电感耦合等离子体光谱法测定镍基高温合金中的硅、锰、磷

建立了电感耦合等离子体光谱测定镍基高温合金中硅、锰、磷元素的方法,优化了试样前处理方法,对前处理所用酸的酸度进行不同比例试验,确定了仪器测量条件及分析谱线.在一定浓度范围内,各元素的浓度与谱线强度呈线性关系,相关系数大于0.9999.加标回收率为93.3%～106.7%,测定结果的相对标准偏差小于3.0%(n=10)....     

电感耦合等离子体发射光谱法测定铝合金中硅、锰、铬

采用电感耦合等离子体发射光谱法测定铝合金中杂质元素硅、锰、铬的含量.以盐酸溶液(1+1)和过氧化氢溶解样品,选择各元素灵敏度较强、光谱干扰较小的波长作为分析线.3种杂质元素的发射强度与其质量浓度在20.00 mg/L以内呈线性关系,方法的检出限为0.0016～0.015 mg/L,测定结果的相对标准偏差为1.10％～2...     

SYNTHESIS,CRYSTAL STRUCTURE AND MAGNETIC PROPERTIES OF A MANGANESE(III) COMPLEX WITH SALICYLATE AND IMIDAZOLE LIGANDS

Abstract

A new manganese(III) complex [HimH][Mn(sal)₂(imH)₂]CH₃OH (sal = salicylate, C₇H₄O₃ ^2-; imH = imidazole, C₃H₄N₂; [HimH]⁺ = imidazole cation (C₃H₅N₂) has been prepared and characterized by X-ray analysis and magnetic measurements. The compound crystallizes in the monoclinic space group P2 ₁ with a = 9.931(2), b = 10.237(1), c = 12.926(7) Å, β = 102.740° and Z = 2. The structure has been refined to R = 0.030 and R_w = 0.031. The Mn(III) ion has elongated octahedral coordination with mutually trans imidazoles occupying axial sites. The equatorial plane is defined by four O atoms of two salicylates. Each [HimH]⁺ cation (imidazolium) is associated with two complex anions through hydrogen bonds as an imidazolium bridge. The variable temperature magnetic susceptibility for the complex in the temperature range 77-300 K has been interpreted in terms of a single-ion zero-field splitting model with a molecular field term correction. The values obtained for D, g. and zj' are -6.93 cm^?1, 2.00 and -0.90 cm^?1.     

SYNTHESES,CRYSTAL STRUCTURES AND ANTIBACTERIAL ACTIVITIES OF MONONUCLEAR NICKEL(II) COMPLEXES WITH SIMILAR SCHIFF BASES

Journal of Structural Chemistry - Two mononuclear nickel(II) complexes, [Ni(L1)2] (1) and [Ni(L2)2] (2), where L1 and L2 are the anions of 4-methylbenzoic acid (1-pyridin-2-ylmethylidene)hydrazide...     

丙氨酸－N－荒酸镍与稀土多核配合物的合成、表征和抗癌、抑菌活性研究

本文报道了稀土与丙氨酸－Ｎ－荒酸镍［Ｈ２ＮｉＬ２］多核配合物的合成和表征。通过元素分析确定配合物的组成为ＲＥ２（ＮｉＬ２）３·ｘＨ２Ｏ（ＲＥ＝Ｌａ、Ｎｄ、Ｓｍ－Ｅｒ、Ｙｂ；ｘ＝１、４、８），并研究了配合物的摩尔电导、红外光谱和核磁共振氢谱。配合物体外抗癌活性及抑菌活性的测定结果表明，丙氨酸－Ｎ－荒酸镍及其稀土多核配合物均具一定的抗癌、抑菌活性。     

2,2,4,13,13,15,—六甲基—1,5,12,16—四氮杂环二十二烷—N′,N″′—二乙酸及其镧系配合物的合成和表征

本文合成了题头所示大环配体,并制备了它的十四种镧系元素(La～Lu,Pm除外)固体配合物。用元素分析,DTA-TG,红外光谱以及电导测定等手段研究了这些化合物的组成和性质.基于这些分析结果可建议配合物化学式为Ln(H_2L)(NO_3)_3·nH_2O。     

SEPARATION OF IRON AND MANGANESE IN THE EARLY DIAGENETIC PROCESSES AND ITS MECHANISM OF BIOGEOCHEMISTRY

Study shows that the reduction of iron (Fe~(3+)) and manganese (Mn~(4+)) in modern sedi-ments and the diffusive flux of the Mn~(2+) from the pore water into the overlying waterare mainly controlled by bacteria, and the distribution of the bacteria is believed to beaffected strongly by the sedimentary environment. It is the diffusive fluxes between Fe~(2+)and Mn~(2+) that lead to the separation of iron and manganese in the modern sediment at theChangjiang Mouth and near the shore. The level of the separation decreases with theincrease of the overlying water salinity and increases from the surface to the depth. Thismechanism has given a new explanation why manganese is concentrated in sediments onthe oceanic floor of ferromanganese-rich nodules.     

SAPO-5分子筛中硅的取代及其性能研究

本文采用三乙胺为模板剂,用水热法合成不同含硅量的SAPO-5分子筛,并用X射线衍射、扫描电镜、电子探针分析、真空重量吸附等方法对其进行了表征,结果表明硅已进入了骨架,硅同晶非等比取代磷和铝,并且分子筛的孔道是畅通的。 用微型反应器测定了AlPO₄-5及不同量硅取代的SAPO-5分子筛上的异丙苯裂解和邻二甲苯异构化催化反应,结果表明Si引入了催化活性很低的磷酸铝骨架后使其催化活性明显增加,进一步证实了硅是同晶非等比取代磷和铝,因而使分子筛骨架带负电性。 硅进入磷酸铝分子筛骨架的SAPO-5分子筛经红外光谱实验发现不仅具有表面羟基,而且都是酸性羟基。吸附吡啶后的红外光谱结果表明SAPO-5上同时存在B酸和L酸中心,B酸中心数目随着硅含量的增加而增加。     

间羟基苯甲酸邻菲啰啉稀土三元配合物的合成、表征和抗菌活性研究

本文用间羟基苯甲酸、邻菲口罗啉与碳酸稀土合成了四种新的固体三元配合物,通过元素分析、摩尔电导、红外光谱、Ｘ射线粉末衍射、差热－热重分析等手段,确定配合物的组成为：Ｌｎ（ｐｈｅｎ）Ｌ３,（Ｌｎ＝Ｌａ,Ｇｄ,Ｄｙ,Ｙ;Ｌ＝ｍ－ＨＯ－Ｃ６Ｈ４ＣＯＯ－）,并对配合物的某些性质进行了研究。     

Mn—CAS—phen—CTMAB四元络合物光度法测定微量锰

表面活性剂和多元络合物在吸收光度法中的应用,可以大大地提高测定的灵敏度,增强选择性,令人瞩目,应用很多,已有不少评述和报导[1-3]。有关锰铬天青S邻菲口罗啉溴化十六烷基三甲基铵(MnCASphenCTMAB)四元络合物的形成及其分析应用已有报导:“该绿色的四元络合物在pH=10.2...     

β-二酮缩β-丙氨酸希夫碱的锰(Ⅲ)配合物

合成了锰(Ⅲ)的双核配合物Mn_2(Hacala-β)_2(O_2CMe)_4和三核配合物Mn_3O(bzala-β)_2(O_2CMe)_3·4H_2O,其中Hacala-β~-和bzala-β~(2-)分别是乙酰丙酮缩β-丙氨酸和苯甲酰丙酮缩β-丙氨酸希夫碱负离子。用电导率、磁化率、热分析、红外及紫外可见光谱等对它们的结构和性质进行了研究。     

2, 2, 4, 13, 13, 15, —六甲基—1, 5, 12, 16—四氮杂环二十二烷—N′, N″′—二乙酸及其镧系配合物的合成和表征

本文合成了题头所示大环配体,并制备了它的十四种镧系元素(La～Lu,Pm除外)固体配合物.用元素分析,DTA-TG,红外光谱以及电导测定等手段研究了这些化合物的组成和性质.基于这些分析结果可建议配合物化学式为Ln(H₂L)(NO₃)₃·nH₂O.     

SYNTHESIS,CHARACTERIZATION AND SOLUTION CHEMISTRY OF NEW Re(V) DIOXO COMPLEXES

Abstract

In this work, we report the synthesis, characterization and potentiometric studies of new Re(V) complexes of general formula [ReO₂(amine)₂]⁺ (amine = 1,2-diaminopropane, 1,4-diaminobutane, N,N′-diethylethylenediamine, diethylenetriamine, triethylenetetramine and N-tris(2-aminoethyl)amine). Compounds were prepared starting from [ReO₂I(PPh₃)₂] and characterized by several techniques. The presence of different substituent groups in the diamines (including alkyl and amine groups) allows the presence of pendant arms. When these groups are free amino groups, they can react with acids such as H⁺ and M²⁺ cations and studied by potentiometry. The formation of very stable binuclear species was demonstrated.     

SYNTHESIS,CHARACTERIZATION AND STRUCTURAL ANALYSES OF THREE LANTHANIDE CYANIDE-BRIDGED COMPLEXES

Abstract

Three lanthanide (Ln) complexes (DMF)₄(H₂O)₃LnFe(CN)₆ · H₂O, where Ln = Er, Yb, and Lu, were structurally determined by means of three-dimensional single-crystal X-ray diffraction analysis. These systems crystallize in the centrosymmetric monoclinic space group P2₁/c (No. 14) with Z = 4 and respective lattice constants of a = 13.956(2), 13.952(1), 13.937(3); b = 8.867(4), 8.864(1), 8.862(2); c = 24.857(3), 24.812(2), 24.770(5) Å; and β = 96.30(1)°, 96.33(1)°, 96.30(3)°. Final least-squares full-matrix refinements based on 3499, 3367, and 2555 unique reflections yielded reliability (R) index factors of 0.071, 0.051, and 0.032, respectively. In each complex, the coordination about the central Ln ion is eight in a square-antiprism arrangement and the coordination about the Fe ions is six, oriented octahedrally. Cyanide bridging links the Ln ions to the FeC₆ groups. Molecules in the crystal lattice of each complex are held together by van der Waals forces and a network of hydrogen bonding. Characterization includes physical property determinations, conoscopical studies, thermal gravimetric analyses, and IR spectrometric identifications. Selected bond lengths and angles are tabularized and a synthesis of these compounds is presented.     

新型过渡金属硅基化合物的合成、表征及反应性

在这篇综述中,我们将简要地介绍我们在新一类的金属硅基化合物(RCH₂)₃MSiR′₃(M=Ti, Zr), (RCH₂)₂Ta(=CHR)SiR′₃和(RCH₂)₂W(≡CR)SiR′₃方面的工作,并讨论亚烷基、氨基化合物与硅烷之间的反应。这些研究具有以下的两重意义：(1)探索从分子前体形成金属硅化物的机理。(2)研究新一类金属硅基化合物的合成、结构及它们与硅烷的反应性。我们还通过对烷基和硅基配体在形成亚烷基配合物时不同的反应机理的研究来比较元素碳和硅之间的反应性。在这方面的研究中,我们发现“(RCH₂)₂Ta(=CHR)Cl”为在(RCH₂)₃TaCl₂和Li(THF)₃SiR₃的反应中形成硅基亚烷基化合物(RCH₂)₂Ta(=CHR)SiR₃(R=SiMe₃)的中间体而Ta(CH₂R)₅(R=CMe₃, SiMe₃)则是从(RCH₂)₃TaCl₂生成烷基亚烷基化合物(RCH₂)₃Ta=CHR的中间体。除此之外,金属氨基(M-NR₂)化合物与硅烷之间的反应被证明可以可逆地生成氨基氢化物和氨基硅烷。我们将一并讨论这一结果对于阐明金属硅化物和M-Si-N三元体系物质的形成机理的意义。     

THE SYNTHESIS AND CHARACTERIZATION OF A NOVEL vic-DIOXIME AND ITS MONO AND TRINUCLEAR COMPLEXES CARRYING A TRIOXADITHIA MACROCYCLE

Abstract

A new vicinal dioxime, l,15-bis(hydroxyimino)-2,14-dithia-5,8,11-trioxacyclopentadecane (H₂L) was synthesized by the reaction of (E,E)-dichloroglyoxime (1) with 1,11-dithio-3.6.9-trioxaundecane (2). Mononuclear copper(II) complexes with a metal/ligand ratio of 1/2 were prepared. The two ligands coordinate to copper(II) through the deprotonated oximate oxygens which then afford the trinuclear structure bridged by the oximate groups with 1,10-phenan-throline or 2,2′-dipyridyl as the end-cap ligand.     

RECENT DEVELOPMENTS IN THE METALLOSUPRAMOLECULAR AND MOLECULAR STRUCTURES OF THE COBALT,IRON AND VANADIUM COMPLEXES OF THE DIANIONIC TETRADENTATE SCHIFF BASE LIGANDS OF SALICYLIDENEIMINE AND ACETYLACETONEIMINE

Abstract

Four different types of metallosupramolecular structures are distinguishable for the title complexes. These types are described as: (a) The metal complex could react with other metal ions as a ligand, (b) Dimerization occurs through Lewis acid and Lewis base interactions of the metal ion and the coordinated oxygen atom of the ligand with those of an adjacent molecule, (c) Dimerization and chain formation occur using the donor-acceptor behaviour of the oxovanadium (IV) ion, and (d) Molecular association occurs through the bridged fluoride. Types (b), (c) and (d) are self-assembly. Chemical understanding of those types could lead to designing, and establishing procedures for, the preparation of new metallosupramolecular structures of homo- and heterobinuclear (as well as polynuclear) metal complexes with similar or mixed ligands.     

ZINC(II), CADMIUM(II), MERCURY(II) AND LEAD(II) SEMIQUINONE-TYPE COMPLEXES OF A NEW SCHIFF-BASE LIGAND: ANTIBACTERIAL STUDIES

Abstract

A new Schiff-base ligand LH₂, has been prepared by reaction of 2,9-diformv 1-1,10-phenan-throline with 2,3-diamino-l,4-naphthoquinone. The formation and characterization of complexes of Zn(II), Cd(II), Hg(II) and Pb(II) with the semi-oxidized ligand LH is described. The M(LH)X₂ (X = CI, Br and AcO) radical species are paramagnetic and the observed EPR signals in the solid state at room temperature, with g values close to the electron free g value are proof of the semiquinonic character of the ligand. The antibacterial activity of the ligand and the metal complexes prepared were tested against four bacteria strains and compared with the activity of penicillin.