Determination of Au, Ir and thirty-two other elements in twelve geochemical reference materials by instrumental neutron activation analysis

Summary Elemental concentrations of twelve geochemical reference materials of ores and mineralized rocks were determined including some for which there were few previously published data. Reference materials CHR-Bkg, CHR-Pt, CCU-1c, NBM-1a, NBM-2a, NBM-4a, NBM-6a, NBM-6b, PM-S, UMT-1, WMG-1, and WMS-1 were analyzed for 34 elements by instrumental neutron activation. To our knowledge, the analytical results in this paper are among the first published for five reference materials from the Nevada Bureau of Mines and Geology. Reliable results for Au and Ir down to concentrations of a few ng^.g^-1were obtained without preconcentration.     

Bestimmung der Edelmetalle Au, Pd, Pt, Rh und Ir in Gesteinen und Erzen mit der elektrothermalen Atomabsorptions-Spektrometrie

Zusammenfassung Nach einem Druckaufschluß bei 170°C von 5 g Gesteinsprobe mit HF und aqua regia werden die Edelmetalle Au, Pd, Pt, Rh und Ir durch selektive Adsorption auf den Ionenaustauscher SARAFION NMRR von der restlichen Matrix abgetrennt. Im Thioharnstoffeluat können die Edelmetalle mit der elektrothermalen AtomabsorptionsSpektrometrie quantitativ bestimmt werden. Die Methode wurde durch Analyse von internationalen Gesteinsstandards und Meteoriten geprüft.

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Determination of the precious metals Au, Pd, Pt, Rh and Ir in rocks and ores by electrothermal atomic absorption-spectrometry

Summary After pressure digestion at 170°C of 5 g rock samples with HF and aqua regia the precious metals Au, Pd, Pt, Rh and Ir are separated from the rest matrix with selective adsorption on SARAFION NMRR ion exchange resin. The precious metals can be determinated in the thiourea eluate by electrothermal atomic absorption spectrometry. The reliability of the procedure was confirmed by analysing rock standards and meteoritic material.

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Die Untersuchungen wurden durch Mittel der Deutschen Forschungsgemeinschaft

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Die Untersuchungen wurden durch Mittel der Deutschen Forschungsgemeinschaft     

Gas-chromatographische Trennung der Edelmetalle Au, Pt, Pd, Rh und Ir als Bis(trifluoroethyl)-dithiocarbamato-Chelate

Zusammenfassung Die Bedingungen für die gas-chromatographische Trennung und Bestimmung der Edelmetalle Au, Pt, Pd, Rh und Ir als Bis(trifluoroethyl)-dithiocarbamato-Chelate wurden untersucht. Die besten Trennergebnisse lieferte eine (1000 mm×2 mm i.d.)-Glassäule mit 3% OV-3 auf Chromosorb G-AW-DMCS. Mit dem ECD konnten Edelmetallkonzentrationen im unteren ppb-Bereich erfaßt werden.

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Gas-chromatographic separation of the precious metals Au, Pt, Pd, Rh and Ir as bis(trifluoroethyl)-dithiocarbamate chelates

Summary The gas-chromatographic conditions for the separation and determination of the precious metals Au, Pt, Pd, Rh and Ir as bis(trifluoroethyl)-dithiocarbamate chelates were ascertained. Best results were obtained with a (1000 mm×2 mm i.d.)-glas column packed with 3% OV-3 on Chromosorb G-AW-DMCS. Using the ECD, precious metal concentrations of the lower ppb-range can be determined.

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Die Untersuchungen wurden durch Mittel der Deutschen Forschungsgemeinschaft (Kr 590/11-1) unterstützt.     

丙醇-氯化钠双水相体系萃取分离铂、钯、铑、金中的铱及其吸收光谱分析研究

提出了一种丙醇－氯化钠双水相体系萃取铱的分离－吸收光谱分析方法，在HCl介质中基于铱生成三氯亚锡酸络阴离子动力学速率与铂、钯、铑、金差异使铱与铂、钯、铑、金分离，其后在KI介质中萃取铱使其与贱金属基体分离，研究了在丙醇萃取相中铱的吸收光谱分析，并应用于实际样品中铱的测定。     

CO hydrogenation over small Pt, Ir and Pt?Ir bimetallic clusters entrapped in the supercage of NaY zeolite

In CO hydrogenation, small (ca. 1 nm) Pt–Ir bimetallic clusters encapsulated in the supercage of NaY zeolite showed significant non-linear Schulz-Flory distributions, especially high selectivity for C₄ hydrocarbons, which is different from those of Pt or Ir clusters entrapped inside the supercage of NaY.     

Hydrogen-oxygen and carbon monoxide adsorption on Ir, Ir?Pt and Ir?Pd alumina-supported catalysis

From dispersity studies and adsorption isotherms on alumina supported Ir, Ir–Pt and Ir–Pd catalysts, the ratios of O/M=1 and CO/M=1 are obtained. Electron microscopiec results agree with chemisorption data.

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Ir, Ir–Pt Ir–Pd, , O/M=1 CO/M=1. - .

     

Fabrication of monometallic (Co,Pd, Pt,Au) and bimetallic (Pt/Au,Au/Pt) thin films with hierarchical architectures as electrocatalysts

Co thin films with novel hierarchical structures were controllably fabricated by simple electrochemical deposition in the absence of hard and soft templates, which were used as sacrificial templates to further prepare noble metal (Pd, Pt, Au) hierarchical micro/nanostructures via metal exchange reactions. SEM characterization demonstrated that the resulting noble metal thin films displayed hierarchical architectures. The as-prepared noble metal thin films could be directly used as the anode catalysts for the electro-oxidation of formic acid. Moreover, bimetallic catalysts (Pt/Au, Au/Pt) fabricated based on the monometallic Au, Pt micro/nanostructures exhibited the higher catalytic activity compared to the previous monometallic catalysts.     

Die Bestimmung von Mikromengen Au, Ag, Pt, Pd, Rh, Os, Ir, Se, Te und Hg durch Ringcolorimetrie

Ohne Zusammenfassung     

Trennung von Pt, Pd, Rh und Ir durch Papierelektrochromatographie

Ohne Zusammenfassung     

Synthesis of Au, Au/Ag, Au/Pt and Au/Pd nanoparticles using the microwave-polyol method

Gold, Au/Ag, Au/Pt and Au/Pd bimetallic nanoparticles with varying mol fractions were synthesized in ethylene glycol and glycerol, using the microwave technique in the presence of a stabilizer poly(N-vinylpyrrolidone) (PVP). It was found that bimetallic colloids of Au/Ag, Au/Pd and Au/Pt form an alloy either on co-reduction of respective metal ions or on mixing individual sols.     

乙二胺改性聚氯乙烯大孔螯合树脂富集分离微量金, 铂, 钯, 铱的性能和机理研究

本文利用ICP化学光谱法对自合成的聚乙烯乙二胺大孔螯合树脂富集分离微量金, 铂, 钯, 铱进行了研究, 讨论了螯合树脂对各微量元素的富集性能、吸附速率和富集机理, 并进行了样品的分析, 获得了较满意的结果。     

纳米团簇Au19Pd和Au19Pt催化解离N2O

采用密度泛函理论研究Au-Pd和Au-Pt 纳米团簇催化解离N₂O. 首先根据计算得到Au₁₉Pd和Au₁₉Pt 团簇的最优构型(杂原子均位于团簇的表面). 以Au₁₉Pd催化解离N₂O为例研究催化解离的反应机理. 对此主要考虑两个反应机理, 分别是Eley-Rideal (ER)和Langmuir-Hinshelwood (LH). 第一个机理中N₂O解离的能垒是1.118 eV, 并且放热0.371 eV. N₂分子脱附后, 表面剩余的氧原子沿着ER路径消除需要克服的能垒是1.920eV, 这比反应沿着LH路径的能垒高0.251 eV. 此外根据LH机理, 氧原子在表面的吸附能是-3.203 eV, 而氧原子在表面转移所需的能垒是0.113 eV, 这表明氧原子十分容易在团簇表面转移, 从而促进氧气分子的生成. 因此, LH为最优反应路径. 为了比较Au₁₉Pd和Au₁₉Pt 对N₂O解离的活性, 根据最优的反应路径来研究Au₁₉Pt 催化解离N₂O, 得到作为铂族元素的铂和钯对N₂O的解离有催化活性, 尤其是钯. 同时, 将团簇与文献中的Au-Pd合金相比较, 得到这两种团簇对N₂O 解离有较高的活性, 尤其是Au₁₉Pd团簇. 再者, O₂的脱附不再是影响反应的主要原因, 这可以进一步提高团簇解离N₂O的活性.     

铂-金交替修饰的铂核纳米颗粒的制备与表征

通过吸附在铂纳米颗粒表面的氢交替还原氯金酸和氯铂酸,得到了复合型纳米颗粒Pt@Au/Pt,用UV-Vis光谱、TEM和XRD对其进行了表征.     

Nanowire-based nanogap electrodes by annealing of multisegmented Pt/Au/Pt nanowires in air

A simple thermally lithographic method for fabricating nanowire-based metallic nanogap electrodes is presented, in which the multisegmented Pt/Au/Pt nanowires were electrodeposited in the pores of porous anodic aluminum oxide (AAO) templates first and then thermally annealed to form a nanoscale gap at the interface of Au/Pt. We proposed that the breaking of the multisegmented Pt/Au/Pt nanowires is due to the chemical and physical transformations of the Au segment with O₂. These electrodes are ideally suited for electron-transport studies of chemically synthesized nanostructures, and their utility is demonstrated here by measuring the electronic conduction of short (54-base-pairs) double-stranded (ds) DNA molecules in a dry state.     

Solid-state photoluminescence sensitization of Tb3+ by novel Au2Pt2 and Au2Pt4 cyanide clusters

The syntheses are reported for two novel Tb(3+) heterotrimetallic cyanometallates, K(2)[Tb(H(2)O)(4)(Pt(CN)(4))(2)]Au(CN)(2)·2H(2)O (1) and [Tb(C(10)N(2)H(8))(H(2)O)(4)(Pt(CN)(4))(Au(CN)(2))]·1.5C(10)N(2)H(8)·2H(2)O (2) (C(10)N(2)H(8) = 2,2'-bipyridine). Both compounds have been isolated as colorless crystals, and single-crystal X-ray diffraction has been used to investigate their structural features. Crystallographic data (MoKα, λ = 0.71073 ?, T = 290 K): 1, tetragonal, space group P4(2)/nnm, a = 11.9706(2) ?, c = 17.8224(3) ?, V = 2553.85(7) ?(3), Z = 4; 2, triclinic, space group P1, a = 10.0646(2) ?, b = 10.7649(2) ?, c = 17.6655(3) ?, α = 101.410(2)°, β = 92.067(2)°, γ = 91.196(2)°, V = 1874.14(6) ?(3), Z = 2. For the case of 1, the structure contains Au(2)Pt(4) hexameric noble metal clusters, while 2 includes Au(2)Pt(2) tetrameric clusters. The clusters are alike in that they contain Au-Au and Au-Pt, but not Pt-Pt, metallophilic interactions. Also, the discrete clusters are directly coordinated to Tb(3+) and sensitize its emission in both solid-state compounds, 1 and 2. The Photoluminescence (PL) spectra of 1 show broad excitation bands corresponding to donor groups when monitored at the Tb(3+) ion f-f transitions, which is typical of donor/acceptor energy transfer (ET) behavior in the system. The compound also displays a broad emission band at ～445 nm, assignable to a donor metal centered (MC) emission of the Au(2)Pt(4) clusters. The PL properties of 2 show a similar Tb(3+) emission in the visible region and a lack of donor-based emission at room temperature; however, at 77 K a weak, broad emission occurs at 400 nm, indicative of uncoordinated 2,2'-bipyridine, along with strong Tb(3+) transitions. The absolute quantum yield (QY) for the Tb(3+) emission ((5)D(4) → (7)F(J (J = 6-3))) in 1 is 16.3% with a lifetime of 616 μs when excited at 325 nm. In contrast the weak MC emission at 445 nm has a quantum yield of 0.9% with a significantly shorter lifetime of 0.61 μs. For 2 the QY value decreases to 9.3% with a slightly shorter lifetime of 562 μs. The reduced QY in 2 is considered to be a consequence of (1) the slightly increased donor-acceptor excited energy gap relative to the optimal gap suggested for Tb(3+) and (2) Tb(3+) emission quenching via a bpy ligand-to-metal charge transfer (LMCT) excited state.     

Controlled Assembly of Au,Ag, and Pt Nanoparticles with Chitosan

Working on the chain gang : A simple method for the controlled assembly of metal nanoparticles (Au, Ag, and Pt) into 1D chains (see figure) has been developed based on the electrostatic interaction of negatively charged carboxylic groups on the citrate ions surrounding the NPs and the positively charged chitosan polymer.

     

Kα3,4 satellites in Mg–Cl elements

The Kα_3,4 satellites in Mg–Cl elements are measured a high-resolution double-spectrometer. Intensity ratio of the Kα_3,4 satellites in these elements relative to the Kα_1,2,3,4 emission lines are compared with those obtained theoretically by a sudden approximation. Moreover, the origin of the Kα_3,4 satellites, especially, for Mg, Al, and Si could not be explained clearly by the contribution of the 1s2s→2s2p and 1s2p→(2p)² spectator holes using GRASP2 code.     

Untersuchungen zum Verhalten des Rh,Pd, Ir und Pt im Chloridmedium an Anionenaustauschern

Investigations on the Behaviour of Rh, Pd, Ir, and Pt on Anion Exchangers in the Chloride Medium Comparative investigation on the behaviour of compounds of Rh, Pd, Ir, and Pt on anion exchangers in the chloride medium have been carried out by varying the basicity of the amino groups, the acidity and temperature of the added solution, and the valance and complex type of the platinum-group metals. The existence of two exchange mechanisms was concluded from the adsorption and desorption behaviour:

• a exchange of unchanged anions of the platinum-group metals (the “pure” ion exchange that is predominant in sufficiently acidified solutions on all resins),
• b complex bonding of the platinum-group metals as a result of the entry of free amino groups into the internal complex sphere (becomes important with decreasing acidity on resins of low up to medium basicity).

Maximum loads of the resins under various conditions and exchange coefficients for the “pure” ion exchange are reported.     

Glühdrahtexperimente mit den Systemen Pt/O2, Ir/O2, Pt/Cl2, Pt/Br und Rh/Br

Glowing Filament Experiments with the Systems Pt/O₂, Ir/O₂, Pt/Cl₂, Pt/Br, and Rh/Br Reactions of glowing filaments of platinum and iridium with oxygen confirmed the usefulness of the method for the determination of the formulae of the volatile compounds (PtO₂, IrO₃) under equilibrium conditions. The afterwards made experiments with glowing filaments of platinum with Cl₂ at 1300 K and with platinum and rhodium with Br at 1900 K under equilibrium conditions lead to the formation of PtCl₂, PtBr, and RhBr.     

Electrooxidation of 2-propanol on Pt, Pd and Au in alkaline medium

Pd and Au are investigated as electrocatalysts for 2-propanol oxidation and compared with the conventional catalyst of Pt in alkaline medium. The current density for 2-propanol oxidation on Pd electrode is much higher than that on Pt electrode. The onset potential for 2-propanol oxidation on Pd electrode is more negative compared with that on Pt electrode. The results show that Pd is a good electrocatalyst for 2-propanol oxidation and the activity for the electrooxidation of 2-propanol is higher than Pt and Au in alkaline medium. Pd has higher electrocatalytic activity and better stability for the electrooxidation of 2-propanol. The present study shows a promising choice of Pd as effective electrocatalyst for 2-propanol electrooxidation in alkaline medium.