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。     

偏最小二乘催化极谱法同时测定铂,钯,铑

应用Ｍ２７３Ａ电化学系统中的线性扫描技术，确定了０．７５ｍｏｌ／ＬＨ２ＳＯ４－１．５％ＮＨ４Ｃｌ－２．８ｍｍｏｌ／Ｌ（ＣＨ２）６Ｎ４－０．００２５％Ｎ２Ｈ４．Ｈ２ＳＯ４为偏最小二乘极谱法同时测定Ｐｔ、Ｐｄ、Ｒｈ的最佳极谱体系。Ｐｔ、Ｐｄ、Ｒｈ的线性范围为３．２ｍｇ／Ｌ、０－１５．０ｍｇ／Ｌ和０－１．０ｍｇ／Ｌ。模拟样品及实际样品的回收率在９０．３－１０７．７％之间。     

18—冠—6修饰碳糊电极测定定金的研究

本文研究了１８－冠－６修饰碳糊电极测定金的条件，金在０．５ｍｏｌ／Ｌ ＨＣｌ－０．００５ｍｏｌ／Ｌ ＫＣｌ底液中富集，介质交换到０．０１ｍｏｌ／Ｌ ＨＣｌ中进行测定。金（Ⅲ）浓度在０．１～１．０μｇ／ｍＬ范围内呈线性关系，相对标准偏差为９．７％，检出限为２０ｎｇ／ｍＬ。可不经预先分离直接测定矿样中的金，结果良好。并研究了Ａｕ（Ⅲ）在１８－冠－６碳糊修饰电极上的还原机理。     

3－氨甲基吡啶树脂的合成及五种氨基吡啶树脂对金铂吸附性的比较

研究了反应物配料比３－ＡＭＰ／Ｃｌ（摩尔比）、反应温度与时间对大孔型３－氨甲基吡啶树脂（３—ＡＭＰＲ）性能的影响规律．在最佳合成工艺条件下制得３－ＡＭＰＲ的功能基含量为３．１６ｍｍｏｌ／ｇ树脂．３－ＡＭＰＲ对ＡｕＣｌ６（２－），ＰｔＣｌ６（２－），ＩｒＣｌ６（２－），ＰｄＣｌ４（２－），ＲｈＣｌ６（３－）的吸附容量分别为８００．８，３８７．８，３８６．３，１３３．０，１０５．５ｍｇ金属／ｇ树脂；配位比分别为１．２９，０．６３，０．６４，０．４０，０．３３。比较了３—ＡＭＰＲ、２－ＡＭＰＲ、４－氨基吡啶树脂（４－ＡＰＫ）、３—ＡＰＲ、２－ＡＰＲ五种树脂对ＡｕＣｌ４－、ＰｔＣｌ６（２－）的吸附性，其中３－ＡＭＰＲ为最佳。     

铂—钯共显色衍生络合物的高效液相色谱研究

研究了Ｐｄ（Ⅱ）和４，４＇－二（二乙氨基）苯硫酮（ＢＤＰＴＫ）共显色所生成的Ｐｔ（Ⅱ）络合物，于Ｎｕｃｌｅｏｓｉｌ Ｃ８柱上，用含３×１０＾－３ｍｏｌ／Ｌ ＣＳＡ和０．０２ｍｏｌ／Ｌ ＨＡｃ－ＮａＡｃ（ｐＨ３．５）的乙腈－丙酮－水（７２：５：２３，Ｖ／Ｖ）作流动相（１．０ｍｌ／ｍｉｎ）分离并检测。Ｐｔ的校正曲线的线性范围为０．２～３．０μｇ／ｍｌ，Ｐｔ检测限为０．７ｎｇ。此方法已应用于抗癌药物顺铂     

应用颗粒状8—氨基喹啉螯合纤维素交换剂分离富集Pt（IV）,Pd（Ⅱ）

采用自制颗粒状８－氨基喹啉纤维素交换剂，对Ｐｔ（Ⅳ）和Ｐｄ（Ⅱ）进行柱分离，当ｐＨ为３．８时，Ｐｄ（Ⅱ）被交换剂的螯合基团螯合，而Ｐｄ（Ⅳ）不被螯合，从而达到Ｐｔ（Ⅳ），Ｐｄ（Ⅱ）的分离，再以１ｍｏｌ／Ｌ的ＨＣｌ作洗脱液将Ｐｄ（Ⅱ）洗脱，此法可达到定量分离，操作简便。     

离子交换法从铂系金属中提取铑的研究

本文研究了阴离子交换树脂从铂系金属混合溶液中使Ｐｈ与Ｐｔ，Ｐｄ，Ｉｒ达到定量分离。合适的分离条件是０．５ｍｏｌ．ｄｍ＾－＾３ＮａＣｌ，ｐＨ＝２，通Ｃｌ２气。Ｒｈ的回收率＝（１００±２）％。     

微量贵金属对Co/γ-Al2O3的作用及其结构表征Ⅰ.Co-M/γ-Al2O3催化剂的活性及其XRD和XP

催化剂采用等量浸渍法，先后将Ｃｏ与贵金属相分浸于γ－Ａｌ２Ｏ３上，经５００℃焙烧，４５０℃氢气还原剂（ｍｃｏ３ｏ４／ｍＡｌ２ｏ３＝０．０８，ｍ贵金属／ｍ催化剂＝１／１０００），ＣＯ氧化活性的测定结果表明，贵金属Ｐｔ和Ｐｄ与Ｃｏ之间具有的协同催化作用，而Ｒｈ与Ｃｏ的协同作用较差，在Ｃｏ－Ｐｔ／γ－Ａｌ２Ｏ３和Ｃｏ－Ｐｄ／γ－Ａｌ２Ｏ３上，ＣＯ１００％转化的温度较在Ｃｏ／γ－Ａｌ２Ｏ３上下降约６０℃，     

电沉积制备钯铂电极上乙醇的电催化氧化

研究了乙醇在碱性介质（１．０ｍｏｌ·Ｌ－１ＮａＯＨ）中电沉积制备的Ｐｄ／ＧＣ、Ｐｔ／ＧＣ和Ｐｄ．Ｐｔ／ＧＣ电极上的电催化氧化．实验结果表明：由此法制备的钯铂系列合金电极对乙醇的电催化氧化表现出明显的协同效应─—乙醇在含把原子分数ｙｐｂ＝０．３３６的Ｐｄ－Ｐｔ／ＧＣ合金电极上的阳极交换电流密度是其在纯铂电极上的３０多倍．     

微量贵金属对Co／γ-Al_2O_3的作用及其结构表征Ⅰ．Co－M／γ－Al_2O_3催化剂的活性及其XRD和XPS表征

催化剂采用等量浸渍法，先后将Ｃｏ与贵金属组分浸于γ－Ａｌ２Ｏ３上，经５００℃焙烧，４５０℃氢气还原制得（ｍＣｏ３Ｏ４／ｍＡｌ２Ｏ３＝０．０８，ｍ贵金属／ｍ催化剂＝１／１０００）．ＣＯ氧化活性的测定结果表明，贵金属Ｐｔ和Ｐｄ与Ｃｏ之间具有明显的协同催化作用，而Ｒｈ与Ｃｏ的协同作用较差．在Ｃｏ－Ｐｔ／γ－Ａｌ２Ｏ３和Ｃｏ－Ｐｄ／γ－Ａｌ２Ｏ３上，ＣＯ１００％转化的温度较在Ｃｏ／γ－Ａｌ２Ｏ３上下降了约６０℃，而在Ｃｏ－Ｒｈ／γ－Ａｌ２Ｏ３上仅下降了２５℃左右．ＸＲＤ和ＸＰＳ的表征结果表明，Ｃｏ／γ－Ａｌ２Ｏ３中Ｃｏ以高分散的金属Ｃｏ相和类似ＣｏＡｌ２Ｏ４的尖晶石相存在，而Ｃｏ－Ｍ／γ－Ａｌ２Ｏ３（Ｍ＝Ｐｔ，Ｐｄ，Ｒｈ）催化剂中，Ｃｏ相已完全被还原为零价．高分散的金属钴相和贵金属相的协同作用，可能与氧从贵金属至Ｃｏ相上的溢流效应有关．     

茜素红S螯合树脂分离富集测定地质样品中的痕量金、铂和钯

用螯合树脂对金属进行分离富集及测定,前人已做了许多有意义的研究^[1～4].曾用含键合S双硫腙(P-D)和脱氢双硫腙(P-DT)功能团的离子交换树脂和螯合树脂分离金和铂族金属^[5],用双硫腙负载树脂分离富集Cu(Ⅱ)^[6]。     

对磺基苯偶氮变色酸螯合形成树脂分离富集微量铂和钯

采用对磺基苯偶氮变色酸（ＳＰＣＡ）作为螯合剂制备具有相应的螯合基团形成树脂。研究了ＳＰＣＡ螯合形成树脂的分析特性及其各种条件对分离富集和测定的影响。实验表明：ＳＰＣＡ螯合形成树脂能在ｐＨ＜５的盐酸溶液中稳定存在；并在ｐＨ１．００时ＳＰＣＡ树脂将微量铂和把的氯络阴离子进行交换并与常见的金属离子分离，采用酸性硫脲溶液定量洗脱。通过对样品加标准回收试验，用原子吸收光谱法测定回收率均在９４％－1０５％之间。     

Synthesis of N-Methyl-2-Thioimidazole Resin and Its Complex Behavior for Noble Metal Ions

The functional group capacity and the percentage of functional group conversion of crosslinked polystyrene resin bearing N-methyl-2-thioimidazole (MTIR) synthesized under optimum conditions are as high as 4.08 mmol/g resin and 96.0%, respectively. The apparent activation energies of sorption of MTIR for Au(III) and Pt(IV) are 13.1 and 13.4 kJ/mol, respectively. The sorption behavior of MTIR for Au(III), Pt(IV), and Pd(II) obeys the Freundlich and Langmuir isotherms. The sorption capacities of MTIR for Au(III), Pt(IV), and Pd(II) are as high as 4.33, 2.12, and 2.33 mmol/g resin, respectively. Au(III), Pt(IV), and Pd(II) adsorbed on MTIR can be eluted quantitatively by the eluant. The resin can be regenerated easily and reused without an obvious decrease in the sorption capacity for Au(III) and Pd(II). The resin has high sorption selectivity for noble metal ions. Au(III) can be separated quantitatively in the presence of high concentrations of Cu²⁺, Fe³⁺, Ni²⁺, and Mn²⁺. The recovery of platinum from the spent industrial catalysts is 98.6% by MTIR. The preconcentration and separation of palladium and platinum from the anode deposits of electrolysis of crude copper have been investigated. The resin may have potential industrial uses.     

Synthesis and Efficiency of a Spherical Macroporous Epoxy-dicyandiamide Chelate Resin for Preconcentrating and Separating Trace Au, Hg, Pd and Ru from Samples

IntroductionThe preconcentration and separation of elements in samples by means of a chelateresin[l--5J or a chelate fibre[6'7J have been reported. However, the synthesis of the resin or thefibre usually takes a long time and a complex synthetic process. Accordingly, the epoxy--tan-ning chelate resin[8] and the epoxy-urea chelate .esin[9] have been synthesized and used for thepreconcentration of trace elements. However, these chelate resins could not be used for theenrichment of trace element…     

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。     

Radiochemical neutron activation analysis for determination of Au,Ag, Pt and Pd in geological samples

A procedure for separation of Au, Ag, Pt, and Pd in geological samples has been developed. After irradiation, samples were fused with Na₂O₂ and silver was separated by filtering through a PbCl₂ filter in 4M nitric acid solution. Au, Pt and Pd were concentrated with rhodium and thiourea as rhodium sulfide and the separation process of these elements was carried out by a chromatographic method. Au, Pt and Pd were retained on a Dowex-1×8 anion column in 1M HCl. Pd was eluted from the column by using a mixture of 75% HCl acid-25% acetone. Au was eluted by using a mixture of 10% HCl-90% acetone. In the gold fraction, Pt was also determined through the photopeak of¹⁹⁹Au radionuclide (158 keV). The method was simple and rapid.     

Application of a macroporous resin containing imidazoline groups to preconcentration and separation of gold, platinum and palladium prior to ICP-AES determination

A new functional resin with a long functional side chain was synthesized by modification of aminated macroporous poly(vinyl chloride) resin with cyanoethylene and ethylenediamine. Traces of Au(III), Pt(IV) and Pd(II) in aqueous solution were quantitatively adsorbed in the acidity range of pH 4 and C(H(+)) 3 M. The rate of equilibration is high; Cu(2+), Fe(3+), Ni(2+), etc. exhibit little interference on the adsorption of the sought noble metals. The saturated adsorption capacities for Au(III), Pt(IV), Pd(II) and Ir(IV) in 2 M HCl were 4.0, 1.57, 2.26, 1.85 mmol g(-1). Adsorbed ions can be quantitatively desorbed by 4% thiourea +0.25 M H(2)SO(4). The resin has good reusability, and can be used for preconcentration and separation of Au(III), Pt(IV) and Pd(II) prior to their determination by ICP-AES with satisfactory results.     

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YPA_4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。     

Determination of the noble metals in chromites and other geological materials by radiochemical neutron activation analysis

A procedure is described for determining the noble metals in geological samples of varied composition (Si enriched or Cr enriched). This rapid separation procedure allows very low detection limits for all PGE (except Rh) and Ag. It uses the coprecipitation of Pd, Pt, Au, Ag and Ru with Se and Te, and the fixation of Os on an ion-exchange resin. Ir is systematically determined by epithermal NAA using multiparameter coincidence spectrometry.     

Electrothermal vaporization inductively coupled plasma atomic emission spectrometry determination of gold, palladium, and platinum using chelating resin YPA(4) as both extractant and chemical modifier

A new method for determination of trace gold (Au), palladium (Pd), and platinum (Pt) in environmental and geological samples by electrothermal vaporization (ETV)-inductively coupled plasma atomic emission spectrometry (ICP-AES) with the use of chelating resin YPA₄ as both solid phase extractant and chemical modifier has been developed. The resin loaded with analytes was prepared to slurry and directly introduced into the graphite furnace without any pretreatment. The factors affecting the vaporization behaviors of Au, Pd, and Pt were investigated in detail. It was found that, in the presence of YPA₄, Au and Pd could be quantitatively vaporized at lower vaporization temperature of 1900 °C. Compared with the conventional electrothermal vaporization, the vaporization temperature was decreased by 700 °C, and the detection limits for Au and Pd was decreased by a three-fold. However, a little effect of YPA₄ on the ETV-ICP-AES determination of Pt was found. Under the optimized conditions, the detection limits (3σ) of Au, Pd, and Pt for this method are 75, 60, and 217 pg, respectively; and their relative standard deviations (R.S.D.) are 4.4, 5.6, and 3.7%, respectively (n=9, C=0.2 μg ml⁻¹). The proposed method has been applied to the determination of trace Pd and Pt in sewage sludge, and the results well agreed with the recommended values. In order to further verify the accuracy of the developed method, a GBW07293 certified geological reference material and an auto catalyst NIST SRM 2557 reference material were analyzed, and the determined values coincided with the certified values very well.