螯合树脂富集—激光气化等离子体发射光谱测定地质样品中铂族元素和金

采用含Ｎ，Ｓ功能团的螯合树脂ＹＰＡ４富集铂族元素和金。Ａｕ，Ｐｔ，Ｐｄ，Ｏｓ的吸附率为９８％以上，Ｉｒ为９２％，Ｒｕ为９０％，Ｒｈ为８７％。把树脂灰化，用激光将其灰份气化输入等离子体激发，光谱测定。取样５ｇ时，可测定０．２ｎｇ／ｇ的Ａｕ，０．６ｎｇ／ｇ的Ｏｓ，Ｉｒ，０．０６ｎｇ／ｇ的Ｐｔ，Ｐｄ，Ｒｈ，Ｒｕ。标样分析结果与标准植吻合。     

以新指示反应高敏催化光度测定痕量钌

钌（Ｒｕ￣Ⅲ）对高碘酸钾氧化无色孔雀绿的显色体系有催化作用，借此催化光度测Ｒｕ￣Ⅲ，灵敏度高。在２０～３０℃下３０～６０ｍｉｎ内，以１ｃｍ吸收池内测得吸光度０．１为可准确测极限，则可测最低浓度为０．０８ｎｇ·ｍＬ￣（－１），若表示为间接摩尔吸光系数则 ＝２．０×１０￣８ｍｏｌ￣（－１）·Ｌ·ｃｍ￣（－１）。工作曲线线性范围为０．０４～０．３６ｎｇ／ｍＬ（室温约为２６℃）．其它贵金属如Ｏｓ￣Ⅷ、Ｒｈ￣Ⅲ、Ａｕ￣Ⅲ、Ａｇ￣Ⅰ、Ｐｄ￣Ⅱ、Ｐｔ￣Ⅳ等至少可允许分别存在２００ｎｇ／ｍＬ、１ｎｇ／ｍＬ、２００ｎｇ／ｍＬ、３０００ｎｇ／ｍＬ、２５ｎｇ／ｍＬ和５ｎｇ／ｍＬ。测定了含所有贵金属和某些其它常见金属人工混合液中的痕量Ｒｕ￣Ⅲ，不含Ｉｒ￣Ⅳ时回收率为９８．５％～１０１．０％，含２．３倍于Ｒｕ￣Ⅳ重量的ｌｒ￣Ⅳ时回收率为１０１．５％～１１２％。     

4─氨基─1，2，4─三氮唑树脂对Ir（Ⅳ）和Ru（Ⅳ）的吸附行为

４－氨基－１，２，４－三氮唑树脂（４—ａｍｉｎｏ—１，２，４—ｔｒｌａｚｏｌｅｒｅｓｉｎ，４－ＡＴＲ）功能基含量３．７６ｍｍｏｌ／ｇ４—ＡＴＲ。它对Ｉｒ（Ⅳ）、Ｒｕ（Ⅳ）的吸附容量分别为５３５（２．７８），３８６（３．８２）ｍｇ／ｇ４—ＡＴＲ（ｍｍｏｌ／ｇ４—ＡＴＲ）；吸附摩尔比分别为０．７４，１．０２（离子／功能基）．４—ＡＴＲ对Ｉｒ（Ⅳ）、Ｒｕ（Ⅳ）的表观吸附活化能分别为１３±２，１９±４ＫＪ／ｍｏｌ；吸附热焓分别为４０±９，２１±７ＫＪ／ｍｏｌ。在Ｉｒ（Ⅳ）、Ｒｕ（Ⅳ）、Ｒｈ（Ⅲ）、Ｆｅ３＋、Ｃｏ２＋、Ｎｉ２＋、Ｃｕ２＋共存的溶液中，４—ＡＴＲ对Ｉｒ（Ⅳ）、Ｒｕ（Ⅳ）、Ｒｈ（Ⅲ）有良好的选择吸附性．树脂吸附Ｉｒ（Ⅳ）、Ｒｕ（Ⅳ）前后红外谱图的变化表明功能基与金属离子形成配合物．     

4—氨基—1,2,4—三氮唑树脂对Ir（IV）和Ru（IV）的吸附行为

４－氨基－１，２，４－三氮唑树脂（４－ａｍｉｎｏ－１，２，４－ｔｒｉａｚｏｌｅ ｒｅｓｉｎ，４－ＡＴＲ）功能基含量３．７６ｍｍｏｌ／ｇ４－ＡＴＲ。它对Ｉｒ（Ⅳ）、Ｒｕ（Ⅳ）的吸附容量分别为５３５（２．７８），３８６（３．８２）ｍｇ／ｇ４－ＡＴＲ（ｍｍｏｌ／ｇ４－ＡＴＲ）；吸附摩尔比分别为０．７４，１．０２（离子／功能基）。４－ＡＴＲ对Ｉｒ（Ⅳ）、Ｒｕ（Ⅳ）的表观吸附活化能分别为１３±２，１９±４Ｋ     

溶剂浮选—偏最小二乘回归光度法测定地质样品痕量贵金属元素

研究了贵金属Ｒｕ、Ｒｈ、Ｐｄ、Ａｕ－ＳｎＣｌ２－ＲＢ体系及缔和物溶剂浮选的条件,采用偏最小二乘回归法对重叠光谱进行解数据处理。对地质样品Ｒｕ、Ｒｈ、Ｐｄ、Ａｕ同时测定,相对误差小于１１．１％,标准差为０．００６２－０．０１９。     

用刚果红离子缔合负载形成树脂分离Rh,Ir,Pt,Pd,Au的研究

研究了锇铱矿的锇钌蒸残液中Ｒｈ、Ｉｒ、Ｐｔ、Ｐｄ、Ａｕ的分离条件。于ｐＨ１．０的ＨＣｌ介质中将贵金属吸附于刚果红负载形成树脂上，以分离贵贱金属。然后用０．５ｍｏｌ／ＬＨＣｌ洗脱Ｒｈ；３ｍｏｌ／ＬＨＣｌ洗脱Ｉｒ；０．５％的ＮａＳＣＮ－０．１ｍｏｌ／ＬＨＣｌ洗脱Ｐｔ；５ｇ／Ｌ硫脲－０．１ｍｏｌ／ＬＨＣｌ洗脱Ｐｄ；５０ｇ／Ｌ硫脲－０．１ｍｏｌ／ＬＨＣｌ洗脱Ａｕ。洗脱顺序是Ｒｈ＞Ｉｒ＞Ｐｔ＞Ｐｄ＞Ａｕ。这五种贵金属的回收率在９５％～１０１％之间。     

高效液相色谱-荧光检测法测定葡萄酒中总亚硫酸盐

建立了测定葡萄酒中总亚硫酸盐的高效液相色谱方法。Ｎ －（９－吖啶基）马来酰亚胺与样品中亚硫酸盐反应生成一种较强的荧光络合物,利用荧光检测器进行检测。方法具有样品用量少、操作简便、灵敏度高等特点,回收率为９８．０％ ～１０３．０％ ,相对标准偏差小于４．６％ 。     

安替比林基重氮氨基-2,4-二硝基苯与银(Ⅰ)的显色反应及其应用

本文报道了安替比林基重氮氨基－２，４－二硝基苯（ＡＰＤＮＢＴ）与银（Ⅰ）的显色反应．在吐温－８０存在下，ｐＨ＝９．０～１０．０的范围内，试剂与银（Ⅰ）形成２∶１的配合物；配合物对试剂的最大吸收在４８５ｎｍ处，ε为７．２×１０４Ｌ－１·ｍｏｌ·ｃｍ－１；提出了消除阳离子干燥的银镜分离法；方法用于测定合成试样及照相显影液中银的含量，回收率为９６～１０３％，相对标准偏差小于２．０％．     

钌系双组分催化剂上α,ω—二元羧酸单酯加氢合成ω—羟基羧酸酯的研究

在小型高压反应釜中，研究了钌系双组分催化剂对α，ω－二元羧酸单酯加氢生成ω－羟基羧酸酯的催化性能，结果表明，Ｒｕ－Ｒｅ及Ｒｕ－Ｍｏ双组分催化具有良好的催 氢性能，α，ω十五一酸单甲酯在Ｒｕ－Ｒｅ以及Ｒｕ－Ｍｏ双组分催化剂另氢，生成ω－羟基十五烷酸甲酯的收率分别为８９．０％和７１．０％，反应温度对α，ω二元羧酸单酯加氢生成ω－羟基羧酸酯的收率有较大的影响。     

高效液相色谱法分析精对苯二甲酸中的微量杂质

应用高效液相色谱法,采用阴离子交换键合固定相,以磷酸盐缓冲溶液为流动相,ＵＶ２５４ｎｍ检测,外标法定量,同时测定了精对苯二甲酸（ＰＴＡ）中的主要杂质４－羧基苯甲醛（４－ＣＢＡ）和对甲基苯甲酸（ｐ－ＴＯＬ）的含量,４－ＣＢＡ和ｐ－ＴＯＬ的回收率分别为９８．３％～１０５．０％和９６．０％～１０３．８％,变异系数分别小于１．７％和３．３％。方法快速、准确,用于实际样品分析可得到满意的结果。     

燃烧过程中碱/碱土金属对重金属迁移转化影响的研究进展

碱/碱土金属广泛存在于各种固体燃料中，在燃烧过程中碱/碱土金属与燃料中重金属及其他矿物发生复杂的物理化学反应，从而影响重金属的迁移和转化。本研究主要介绍了碱/碱土金属对As、Se、Pb和Cr四种重金属迁移转化的影响规律，包括碱金属和碱土金属对重金属迁移转化的影响，颗粒物团聚与黏结对重金属排放的影响三个方面。碱/碱土金属能够抑制重金属的挥发：碱金属与Cl元素的结合，降低了PbCl₂的生成；碱金属的存在有利于提升高岭土对Pb的吸附效率；碱/碱土金属可以与As和Se形成稳定的化合物。但同时需要注意碱/碱土金属与Cr的部分结合产物中，Cr以六价态存在，具有较高的毒性。碱/碱土金属对于团聚现象发生，分别起到了促进和抑制作用，适当含量的碱金属有利于减少重金属的释放。通过总结碱/碱土金属对重金属迁移转化的影响规律，以期为降低重金属的危害提供思路。     

二元合金Ag_(50)Rh_(50)从液态到非晶的分子动力学计算

本文对贵重金属银铑合金Ag50Rh50的液态结构和激冷过程进行了分子动力学模拟研究原子间作用势采用紧束缚势模拟在施加了周期性边界条件的常压状态下进行。采用了偶关联函数、键对分析技术和键取向序参数以分子动力学模拟计算方法揭示了Ag50Rh50的液态结构存在原子偏聚特征以及在快速凝固过程形成原子偏聚的不均匀非晶并与同族过渡金属进行了非晶形成能力的比较。     

Utilization of olive pomace in nano MgO modification for sorption of Ni(II) and Cu(II) metal ions from aqueous solutions

Magnesium oxide nanoparticles were synthesized and modified by olive pomace (NMOOP700) as a novel sorbent and characterized using Fourier Transform Infrared Spectra, Scanning Electron Microscope, Transmission Electron Microscope, X-ray Diffraction, Differential Thermal Analysis and Thermal Gravimetric Analysis. Sorption of Cu (II) or Ni (II) ions were achieved taking into account important parameters including initial pH of the medium, contact time, initial metal ion concentration and temperature. A comparative study between Magnesium oxide nanoparticles and NMOOP700 material for the sorption of Cu (II) or Ni (II) ions was implemented. The obtained data revealed that the sorption process is significantly improved using NMOOP700. The monolayer capacity of Ni (II) and Cu (II) metal ions on NMOOP700 at pH 5 were found to be 149.93 ± 4.4 and 186.219 ± 6.3 mg/g, respectively. Findings of the present work highlight the potential use of NMOOP700 as a novel and effective sorbent material for the removal of Cu (II) or Ni (II) ions from the liquid phase.     

Solution extraction of transition and post-transition heavy and precious metals by chelate and macrocyclic ligands

This review focuses on compounds and methods that can be used for the extraction and separation from solution of two classes of elements that we define as heavy metals and precious metals. These elements are often targeted because they are toxic, costly, and their coordination chemistry has already been well studied, and because there is a need to develop methods of economically extracting, separating and recovering them from waste sites. This review outlines possible strategies that can be used, and reviews the present literature regarding the available methods for their extraction.     

The Cadmium Oxide Route to Alkali Metal Oxometallates with Uncommon Structural Features

The aim of this research report is to give an introduction to a specific solid state reaction applied in the field of alkali metal rich transition metal compounds. The approach is an explorative investigation of the oxidation of transition metals with CdO in the presence of alkali metal oxides and / or compounds with complex anions such as Na₂SO₄. Thereby, a range of unusual compounds have been obtained and structurally characterized. In particular, low valences and uncommon coordination numbers (C.N.) of the late 3d transition metals, as well as interesting varieties in the anionic part of the structures are accessible. The presented examples were selected mainly in order of their inherent aspects concerning the reactivity, structural features or electronic structures.     

Monitoring and statistical evaluation of heavy metals in airborne particulates in Cairo, Egypt

Airborne particulate material was monitored as total suspended particles and particulate matter less than 10 μm at selected sites in Cairo. The selected sites represent heavily industrial and industrial–residential areas of Cairo, Egypt. The filters were further analyzed for lead, cadmium, zinc and nickel using ion chromatography. The chosen method was modified to improve resolution and decrease the retention time. The data obtained were treated statistically using one-way analysis of variance and correlated with the anthropological and industrial activities of the sites. The concentrations of the heavy metals are studied in terms of particle size, time dependence, and safety.     

Response of polyacrylamide—acyclic poly(oxyethylene)-coated ion-selective electrodes to alkali and alkaline earth metal ions in propylene carbonate and its thermodynamic application

The response of ion-selective electrodes with a membrane of polyacrylamide (PAA) coupled to acyclic poly(oxyethylene) neutral carriers to lithium, sodium, potassium, magnesium and barium ions in propylene carbonate (PC) was investigated. Tetraethylene glycol monododecyl ether (POE4) and hexaethylene glycol monododecyl ether (POE6) were used as the acyclic poly(oxyethylene). Both the PAA-POE4 and the PAA-POE6 electrodes showed a more rapid dynamic response in PC than that in acetonitrile. Nernstian responses to lithium, magnesium and barium ions were obtained with the PAA-POE4 electrode. The selectivity coefficients, logk_Ba²⁺,M^x+, for lithium, sodium, potassium and magnesium ions vs. barium ion obtained in PC with the PAA-POE4 electrode were 3.6, 0.23, 0.02 and 1.1, respectively. The PAA-POE4 electrode was applied to obtain the successive formation constants of the barium ion in PC with N, N-dimethylacetamide (DMA). From the successive formation constants obtained in PC-rich solutions, the Gibbs free energies of transfer of the barium ion from PC to DMA and to PC-DMA mixtures were calculated. The electrode was also used to obtain directly the Gibbs free energies of transfer of the barium ion from PC to PC-DMA mixtures. The calculated values of the free energies were in good agreement with the values obtained experimentally, suggesting that the electrode responded to variations in solvation energy for the barium ion.     

水溶性环境友好型防锈剂的研制

为了克服目前水溶性防锈剂防锈效果差、含亚硝酸盐等有毒物质,以及成本较高、污染较严重等缺点,本文以三乙醇胺、苯甲酸钠、四硼酸钠、碳酸钠、葡萄糖酸钠为主要原料研制出一种水溶性环保防锈剂。通过正交试验分析了各组分用量对防锈性能的影响,优选出最佳方案。采用一系列实验方法对研制的防锈剂性能进行了评价,结果表明该新型防锈剂不仅对黑色金属如铸铁、钢,而且对多种有色金属,如铜、铝、镁等均有较好的防锈效果。     

Recent achievements in the synthesis and characterization of metal hexafluorantimonates and hexafluoroaurates

The efforts to prepare new MSbF₆/MSb₂F₁₁ (A = In, Cu, Au, Hg) compounds were partly successful. Reaction between InBF₄ and excess SbF₅ in anhydrous hydrogen fluoride (aHF) yields a mixture of InF₃·3SbF₅ and unidentified SbF₃·xSbF₅. The attempts to synthesize MSbF₆/MSb₂F₁₁ salts (A = Au, Hg) by controlled reduction of Au(SbF₆)₂ or Hg(SbF₆)₂ solutions in aHF/SbF₅ by elemental hydrogen, resulted in the precipitation of metallic Au or Hg₂(Sb₂F₁₁)₂. In the reaction of metallic Cu and deficit SbF₅, the synthesis of CuSbF₆ was achieved. CuSbF₆, like CuAsF₆, is a rare example of a Cu(I) compound in a pure fluorine environment.Vibrational spectra of M(II) hexafluoroantimonates (M = Ni, Fe, Co, Cu, Cr, Pd, Ag) were reinvestigated. It was found that many of them originally assigned to M(SbF₆)₂ compounds, belong to their mixtures with oxonium salts H₃OM(SbF₆)₃, H₃OSbF₆, and/or H₃OSb₂F₁₁.Reactions were studied between MF₂/2AuF₃ (M = Ni, Cu, Ag, Zn, Cd and Hg) and KrF₂ or UV-irradiated elemental fluorine in aHF as solvent at room temperature. On the basis of mass balances, Raman spectroscopy and X-ray powder diffraction analysis it can be concluded that the isolated solids have structures that can be considered in terms of an M(AuF₆)₂ formulation. Previously reported syntheses and characterization of M(AuF₆)₂ (M = Mg, Ca, Sr, Ba) were reinvestigated. In the case of M = Ba two different Au⁻F₆ salts were isolated.Raman spectra of the majority of synthesized metal hexafluoroaurates (M = Ni, Cu, Ag, Zn, Cd, Hg, Mg and Ca) show more bands than expected for regular Au⁻F₆ anion, indicating that the salts obtained exhibit relatively strong cation-anion interactions. The Raman spectra of the remaining Sr and Ba salts show the presence of more regular Au⁻F₆ octahedra, indicating weak cation-anion interactions.