沉淀分离ICP—AES测定铅锭中Te,Cr,Co,Ni杂质元素

采用硫酸沉淀分离基本元素铅后，ＩＣＰ－ＡＥＳ直接测定铅锭中Ｔｅ、Ｃｒ、Ｃｏ、Ｎｉ杂质元素。试验证明在本文提供的条件下Ｓｅ会以ＰｂＳｅＯ３的形式与ＰｈＳＯ４共沉淀，而Ｔｅ、Ｃｒ、Ｃｏ、Ｎｉ等待测元素则保留在溶液中。待测元素加标回收率在８６．４％￣１０８．４％之间。     

直读光谱仪单SAFT光源测定锌锭中的杂质元素

采用直读光谱仪单SAFT光源测定锌锭中杂质元素的含量。通过试验确定仪器工作条件如冲洗时间、预激发时间、SAFT激发时间等。将样品用车床加工出符合测定要求的平面,在选定的仪器工作条件下,单独使用SAFT光源对样品进行激发,测量发射光强度,根据工作曲线计算并输出杂质元素含量。该方法测定锌光谱标样中杂质元素含量的结果与标准值相符,与其它方法比对结果一致,测定结果的相对标准偏差不大于5%(n=11),所有元素的线性相关系数均大于0.999 7。该方法准确度高,精密度好,可用于测定锌锭中的杂质元素含量。     

共沉淀分离富集-电感耦合等离子体原子发射光谱法测定高纯氧化钨中痕量金属杂质

提出了以Ｌａ（ＯＨ）３为共沉淀剂，对高纯氧化钨中的痕量金属杂质元素经共沉淀预分离富集后进行ＩＣＰ－ＡＥＳ测定的分析方法。探讨了影响杂质元素回收率和钨残留量的若干因素，确定了合适的分离富集条件。合成试样和标准样品的测试结果表明： Ｂｉ、Ｃａ、Ｃｄ、Ｃｏ、Ｃｕ、Ｆｅ、Ｍｇ、Ｍｎ、Ｎｉ、Ｐｂ、Ｓｂ、Ｓｎ、Ｔｉ等元素能被定量分离回收，回收率和精密度均令人满意。     

共沉淀分离富集—电感耦合等离子体原子发射光谱法测定高纯氧化？…

提出了以Ｌａ（ＯＨ）３为共沉淀剂，对高纯氧化钨中的痕量金属杂质元素经共沉淀预分离富集后进行ＩＣＰ－ＡＥＳ测定的分析方法，探讨了影响杂质元素回收率和钨残留量的若干因素，确定了合适的分离富集条件，合成试样和标准样品的测试结果表明，Ｂｉ，Ｃａ，Ｃｄ，Ｃｏ，Ｃｕ，Ｆｅ，Ｍｇ，Ｍｎ，Ｎｉ，Ｐｂ，Ｓｂ，Ｓｎ，Ｔｉ等元素能被定量分离回收，回收率和精密度均令人满意。     

电感耦合等离子体质谱测定高纯氧化铈中14种稀土杂质

用电感耦合等离子体质谱（ＩＣＰ－ＭＳ）建立了直接测定９９９９％ＣｅＯ２中１４个稀土杂质含量的方法。采用基体匹配法扣除Ｃｅ对Ｌａ、Ｐｒ、Ｇｄ和Ｔｂ元素的干扰，以Ｉｎ为内标，１４种稀土元素的测定下限之和≤０００８％，加标回收率为９０％～１１０％。     

ICP—AES法测定陶瓷二氧化铀芯块粉末标准物质中铝,钡,钴,钽,钛和钒

随着大型核电事业的发展,对核纯陶瓷二氧化铀芯块的质量控制、质量保证及对测试方法的校准和确认等方面,迫切需要研制核纯陶瓷二氧化铀芯块的杂质标准物质.测定铀及其化合物中痕量杂质元素,需预先将铀与杂质元素分离,国外大多采用萃取法,国内都采用萃取色谱法.所用萃取剂有TBP、TOPO以及TEHP等.本文用我院合成的237季铵萃取树脂进行分离富集,并用ICP-AES法同时测定陶瓷二氧化铀芯块粉末标准物质中铝、钡、钴、钽、钛和钒.     

电感耦合等离子体原子发射光谱法高纯三甲基镓中的痕量杂质

对电感耦合等离子体原子发射光谱（ＩＣＰ－ＡＥＳ）法测定高纯三甲基镓（９９．９９９９Ｔ,相对于金属镓的含量）中Ｃu、Ｆe、Ｓi、Ｚn等３１种痕量杂质元素的含量进行了研究,考察了基体元素镓对杂质元素的光谱和非光谱干扰以及基体浓度对杂质元素谱线信噪比和检出限的影响在优化的实验条件下,获得了满意的结果。     

全反射X射线荧光光谱法同时测定地气样品中锰,镍,铜,锌,铅,铷和锶

论述了利用自行研制的有３个反射体的全反射分析装置，用钼靶Ｘ光管激光发，以Ｓｅ为内标，同时测定了地气样品中Ｍｎ，Ｎｉ，Ｃｕ，Ｚｎ，Ｐｂ，Ｒｂ和Ｓｒ等元素。对纳克级元素含量，方法的精密度为７．２％，绝对检出限为１０＾１０－１０＾－１１ｇ。其分析结果的准确度与无火焰原子吸收相符。     

萃取分离 ICP-AES 法测定含铪铀中微量杂质元素

用盐酸-硝酸-氢氟酸溶解含铪的铀试样,以磷酸三丁酯为萃取剂,分离铀、铪与待测杂质元素.用 ICP-AES 法同时测定了试样中钼、钨、铁、硼、锰、铍、铜、镁、钙、铝和镍等11种杂质元素的含量.将 0.0900 g～0.1100 g 试样制成 6 mL 溶液时,各杂质元素测量范围为 1.0×10-3%～1.0×10-1%,回收率在 94%～105% 之间,相对标准偏差优于 10%.     

以 N_2作冷却气的小功率 ICP 发射光谱法测定钛合金中钼、钒、铬、铝、铁和钇

Ar-ICP发射光谱法测定合金成分和杂质元素以及有关N_2/Ar ICP光源研究已见诸报导。本文提出以N_2作冷却气的小功率低气流ICP-发射光谱法测定钛合金中六个元素。通过实验选定了N_2冷却ICP的最佳工作条件,进行了钛合金基体干扰,溶液酸度,K~+、NH_4~+离子对分析线的影响试验。本方法用一次溶样同时测定钛合金中四种合金成分钼、钒、铬、铝和两种杂质元素铁及钇。相对标准偏差合金成分元素为1.48～2.21％;杂质元素为3.8～6.0％。     

Oxidations and reductions of iron-cyanogen compounds of cobalt,nickel, cadmium and zinc

I. Cobalt ferrocyanide is oxidized by bromine water, by nitrous acid or by hydrogen peroxide in presence of acids to cobalt ferroferricyanide (cobalt Prussian blue), while cobalt ferricyanide is reduced by sulfurous acid to cobalt Prussian blue.II. Nickel ferrocyanide is oxidized by nitrous acid or by hydrogen peroxide in presence of acids to nickel ferricyanide.III. Nickel ferrocyanide and cadmium ferrocyanide are oxidized by bromine water to the ferricyanides.IV. The ferricyanides of nickel, cadmium and zinc are reduced by sulfurous acid to the ferrocyanides.     

Role of substrate on film thickness,structural, compositional and magnetic properties of CoNi alloy thin films by low temperature electrodeposition technique

Impressment of Cobalt and Nickel based alloys in industries for the last few years attracted many researchers due to its significant features of physical, chemical and magnetic properties. The present work focused the structural, compositional, morphological and magnetic properties of Cobalt Nickel alloy thin film growth by one of the chemical methods. Thin films of Cobalt Nickel have been deposited on various substrates by means of low cost galvanostatic electrodeposition technique. Structural investigation showed that the deposited films have face centred cubic structure with orientation of crystallites along (1 1 1) plane. The structural parameters such as crystallite size, rms microstrain, dislocation density and stacking fault probability are estimated for the deposited films. Morphological features along with film composition showed that the deposited films have smooth surface with stoichiometry. Magnetic properties such as coercivity, remanence, retentivity was estimated and the results are reported.     

NiSO4·6H2O as a new,efficient, and reusable catalyst for the α-aminophosphonates synthesis under mild and eco-friendly conditions

Research on Chemical Intermediates - Nickel (II) sulfate hexahydrate is used for the first time as an efficient catalyst for the one-pot synthesis of α-aminophosphonates by three-component...     

Poly(alkylene-H-phosphonate)s obtained by direct esterification and oxidation of hypophosphorous acid with ethylene glycol

This paper presents for the first time the synthesis of poly(alkylene-H-phosphonate)s by one-pot tandem reaction of hypophosphorous acid and ethylene glycol. Zirconium oxychloride was used as esterification catalyst, Nickel vinylphosphonate, Nickel sulfate, Nickel chloride hexahydrate were used as transfer hydrogenation catalyst. Nickel vinylphosphonate was synthesized in our laboratory and used for the first time as catalyst in this process. The compounds were characterized by ¹H-NMR, ¹³C-NMR and ³¹P-NMR spectroscopy. Molar masses were determined by SEC-MALLS technique and depend on the catalyst used. The obtained poly(alkylene-H-phosphonate)s have molar masses between 1.50 and 11.85 kDa, higher than those obtained by other methods mentioned in the literature.     

稀土在电沉积锌—镍合金中的作用

锌—镍合金镀层具有耐蚀性高、低氢脆性和与基体的结合力好等特性 ,是良好的防护性镀层。当合金镀层的镍含量在 7～ 1 8% (质量 )时 ,镀层的耐蚀性最高 ,因此它可代替传统的锌镀层、锡镀层和镉镀层而广泛应用于电镀汽车钢板、航空航天及家电等行业[1～ 3] 。稀土元素 ( RE)包括了 1 5个镧系元素和钇元素 ,共 1 6个元素。由于稀土元素具有独特的电子层结构和化学性能 ,使稀土及其化合物在材料科学领域中的应用越来越广泛 ,尤其是稀土在电沉积过程中的研究及应用正日趋深入。文献资料表明 ,在电镀溶液中加入少量的稀土化合物后 ,可以改善镀液…     

Synthesis and Characterization of Nickel Oxide Nanoparticles from Ni(salen) as Precursor

Nickel oxide nanoparticles have been synthesized by thermal treatment of N,N′-(bis(salicylidene)-ethylene-1,2-diamine)Nickel(II); [Ni(salen)]; as precursor which has been synthesized via two methods: [Ni(salen)] were obtained by solid state reaction in absence solvent and co-precipitation reaction in presence of propanol as solvent, respectively. Nickel oxide nanoparticles were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and Fourier transform infrared spectroscopy.     

Die Bestimmung von Kupfer- und Nickelspuren in Gallium

Zusammenfassung Nickel- und Kupferkontaminierungen in Gallium im ppm-Bereich und darunter stören empfindlich bei der Verwendung in der Halbleiterphysik. Der Chloridkomplex des Galliums in 6-n HC1 wird von einem stark basischen Anionenaustauscher effektiv zurückgehalten, während Nickel die Säule als Kation durchläuft. In 4-n HC1 werden Kupfer und Nickel vom Gallium abgetrennt und voneinander isoliert. Nickel geht ohne Verzögerung in den Auslauf, während Kupfer infolge der Bildung schwacher Chloridkomplexe nachfolgt. Der Galliumkomplex wird auch in diesem Medium am Harz zurückgehalten. Isoliertes Nickel wird unter Verwendung eines Kationenaustauschers und Rubeanwasserstoffs getüpfelt. Mit dem gleichen Reagens, aber auf Filterpapier tüpfelt man das abgetrennte Kupfer. Die vorgeschlagene Methode erlaubt es, bis zu 0,03 ppm Nickel und 0,5 ppm Kupfer rasch und sicher in Gallium zu bestimmen.

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Assay of copper and nickel traces in gallium

Summary Nickel and copper contaminations in ppm levels and below give rise to critical disturbances when gallium is used in semiconductor physics. The chloride complex of gallium in 6N HCl is effectively retained by a strongly basic anion exchanger, while as a cation nickel passes through the column. Copper and nickel are separated from gallium in 4 N HCl and isolated from each other. Nickel passes into the outflow without delay, whereas copper follows later in consequence of the formation of weak chloride complexes. The gallium complex is also retained on the resin in this medium. Isolated nickel is spotted using a cation exchanger and thiocyanic acid. The separated copper is spotted with the same reagent, but on filter paper. The suggested method permits up to 0.03 ppm nickel and 0.5 ppm copper to be determined quickly and surely in gallium.

     

Electrophoretic deposition of network-like carbon nanofiber as a conducting substrate for nanostructured nickel oxide electrode

A vapor-grown carbon nanofiber (VGCF) film with network-like architecture was fabricated by electrophoretic deposition (EPD) in the isopropanol suspension containing Ni(NO₃)₂ additive. Nickel ions adsorbed on the VGCFs increase the zeta potential of VGCFs, consequently, the EPD rate and nanofiber dispersion are remarkably improved. Nickel deposition is accompanied by reducing the nickel ions on the surface of VGCFs. Nickel appears to be suitable as a conducting metal binder for attaching the VGCFs. EPD of the nickel oxide on VGCF-coated film exhibits excellent capacitive behavior compared with that bare NiO electrode, resulting from the reduced electron conducting and charge-transfer resistances.     

Functionalized polyolefin synthesis using [P,O]Ni catalysts

Nickel olefin polymerisation catalysts containing bulky phosphino-enolate ligands are shown to give methyl methacrylate end-functionalized polyolefins.     

Bestimmung von Nickel, Kobalt, Kupfer, Eisen und Zink in Molybd?n und Wolfram

Zusammenfassung Durch Kationenaustauschtrennung wird die Summe der Spurenverunreinigungen von Molybdän bzw. Wolfram abgetrennt. Anschließend trennt man die Verunreinigungselemente durch Anionenaustauschchromatographie voneinander und bestimmt in den einzelnen Fraktionen Nickel, Kobalt, Kupfer und Eisen spektrophotometrisch sowie Zink durch inverse Voltammetrie. Die Nachweisgrenzen betragen für 0,5 g-Einwaagen 0,5 ppm Nickel, 0,5 ppm Kobalt, 0,5 ppm Kupfer, 1 ppm Eisen und 5 ppm Zink.

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Summary The sum of trace impurities in molybdenum or tungsten is separated by cation-exchange chromatography, before separating the impurities from each other by anion-exchange chromatography. In different parts of the eluate nickel, cobalt, copper, and iron are determined spectrophotometrically whereas zinc is determined by anodic-stripping voltammetry. The limits of detection are 0.5 ppm for nickel, cobalt, and copper, 1 ppm for iron and 5 ppm for zinc related to 0.5 g of molybdenum or tungsten.

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Herrn Prof. Dr. W. Geilmann zum 75. Geburtstag gewidmet.