二邻巯基苯酚-苯甲酰肼合钼(Ⅳ)酸双三乙基亚铵三元固态配合物的合成及谱学特性

以(Bu₄N)₄Mo₈O₂₆为原料,以邻巯基苯酚和苯甲酰肼为配体,在甲醇中合成了未见报道的单核三元配合物二邻巯基苯酚-苯甲酰肼合钼(Ⅳ)酸双三乙基亚铵.通过元素分析、红外光谱、¹H NMR谱、电子光谱、差热-热重分析对化合物的性质进行了表征,发现它是无端基氧钼配合物,并提出了其可能结构.     

Mo(Ⅵ)-邻羟基苄胺-N,N,O-三乙酸与Cu2+交换反应动力学研究

邻羟基苄胺-N,N,O-三乙酸(HBATA,H₃L)为1种带苯氧乙酸基团的氨羧螯合剂。我们曾报道过它的一些过渡金属络合物在溶液中的稳定性、络合物晶体结构及其与Fe(Ⅲ)的络合反应机理,并探讨了Mo(Ⅵ)、Mo(Ⅴ)与其在水溶液中的络合平衡。本文在10℃、Ⅰ=0.5mol/LNaCl、pH3.31～4.16条件下用截流分光光度法研究了Mo(Ⅵ)-HBATA络合物与Cu²⁺的交换反应动力学,并确定了反应机理。     

Electrochemical and Spectroelectrochemical Studies of Molybdenum and Neodymium Complex with Diethyld

ＥｌｅｃｔｒｏｃｈｅｍｉｃａｌａｎｄＳｐｅｃｔｒｏｅｌｅｃｔｒｏｃｈｅｍｉｃａｌＳｔｕｄｉｅｓｏｆＭｏｌｙｂｄｅｎｕｍａｎｄＮｅｏｄｙｍｉｕｍＣｏｍｐｌｅｘｗｉｔｈＤｉｅｔｈｙｌｄｉｔｈｉｏｃａｒｂａｍａｔｅＬｉｇａｎｄＹＵＺｈｅｎ－ｘｉｎｇ,ＦＵＱ...     

双显色剂高灵敏协同显色反应的研究——钼-溴邻苯三酚红-乙基紫体系

本文研究了在聚乙烯醇存在下,钼(Ⅵ)与溴邻苯三酚红和碱性染料-乙基紫产生的协同显色反应。探讨了利用协同显色反应进行分光光度测定痕量钼的可能性。在乙酸介质中,钼(Ⅵ)与溴邻苯三酚红和乙基紫形成[EV]₃[MoO₂(BPR)]离子缔合型配合物,其吸收峰位于535nm,相应试剂(BPR+EV)的吸收峰则位于640nm。摩尔吸光系数e₅₃₆=1.70×10⁵L·mol^-1·cm^-1。双峰双波长法可使灵敏度倍增。Δε_535～640=3.20×10⁵L·mol^-1。钼含量为0～0.16^μg/mL时,吸光度遵守比尔定律。桑德尔灵敏度(S)为0.00057μg/cm²。反应具有较高的选择性,除锗、钛、钨、钒有较严重干扰以外,其它常见金属离子不干扰钼的显色。根据配合物的组成,推测了它的可能结构。     

MoO3在Ga2O3上的分散研究

采用ＸＲＤ,ＬＲＳ,ＦＴ－ＩＲ,ＵＶ－ＤＲＳ和ＴＰＲ研究了ＭｏＯ３在体载体Ｇａ２Ｏ３上的分散情况。结果表明：ＭｏＯ３的分散状态受Ｇａ２Ｏ３表面结构的影响,ＭｏＯ３在Ｇａ２Ｏ３上的分散容量约为８．４μｍｏｌ／ｍ＾２;低于该分散容量时,Ｍｏ＾６＋主要以高分散态存在于Ｇａ２Ｏ３表面,而高于该分散容量时,除在分散态的Ｍｏ－Ｏ物种外,还有残余的ＭｏＯ３晶相出现。ＴＰＲ结果表明：ＭｏＯ３低于分散容量时,体系中     

庚烷与液态三氧化硫反应特性的研究

研究了庚烷与三氧化硫在1,2-二氯乙烷溶剂下的磺化反应。采用阳离子交换树脂测定反应总酸量的方法,讨论了滴加速度、反应温度、反应物浓度及其相对比例对磺化程度的影响,发现其磺化程度主要与反应物浓度、反应物相对比例有关,而阳离子树脂交换滴定测定反应总酸量的方法与传统的滴定二氧化硫的方法相比,具有简单、方便而且准确的优点。此外,还考察了其它直链饱和烷烃的磺化反应。     

Syntheses and Characterization of Molybdenum Complexes with the (1,3-Dithioliumyl)diphenylphosphine Containing Ligands

Treatment of [Et₄N][Mo(CO)₅(PPh₂CS₂)], 1 with unsaturated organic halides afforded the neutral complexes Mo(CO)₅(PPh₂CS₂R) (R = CH₂CN, 2 ; R = CH₂C≡CH, 3 ). Alkylation reactions take place at the sulfur atom. Protonation of complex 2 and 3 with HBF₄ produced the intramolecular cyclization products [Mo(CO)₅(PPh₂CS₂C₂H₃N)][BF₄], 4 and [Mo(CO)₅(PPh₂CS₂C₃H₄)][BF₄], 5 , respectively. In complex 4 and 5 , two five-membered 1,3-dithiolium rings formed. Protonation of 3 to 5 is not reversible, but deprotonation of 4 by n-BuLi or PPh₃ gave 2 quantitatively. Treatment of 4 with n-Bu₄NF yielded complex Mo(CO)₅PPh₂F, 6 and 2 with 1:1 ratio, but in the reaction of 5 and n-Bu₄NF only compound 6 was formed. All of these complexes are identified by spectroscopic methods.     

Nax/2Bi1−x/2MoxV1−xO4 and Bi1−x/3MoxV1−xO4 New Scheelite-related phases

New Scheelite-related solid solutions of the compositions Na_x/2Bi_1−x/2Mo_xV_1−xO₄ (0≤x≤1) and Bi_1−x/3 Mo_xV_1−xO₄(0≤x≤0.2) have been synthesised by the substitution of Na and Mo at the A and B sites respectively of the ABO₄ type ferroelastic BiVO₄. The phases were characterised using chemical analysis, powder X-ray diffraction, scanning electron microscopy, EDAX, and Raman spectroscopy. While almost a continuous solid solution is obtained for the series Na_x/2Bi_1−x/2Mo_xV_1−xO₄, the absence of Na at the A-site results only in a narrow stability region for the other series, Bi_1−x/3 Mo_xV_1−xO₄ where 0≤x≤0.2. Raman spectra of selected samples at room temperature also suggest that vanadium and molybdenum atoms are disordered at the tetrahedral sites.     

人体脏器中钼的石墨炉原子吸收测定方法的研究

本文讨论了用衬钽石管测定人体脏器中钼的方法。初钽管完全消除了形成稳定碳化物的影响,灵敏度较用普通石墨炉管提高约８４倍,较用热解石墨管提高了一个数量级,完全消除 记忆效应,减少了钠、钾、铁等共存元素的干扰．方法简单、准确、快速。     

Moiré pattern in LEED obtained by van der Waals epitaxy of lattice mismatched WS2/MoTe2(0001) heterointerfaces

Thin films of WS₂ have been grown by van der Waals epitaxy (vdWE) on the basal planes of 2H-MoTe₂(0001). Despite a lateral mismatch of 10.3%, epitaxial growth is achieved by metal organic vdWE (MOvdWE). In low energy electron diffraction (LEED) measurements a Moiré-like superstructure is observed originating from and correlated to the lateral mismatch between film and substrate. I–V LEED investigations in the course of sequential film growth reveal an undulation of the lattice at the interfaces as the origin of the Moiré-like structure rather than simple multiple scattering between overlayer and substrate.