二乙烯苯和丙烯腈聚合物浸渍磷酸三丁酯为固定相萃取色谱法富集分离铂与金

报道了以GDX501（二乙烯苯和丙烯腈的聚合物）型树脂浸渍磷酸三丁脂（TBP）为固定相，用萃取色谱法使微量铂、金与常见贱金属分离。富集在色谱柱上的铂与金分别用0.25mol/L HNO-0.5mol/L NaClO3溶液和0.1mol/L HCl-0.2mol/L硫脲溶液连续洗脱并用原子吸收光谱法进行测定。铂与金的回收率分别为89.5%-113.9%和90.1%-105.3%。     

The Gas Chromatographic Determination of the Decomposition Products of Tributyl Phosphate

Abstract

The products formed from tributyl phosphate in different diluents have been quantitatively analyzed for components by gas chromatography. Methylation yields and limits of detection of di butyl phosphate are given.     

磷酸三丁酯色层分离-电感耦合等离子体原子发射光谱法测定U_3Si_2中22个微量杂质元素

本法对U_3Si_2中22个微量杂质元素的测定,进行了较系统的实验研究.取样100mg时,Al、Ca、Cd、Co、Cr、Cu、Fe、Hf、In、Mg、Mn、Mo、Nb、Ni、Pb、Sn、Ta、Ti、V、Y Zn和 Zr的测定范围5μg/g~800μg/g,回收率为94%~105%,RSD(n=8)为0.4%~1.2%.     

Solvent Extraction of Pb(II) with AGDOMD

Abstract

The distribution of Pb(II) between an aqueous phase and a toluene phase containing dehydrated fatty acids found in distilled castor oil (AGDOMD) has been studied. Using the slope technique the conditional equilibrium constant of extraction was determined (kext = 1.02 × 10^?7) and the main species present in the organic phase was identified as (PbNO₃R. 2HR)_(o), where HR represents the fatty acid used.     

磷酸三丁酯—钛—钽试剂第三相的形成与应用

本文研究了强酸性介质中，磷酸三丁酯萃取体系（ＴＢＰ．ＨＡ）第三相的形成条件；探讨了ＴＢＰ．ＨＡ对钛的萃取行为；建立了ＨＣｌＯ４－Ｈ２ＳＯ４介质中，利用ＴＢＰ．ＨＡ第三相萃取，然后用ＩＣＰ－ＡＥＳ温室痕量钛的方法。结果表明，由于第三相体积小，对钛有较高的富集倍数，降低了分析的检出限，用ＩＣＰ－ＡＥＳ检测，可以消除基体及其他大部分元素对测定的干扰，测定钛的回收率在９７％－１０１％。利用本法对钢样标准物     

磷酸三丁酯萃淋树脂富集水中痕量酚类化合物的研究

本文对磷酸三丁酯（ＴＢＰ）萃淋树脂为柱填料，研究了富集水中酚类化合物及其洗脱条件。结果表明，以ＴＢＰ萃淋树脂为富集剂，水样ｐＨ值为１－７，以３０ｍｌ／ｍｉｎ的流速通过吸附柱，用８ｍｌ０．１ｍｏｌ／Ｌ的ＮａＯＨ洗脱，多种酚类化合物回收率在９７％－１０３％。此外还试验了地面水中常见干扰物的影响，该方法富集倍数达１２５倍，最低检测限０．５μｇ／Ｌ。对实际样品１－１００μｇ／Ｌ范围内的测定相对标准偏差４．     

Equilibrium and Kinetic Aspects of Hg(II) Extraction from Natural Waters with Diphenylthiocarbazone

A diphenylthiocarbazone (dithizone) based liquid-liquid extraction method of general utility is proposed for small-scale Hg(II) extraction from natural waters. The quantitative aspects related to the extraction are studied in terms of distribution of mercury dithizonate in carbon tetrachloride-water system at 293 K (20±1°C). Various distribution constants related to the reagent and the complex formed are evaluated. The equilibrium and kinetic studies of extraction and complex formation are analytically based on atomic absorption and colorimetric methods. Local natural waters were subjected to the proposed method for Hg(II) removal. The method is found to be capable of removing above 98% mercury in a single-step extraction under the conditions evaluated in terms of matrix pH, equilibration time and amount of reagent.     

三(2-苯并咪唑亚甲基)胺合锰的结构和量化计算

合成了三 ( 2 苯并咪唑亚甲基 )胺合锰 (II) (C48H5 0 N1 4 O4Mn2 Cl4) ,采用X射线单晶衍射方法测定了晶体结构 ,并进行了量子化学计算 .晶体属于单斜晶系 ,空间群P2 1 /C ,晶胞参数 :a =1 4 2 38( 7)nm ,b =2 4 80 2 ( 3)nm ,c =1 6 977( 7)nm ,β =92 51( 4)° ,V =5 9893nm3 ,Z =4 用重原子法及傅里叶合成方法解出结构 ,最终R值为 0 0 7 Mn2 处于变形三角双锥配位环境中 .量子化学计算表明配体具有负电荷空穴 ,使其易于与金属离子配位     

Synthesis,Characterization, and Crystal Structures of a New Coordination Polymer of Manganese(II) Containing Dimethyl Phosphate

The reaction of MnCl₂ with TMP (TMP = Trimethyl phosphate) in THF (THF = tetrahydroforan), led to the coordination polymer [Mn₂(μ₃‐DMP)₂(μ‐DMP)₂]_n (1) (DMP = dimethyl phosphate). This complex was characterized by elemental analysis, IR spectroscopy and single‐crystal structure of 1 . Crystal data for 1 at ?173 °C: triclinic, space group , a = 9.7071(11), b = 10.4482(11), c = 10.6242(11) Å, α = 88.892(2)°, β = 80.829(2)°, γ = 87.572(2)°, Z = 2, R1 = 0.0441.     

Bromamine-T mediated aziridination of olefins with a new polymer supported Manganese(II) complex as catalyst

Chloromethylated styrene-divinyl benzene of 8% cross-link was functionalized using o-phenylene diamine and finally it was treated with Mn(II) for the formation of metal complex on the surface. The metal content was estimated using atomic absorption spectroscopy. The thermal stability of the catalyst was seen by the use of DTA-TG analyses and the catalyst was found to be stable up to ˜125°C. The modern spectroscopic methods such as FT-IR, ESR were used in order to confirm the probable structure of the catalyst. The catalytic activity of this supported Mn(II)-complex was investigated for aziridination of olefins with bromamine-T as the source of nitrogen. The catalyst was found to be effective in this reaction and could be reused with no substantial loss of activity for up to three cycles.     

Spectrophotometric Simultaneous Determination of Zinc(II), Manganese(II) and Iron(II) in Pharmaceutical Preparations Using OSC-PLS

The purpose of this paper is to develop a fast and sensitive spectrophotometric method for the simultaneous determination of zinc(II), manganese(II) and iron(II) in pharmaceutical preparations. The method presented in this work is based on the well-known reaction of these ions with 4-(pyridylazo)resorcinol (PAR)1. The application of quantitative chemometric methods, particularly PLS to multivariate chemical data is becoming more widespread owing to the availability of digitized spectroscop…     

Complex formation of copper(II) and nickel(II) with N-arylthiopicolinamides

The reactions of N-arylthiopicolinamides (HL) with copper(II) and nickel(II) ions in organic and aqueous-organic solutions were studied. On addition of HCl, the transformation of ML₂ complexes into M(HL)Cl₂ occurs, while the reverse reaction takes place under the action of amphoteric protic solvents. The structures of the isolated complexes were established by IR and UV spectroscopy.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 1546–1550, September, 1993.     

Crystal Structure and Thermal Property of a Binuclear Manganese(II) Sulfate Complex with Carbohydrazide

The binuclear manganese(II) complex of formula [Mn₂(CHZ)₂(H₂O)₂(SO₄)₂] (CHZ = carbohydrazide) (1) has synthesized in aqueous solution and characterized by elemental analysis, IR, and single crystal X-ray diffraction. The compound 1 crystallizes in monoclinic system, space group P2(1)/n, a = 7.083(1) Å, b = 7.985(1) Å, c = 14.045(2) Å, β = 90.46(1)^°, V = 794.42(16) ų, Z = 2, R = 0.0308 with 1481 reflections. In the title complex, two Mn(II) cations are bonded via the bridging oxygen atoms into a centrosymmetric dimeric unit. The Mn(II) dimers are further extended into layers by means of the bridging sulfate groups. Each Mn atom in the complex is in bivalent state with a distorted pentagonal bipyramid configuration and has a N₂O₅ donor set which consists of two nitrogen atoms and five oxygen atoms provided by the ligands of two CHZ molecules, one water molecule, and two sulfate ions. The CHZ tridentate ligands are coordinated with adjacent Mn(II) cation via two terminal N atoms and the carbonyl O atom and sulfate anions act as bidentate bridge ligand. Four kinds of Mn(II) CHZ complex structures are compared. The thermal property of title complex was studied by using DSC and TG-DTG techniques. The results exhibit the title complex is highly stable.     

Hydrothermal synthesis,crystal structure and antibacterial studies of nickel(II) and manganese(II) complexes with ciprofloxacin

Hydrothermal treatments of ciprofloxacin with Ni(NO₃)₂·6H₂O and Mn(ClO₄)₂·6H₂O yield two metal complexes: [Ni(H-cip)₂(H₂O)₂](NO₃)₂·2H₂O (1) and [Mn(H-cip)₂(H₂O)₂] (ClO₄)₂·2H₂O (2), confirmed by elemental analysis, IR and single crystal X-ray diffraction analyses. Complexes 1 and 2 were screened for antibacterial activity against Staphylococcus aureas, E. coli, Pseudomonas aeruginos and Candidaalbicans.     

Manganese(II)-phenanthroline-azide compounds: Versatile Precursors as Ligands in Designing Heteropolymetallic Systems

Two novel manganese(II) complexes, [Mn(phen)₂N₃·H₂O]ClO₄·H₂O and Mn(phen)₂(N₃)₂ have been synthesized by the reaction of Mn(ClO₄)₂·6H₂O and Mn(CH₃CO₂)₂·4H₂O with NaN₃ and phen in EtOH/H₂O solution, respectively (where phen = 1,10-phenanthroline). Their crystal structures have been determined by X-ray diffraction. Both complex molecules have distorted octahedral geometry and two 1,10-phenanthroline molecules chelate to a Mn(II) atom with a cis-configuration. To [Mn(phen)₂N₃·H₂O]ClO₄·H₂O, one nitrogen atom from an azide anion and one oxygen atom from a water molecule cis-coordinate to the Mn(II) atom while two nitrogen atoms occupy cis positions in Mn(phen)₂(N₃)₂. These complexes are versatile precursors for the design of heteropolymetallic systems.     

Hydrothermal synthesis and crystal structures of Mn(II) and Cd(II) aminophosphonates with a layered structure

Two new divalent metal aminodiphosphonates with a layered structure, Mn₂[(HL)(H₂O)F]·H₂O (1) and Cd_3.5[(HL)L] (2) (H₄L =?CH₃CH₂CH₂N(CH₂PO₃H₂)₂), have been hydrothermally synthesized and characterized by single-crystal X-ray diffraction as well as with infrared spectroscopy, elemental analysis and thermogravimetric analysis. In 1, two MnO₄F₂ and two MnO₅F polyhedra are interconnected via edge-sharing into a tetramer, and such tetramers are bridged by the diphosphonate ligands into a Mn(II) phosphonate layer in the ab-plane. The structure of 2 also features a 2D layered structure, in which the CdO₅N and CdO₆ polyhedra are interconnected into a 1D chain. The chains are then cross-linked via phosphonate oxygen atoms to form Cd(II) phosphonate layers in the ab-plane.     

Analytical Separation of Copper(II), Cobalt(II) and Nickel(II) Using Polymer Bound Anthrantic Acid

Abstract

The preferential complexing tendency of different nietal ions towards chelating agents anchored on a polymer has been used for separation of transition metals. the anthranilic acid group was anchored on the polymeric cellulose back-bone by successive coupling with trifunctional reagent cyanuric chloride, in diozane medium, at pH 7 and 9–10, respectively. This polymer bound chelating agent was used to separate copper(II), nickel(II) and cobalt(II) in the concentration range 1.0–0.1 mmol/L. the separation of a mixture of two components was quantitative using column chromatography.     

Silica gel surface modified with sulfanilamide for selective solid-phase extraction of Cu(II), Zn(II) and Ni(II)

A new chelating matrix has been prepared by immobilising sulfanilamide (SA) on silica gel (SG) surface modified with 3-chloropropyltrimethoxysilane as a sorbent for the solid-phase extraction (SPE) Cu(II), Zn(II) and Ni(II). The determination of metal ions in aqueous solutions was carried out by inductively coupled plasma optical emission spectrometry (ICP-OES). Experimental conditions for effective sorption of trace levels of Cu(II), Zn(II) and Ni(II) were optimised with respect to different experimental parameters using the batch and column procedures. The presence of common coexisting ions does not affect the sorption capacities. The maximum sorption capacity of the sorbent at optimum conditions was found to be 34.91, 19.07 and 23.62 mg g^?1 for Cu(II), Zn(II) and Ni(II), respectively. The detection limit of the method defined by IUPAC was found to be 1.60, 0.50 and 0.61 µg L^?1 for Cu(II), Zn(II) and Ni(II), respectively. The relative standard deviation (RSD) of the method under optimum conditions was 4.0% (n = 8). The method was applied to the recovery of Cu(II), Zn(II) and Ni(II) from the certified reference material (GBW 08301, river sediment) and to the simultaneous determination of these cations in different water samples with satisfactory results.