PMBP为载体的乳状液膜提取钪的研究

研究了以１－苯基－３－甲基－４－苯甲酰基吡唑酮－５（ＰＭＢＰ）为流动载体的乳状液膜（ＥＬＭ）法提取钪，确定最佳液膜体系组成为０．４％ＰＭＢＰ－３％Ｓｐａｎ８０－５％液体石蜡－煤油－３ｍｏｌ／ＬＨＣｌ，Ｒｏｉ＝１：１（油内比）．Ｒｗｅ（水乳比）可达２０：１．用该体系对钪与混合稀土进行分离，钪的回收率可达９５．５％，分离系数β（ＳＣ／ＲＥ）＝３２．０。     

以PMBP为化学改进剂的电热蒸发／ICP—AES测定痕量钪的研究

报道了以１－苯基－３－甲基－４－苯甲酰基－吡唑酮「５」为化学改进剂的ＥＴＶ－ＩＣＰ－ＡＥＳ测定痕量钪的新方法。详细研究了属螯合在石墨炉内的形成、挥发及其影响因素；发现过量ＰＭＢＰ的存在有利于该螯合物的形成，     

用钼酸盐和罗丹明B连续光度法测定铈和钪

聚乙烯醇存在下，铈或钪钼杂多酸与罗丹明Ｂ（ＲＢ）形成离子缔合物，最大吸收均位于５７０ｎｍ，摩尔吸光系数分别为１．１６×１０＾６和５．６２×１０＾５Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，ｃｍ＾－１，０－１．２μｇ／２５ｍＬＣｅ和０－２．０μｇ／ｍＬＳｃ服从比耳定律，检测限１．５ｎｇ／ｍＬＣｅ（ｎ＝１０）和１．１ｎｇ／ｍＬＳｃ（ｎ＝９）。缔合物的摩尔比为Ｃｅ：ｍＯ：ＲＢ＝１：６：３和 Ｓｃ：Ｍｏ：ＲＢ＝１：１     

丁基罗丹明B—钼酸盐光度法连续测定铈和钪

在聚乙烯醇（ＰＶＡ）存在下，丁基罗丹明Ｂ（ＢＲＢ）分别与铈钼、钪钼杂多酸络阴离子形成离子缔合物，其最大吸收均位于５７０ｎｍ，表面摩尔吸光度分别为εＣｅ＝３．９６×１０＾６Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，εＳｃ＝４．７１×１０＾５Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，服从比耳定律范围分别为０－２４μｇ／Ｌ Ｃｅ和０－６０μｇ／ＬＳｃ，测定极限为Ｃｅ１．０μｇ／Ｌ（ｎ＝１２）和Ｓｃ１．９μｇ／Ｌ（ｎ＝１０），对     

以PMBP为萃取剂和化学改进剂/电热蒸发电感耦合等离子体原子发射光谱测定二氧化锆中痕量铕

提出了用β－二酮类试剂１－苯基－３－甲基－４苯甲酰基－吡唑酮［５］（ＰＭＢＰ）为萃取剂和 化学改进剂的电热蒸发电感耦合等离子体原子发射光谱（ＥＴＶ—ＩＣＰ—ＡＥＳ）测定高纯ＺｒＯ２ 中痕量Ｅｕ的新方法。讨论了影响Ｅｕ－ＰＭＢＰ 螯合物蒸发的主要因素。在优化实验条件下，Ｅｕ 的检出限为０．９μｇ／Ｌ，相对标准偏差为３．４％，试样分析的回收率为９４．５％～１０５．２％．     

聚乙烯醇存在下钼酸盐和罗丹明B光度法测定钪

在聚乙烯醇存在下，钪相杂多酸和罗丹明Ｂ（ＲＢ）形成离子缔合物，其最大吸收位于５７０ｎｍ，表观摩尔吸光系数ε值为５．６２×１０＾５Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，服从比耳定律范围０－１．０μｇＳｃ／２５ｍＬ，检出限１．１ｎｇ／ｍＬ（ｎ＝９），考察了５０多种外来离子影响，缔合物的摩尔组成为Ｓｃ：Ｍｏ：ＲＢ＝１：１２：６，方法用于地质样品中钪的分析，结果满意。     

铌（Ⅴ）—1—苯基—3—甲基—4—苯甲酰基—吡唑啉酮—5络合物吸附波的研究

在ｐＨ＝５．０的ＨＡｃＮａＡｃ介质中，Ｎｂ（Ⅴ）与１－苯基－３－甲基－４－苯甲酰基－吡唑啉酮－５（ＰＭＢＰ）生成络合物，于一０．９６Ｖ（ｖｓ．ＳＣＥ）出现一尖极谱波。在滴汞电极上用示波极谱仪或在悬汞电极上则吸附伏安曲线。峰电流与Ｎｂ（Ⅴ）浓度分别在０．００７５－０．８０μｇ／ｍＬ及０．００００７５－０．００７５μｇ／ｍＬ范围内呈线性关系。实验 ３     

钪—水杨醛苯甲酰腙高灵敏度荧光反应及其应用

研究了水杨醛苯甲酰腙（ＳＡＢＨ）与钪荧光反应新体系的最佳条件。在ｐＨ＝６．４乙醇／水（６．２：３．８）溶液介质中，形成络合物的组成比１：３（钪、试剂），λｅｘ／λｅｍ＝３８５ｎｍ／４５５ｎｍ，建立钪荧光分析法的线性范围为０￣１００μｇ／Ｌ；相对标准偏差１．５％；检出下限为０．０２５μｇ／Ｌ。考察了３０种共存离子的干扰情况，方法成功用于地质中样中痕量钪的测定。     

镉（Ⅱ）—1—苯基—3—甲基—4—苯甲酰基—吡唑啉酮—5配合物吸附波的研究

在ＰＨ４．８的ＨＡｃ－ＨＮ４Ａｃ介质中，Ｃｄ（Ⅱ）与１－苯基－３－甲基－４－苯甲酰基－吡唑啉酮－５（ＰＭＢＰ）生成配合物，于－０．６７Ｖ（ｖｓ．ＳＣＥ）出现一尖锐、灵敏的极谱波。镉含量在０．００１－１．０μｇ／ｍＬ范围内与峰高成线性关系。     

镉（Ⅱ）－1－苯基－3－甲基－4－苯甲酰基－吡唑啉酮－5配合物吸附波的研究

在ｐＨ４．８的ＨＡｃ－ＮＨ＿（４）Ａｃ介质中，Ｃｄ（Ⅱ）与１－苯基－３－甲基－４－苯甲酰基－吡唑啉酮－５（ＰＭＢＰ）生成配合物，于－０．６７Ｖ（ｖｓ．ＳＣＥ）出现一尖锐、灵敏的极谱波。镉含量在０．００１～１．μｇ／ｍＬ范围内与峰高成线性关系。用多种电化学方法研究了极谱波的性质及电极反应机理，证明－０．６７Ｖ处的极谱波为配合物吸附波，峰电流由中心离子Ｃｄ（Ⅱ）还原产生。配合物组成为Ｃｄ（Ⅱ）：ＰＭＢＰ＝１：１。试验了３０多种离子对峰电流的影响，用ＳｒＳＯ＿４共沉淀分离Ｐｂ（Ⅱ），再经巯基棉分离其它干扰离子。用于矿样中镉的测定，结果满意。     

Zwei neue Ammoniakate des Scandiumtrichlorides,ScCl3(NH3) und ScCl3(NH3)2

Two New Ammoniates of Scandium Trichloride, ScCl₃(NH₃) and ScCl₃(NH₃)₂ Reactions of scandium with ammonium chloride in the presence of cupric chloride in sealed copper ampoules yield colorless single crystals of the two new ammoniates of scandium trichloride, ScCl₃(NH₃) und ScCl₃(NH₃)₂. The crystal structures were determined from single crystal data; they both crystallize with the triclinic crystal system. In ScCl₃(NH₃)₂ isolated unsymmetrical dimers of double octahedra, according to [Sc‐mer‐(NH₃)_3/1Cl_1/1Cl_(2/2)×2Sc(NH₃)_1/1Cl_3/1] are the characteristic structural features. The crystal structure of ScCl₃(NH₃) also contains double octahedra, [Sc(NH₃)_2/1Cl_2/1Cl_2/2]₂; these dimers are, however, connected via common edges forming infinite zig‐zag chains according to the formulation [Sc(NH₃)_1/1Cl_1/1Cl_4/2].     

A Study on the Fluorescence System of Sc-BPMPHD-CTMAB and Its Analytical Application

IntroductionThe fluorescence of Sc(3+) itself in solution is not observed. After complexed with an organic ligand with a chromophore, Sc(3+) makes the ligand, which has no or has weak fluorescence, emit strong fluorescence. The fluorescence reagents of Sc~(3+) have been summarized inreferences[1,2], but the derivative of diacylated pyrazolone as a fluorescence reagent of Sc~(3+) hasnot been reported. The experiments indicated that the synthetic derivative of diacylated pyrazolone, 1, 6-bi (1…     

CTMAB存在下钪多元络合物的研究

本文系统研究了在阳离子表面活性剂存在下钪与溴邻苯三酚红及三乙烯四胺形成多元络合物的条件，测定了络合物的最大吸收波长和摩尔吸光系数，确定了络合物的组成。并初步探讨了反应机理。     

Synthesis,Characterization, and Syndio‐Specific Styrene Polymerization of Pyrrolyl‐Substituted Cyclopentadienyl Scandium Complexes

Acid‐base reaction of Sc(CH₂C₆H₄NMe₂‐o)₃ with 1 equiv. of pyrrolyl‐substituted cyclopentadienyl ligand C₄H₂Me₂NSiMe₂C₅Me₄H in toluene gave the half‐sandwich scandium bis(aminobenzyl) complex (C₄H₂Me₂NSiMe₂C₅Me₄)Sc(CH₂C₆H₄NMe₂‐o)₂ ( 2 ). Amine elimination between Sc[N(SiHMe₂)₂]₃(THF) and one equivalent of C₄H₂Me₂NSiMe₂C₅Me₄H afforded the scandium bis(silylamide) complex (C₄Me₂H₂NSiMe₂C₅Me₄)Sc[(NSiHMe₂)₂SiMe₂](THF) ( 3 ). Both scandium complexes 2 and 3 were characterized by elemental analysis, NMR spectroscopy, and single‐crystal X‐ray diffraction. 2 and 3 could serve as highly active precursors for styrene polymerization to give syndio‐tactic polystyrene (rrrrrr > 99 %).     

Formation of scandium carbides and scandium oxycarbide from the elements at high-(P, T) conditions

Synchrotron diffraction experiments with in situ laser heated diamond anvil cells and multi-anvil press synthesis experiments have been performed in order to investigate the reaction of scandium and carbon from the elements at high-(P,T) conditions. It is shown that the reaction is very sensitive to the presence of oxygen. In an oxygen-rich environment the most stable phase is ScO_xC_y, where for these experiments x=0.39 and y=0.50-0.56. If only a small oxygen contamination is present, we have observed the formation of Sc₃C₄, Sc₄C₃ and a new orthorhombic ScC_x phase. All the phases formed at high pressures and temperatures are quenchable. Experimentally determined elastic properties of the scandium carbides are compared to values obtained by density functional theory based calculations.     

钪—偶氮氯膦Ⅲ—铜—邻菲罗啉混合多核配合物显色反应研究

本文研究了钪—偶氮氯膦Ⅲ—铜—邻菲罗啉配合物的形成条件。在pH3.6醋酸钠—盐酸介质中配合物的最大吸收峰在606nm处,摩尔吸光系数ε_(606)=7.02×10~(-4)L·mol~(-1)·cm~(-1)。配合物各组分摩尔比Sc∶R ∶Cu∶Phen=1∶1∶1∶3。分子式为[ScOH·H_4R][Cu(Phen)_3]。应用于以铜基合金合成试样中钪的直接测定,结果较好。     

钪-铬天青S-铜-邻菲啰啉混合多核络合物显色反应的研究

本文研究了钪-铬天青S-铜-邻菲啰啉(Sc-CAS-Cu-Phen)络合物的形成条件.在pH=5.5～6.1的酸度范围内络合物最大吸收峰在625nm,表观摩尔吸光系数占ε_(625)=6.52×10~4L·mol~(-1)·cm~(-1).其组成摩尔比为Sc:CAS:Cu:Phen=2:6:3:9.相应分子式为[Sc(CAS)_3]_2[Cu(Phen)_3]_3。应用于以铜基合金合成试样中钪的直接测定,结果较好.