使Ni-Al合金的组成偏离热力学预测结果.在电沉积Ni-Al合金的沉积电流小且平稳,电沉积速率慢条件下,Ni-Al合金表面形貌致密均一,反之就会出现瘤节.电沉积Ni-Al合金的电流效率＞90％.电沉积物的组成接近于Ni3Al合金.     

溶剂化金属原子浸渍法制备高分散负载型催化剂(Ⅶ)——Ni-Cu/SiO2双金属催化剂的结构与性能

利用金属蒸气法制备了不同组成的Nj-CujSiO₂双金属催化剂,XRD、TEM和磁性测定表明有Ni-Cu合金形成,合金颗粒的组成不均匀,而且有部分自由的Ni和Cu存在;Ni/Cu摩尔比为1:1催化剂的催化活性大于2:1和3:1的双金属催化剂以及Ni和Cu的单金属催化剂。     

Effect of surface structure on the catalytic behavior of Ni：Cu/Al and Ni：Cu：K/Al catalysts for methane decomposition

Methane decomposition using nickel, copper, and aluminum （Ni：Cu/Al） and nickel, copper, potassium, and aluminum （Ni：Cu：K/Al） modified nano catalysts has been investigated for carbon fibers, hydrogen and hydrocarbon production. X-ray photoelectron spectroscopy （XPS）, static secondary ion mass spectrometry （SSIMS）, thermal gravimetric analysis （TGA）, Fourier transform infrared （FT-IR）, secondary electron microscopy/X-ray energy dispersive （SEM-EDX）, and temperature programmed desorption （TPD） were used to depict the chemistry of the catalytic results. These techniques revealed the changes in surface morphology and structure of Ni, Cu, Al, and K, and formation of bimetallic and trimetallic surface cationic sites with different cationic species, which resulted in the production of graphitic form of pure carbon on Ni：Cu/Al catalyst. The addition of K has a marked effect on the product selectivity and reactivity of the catalyst system. K addition restricts the formation of carbon on the surface and increases the production of hydrogen and C2, C3 hydrocarbons during the catalytic reaction whereas no hydrocarbons are produced on the sample without K. This study completely maps the modified surface structure and its relationship with the catalytic behavior of both systems. The process provides a flexible route for the production of carbon fibers and hydrogen on Ni：Cu/Al catalyst and hydrogen along with hydrocarbons on Ni：Cu：K/Al catalyst. The produced carbon fibers are imaged using a transmission electron microscope （TEM） for diameter size and wall structure determination. Hydrogen produced is COx free, which can be used directly in the fuel cell system. The effect of the addition of Cu and its transformation and interaction with Ni and K is responsible for the production of CO/CO2 free hydrogen, thus producing an environmental friendly clean energy.     

铜镍和铜钴合金电极在碱性介质中的光电化学

用动电位伏安法对含镍量10％、30％和50％的铜镍合金以及含钴量5.1％、9.7％、15 ％、25％和40％的铜钴合金电极在硼砂-硼酸缓冲溶液（pH 8.5）中的光电化学行为进行了 研究.铜镍合金和铜钴合金均显示p-型光响应,铜镍合金的光响应来自Cu2O,铜钴合金的光 响应来自Cu2O和氧化钴.含镍量10％和30％的铜镍合金电极以及含钴量5.1％铜钴合金电极的 最大光电流iph,max均大于纯铜电极,含钴量15％、25％和40％的铜钴合金电极以及含镍量 50％的铜镍合金电极由于电极表面相当一部分面积分别被氧化钴和氧化镍所占有,iph,max 小于纯铜电极.铜镍合金电极的φv值（电位负向扫描过程中电极表面完全还原为Cu时的电位 ）负于纯铜电极,而铜钴合金电极的φv值与纯铜电极大致相等, NiO的存在致使铜镍合金 表面Cu2O膜具有更大的稳定性.从光电化学角度通过φv和iph,max反映铜合金的耐腐蚀性能 与交流阻抗法测得的结果相符.     

Untersuchungen an Metallkatalysatoren. XIX. Zur katalytischen Wirksamkeit von Ni?Cu?Re-Katalysatoren

Investigations on Metal Catalysts. XIX. Catalytic Efficiency of Ni? Cu? Re Catalysts Alloying of Ni? Cu catalysts with rhenium causes an increased activity in the case of dehydrogenation of cyclohexane as well as the hydrogenolysis of ethane. The catalytic dehydrogenation activity is essentially determined by the f.c.c. phase of the ternary alloy system. In the case of ethane hydrogenolysis, both the f.c.c. and the h.c.p. phases are active, and both are desactivated by copper. The dehydrogenation activity of Ni? Cu? Re samples with medium copper content and low rhenium content is higher by one order of magnitude in comparison with nickel, and their hydrogenolysis activity is considerably lower.     

化学镀镍诱发过程的研究 II.用电子能谱研究诱发过程

In the previous paper, it was reported that a sudden decrease down to -0.6V and lower in stationary potential was observed from the stationary potential-time curve and the reaction of electroless nickeling could be induced by metallic iron catalyst when it was in contact with substrate metallic copper. In this paper, AES and XPS surface analysis and depth profile technique was employed to investigate the surface and depth distribution of Ni, Cu, Fe and P in the nickel coating deposited on the substrate metal. The experimental results showed that there was a thin adsorption layer consisting of C, S and Cl. The pure electroless nickel deposition, its Ni/P ratio being about two, existed under the adsorption layer. A layer with rapidly changed Ni/P ratio occurred close to the surface of substrate metal, under this layer the substrate metal was alloyed with Ni and P, thus becoming Cu-Ni-P alloy. The ratio of components in this alloy was found to be Cu:Ni:P=56:36:5. This fact explained why the electroless nickel deposition can preferably adhered to the substrate metal. In inducing process, Fe was not detected by AES from the substrate metal and nickel deposition. Thus it showed that the inducing reaction takes place without the deposition of inducing metal.     

Test Determination of Cu(II), Ni(II), and Cr(VI) in a Single Sample

It was shown that Cr(VI), Ni(II), and Cu(II) can be simultaneously adsorbed on a solid phase consisting of two filled fibrous disks and then determined visually using organic reagents. One sorbent disk, a fibrous material filled with an AB-17 anion exchanger, was used to determine chromium by its reaction with 1,5-diphenylcarbazide. Another disk filled with an KU-2 cation exchanger was used for the simultaneous sorption of copper and nickel followed by the consecutive determination of nickel with dimethylglyoxime and copper with sodium diethyldithiocarbamate. The conditions were optimized for the determination of nickel in the presence of copper and of copper in the presence of nickel after decomposing its dimethylglyoxime complex with 1 M HCl. The detection limits were 0.02, 0.1, and 0.05 mg/L for Cr, Ni, and Cu, respectively. The time of analysis was no longer that 20 min.