微波消解技术在难处理贵金属合金PtPdRhIr分析中的研究与应用

提出了微波密闭消解难处理贵金属合金PtW、PtRh、PtPdRh和PdIr、PtIr、PtIrRE、PtRuIr的方法;对比了它们的微波密闭消解和传统分解法的条件;分析了消解后贵金属Pt、Pd、RhI、r的含量。结果表明:上述各类合金对应消解时间分别为传统法的1/14~1/15和1/24~1/8倍;总分析流程大大缩短;两种方法测得贵金属结果相吻合。     

微波消解方法在贵金属分析中的应用

贵金属包括铂族元素和金银共8种。铂族金属对酸的化学稳定性比所有其它金属都高,其中钌和锇、铑、铱对酸的化学稳定性特别高,不仅不溶于普通酸,甚至也不溶于王水,钯和铂能溶于王水。钯是铂系元素中最活泼的一个,可溶于浓硝酸和热硫酸。金一般只溶于王水。银是贵金属中最活泼的,能溶于硝酸和热的浓硫酸,但因生成氯化银沉淀而不溶王水。由于贵金属的溶解困难,在贵金属的分析中,样品制备显得尤为重要,因为制备过程中的掺杂问题,许多试验者选择固体粉末直接检测方法,使贵金属的检测准确度和灵活性差,并因基体效应增加了基体匹配的难度。     

微波在样品消解中的应用

介绍微波消解样品的基本原理、特点、应用及注意事项。用微波消解样品，效率高、速度快、易于控制、对环境无污染，应用于矿石、金属、食品、化工产品、医药及环境样品等样品化学分析的预处理，是传统加热消解样品的理想替代方法。     

微波消解技术在农业样品分析中的应用

利用光纤压力自控密闭微波消解系统对土壤和植株样品中重金属元素测定的影响进行了研究，确立了样品消解试剂、微波消解每件及样品预处理方法。结果表明，该方法与常压湿法消解相比，具有样品消解时间短、消解试剂用量少、样品污染小等特点，是准确可靠的土壤及植株样品中重金属元素检测样品消解处理方法。     

微机处理副反应存在下不同类型难溶化合物的溶解度

微机处理副反应存在下不同类型难溶化合物的溶解度沙岗，余嘉政，黄干初（湖南医科大学化学教研室长沙４１００７８）进行沉淀滴定和重量分析时，要求沉淀反应趋于完全。反应完全的程度，一般可根据沉淀的溶解度来衡量。溶解度越小，反应越完全，测定的误差也越小。在定量...     

微波消解电感耦合等离子体质谱法测定大气气溶胶中的铂元素

采用高压密闭微波消解系统消解样品,结合电感耦合等离子体质谱(ICP-MS)法,测定了上海市区大气气溶胶样品中Pt元素的含量。实验采用数学校正方法扣除HfO复合离子对Pt元素测定的干扰,用标准溶液模拟样和铂族元素标准物质检验方法的可靠性,其测定值与标准值相吻合。Pt、Hf的检出限分别为0.3 ng/L、3.0 ng/L;Pt和Hf的空白值分别为1.0±0.1 ng/L和29.0±1.0 ng/L。对采集的3个气溶胶样品的测定结果表明:上海市区大气气溶胶中Pt的平均含量为1.5±1.0 pg/m3,低于世界其他城市。     

微波在合成六元杂环化合物中的应用

对微波技术在合成六员杂环化合物中的应用做了概述:(1)含氧六员杂环化合物;(2)含氮六员杂环化合物。     

超级微波消解电感耦合等离子体质谱法测定车用陶瓷催化剂中铂、钯、铑

建立了一种检测车用陶瓷催化剂中铂、钯、铑的超级微波消解电感耦合等离子体质谱法.通过单因素试验和正交试验优化酸配比、称样量、消解温度、消解时间及回流溶剂参数,确定了最佳消解方法:0.1 g样品中加入1 mL盐酸、5 mL硝酸、1 mL氢氟酸,在220℃的消解温度下保持30 min,赶酸后加入10 mL逆王水于170℃回流...     

贵金属元素电化学分析研究(Ⅷ)——痕量铂的阳极溶出伏安法测定

用伏安法或石墨电极阳极氧化伏安法测定痕量铂虽有报道,但其灵敏度均不够高。Ghulkina等发现在HCl介质中含Sn(Ⅳ)或Sn(Ⅱ),以Pt-Sn共沉淀在碳糊电极上,使铂的测定限达5×10-9g/L。本文用0.3mol/LH_2SO_4-Hg(Ⅱ)-3.0×10~(14)mol/L KMnO_4体系测Pt,其检测限为0.5μg/L。探讨了利用黄原酸钠纤维素酯(CCX)分离除去试液中Au~(3+)Pd~(2+)等干扰元素。本法已用于实际样品分析,结果较好。     

植物中多元素测定的微波消解前处理技术

植物中多元素同时测定的前处理采用微波消解技术,利用原子吸收法和单频直流等离子体原子发射法测定茶叶和中药中的Ｂａ、Ｃａ、Ｃｕ、Ｆｅ、Ｋ、Ｍｇ、Ｍｎ、Ｎａ、Ｓｒ、Ｔｉ和Ｚｎ。用四种国家标准参考样品进行考察,结果表明这是一项安全可靠且快速无污染的技术。     

贵金属分析

本文是《分析试验室》定期评述中“贵金属分析”的第四篇文章，评述了１９９６年１月至１９９７年１２月间我国贵金属分析的进展。内容包括概述，试样前处理，分离富集和各种分析方法及研究等。引用文献３４３篇。     

Voltammetric Determination of Platinum in Plant Material

A very sensitive procedure for the determination of platinum in hydroponically cultivated plant samples (Sinapis alba L and Lolium perenne) is presented. A microwave digestion with HNO₃, HClO₄ and HCl acids with additional UV irradiation is followed by the platinum determination by adsorptive stripping voltammetry at hanging mercury drop electrode. The influence of HNO₃ acid on voltammetric determination of platinum is discussed. For validation of the obtained results the recovery of Pt was examined and the Pt determination by ICP MS was carried out. The highest platinum amounts were found in the roots of the plants, nevertheless the effective transport of platinum to the steams and leaves was also observed.     

微波消化技术在生物微量元素测定中的应用

用微波消化技术消化了多种食物样品．与传统的干、湿消化法相比，微波消化更加简单、快速、节省、沾污少、损失少、环境污染少．用原子吸收测定样品中的Ｆｅ，Ｃ．Ｖ＜２％，加标回收率为９８％～１００％，测定美国生物标准物质牛肝中的Ｆｅ的相对误差为０．３％，结果令人满意．     

电感耦合等离子体-原子发射光谱法测定贵金属-难熔金属涂布液中的铱和钌

报道了采用ＩＣＰ－ＡＥＳ法测定贵金属－难溶金属涂布液中铱和钌。考察了基体及无机酸对发射强度的影响。采用铬作为内标元素以提高方法的精密度。在优化条件下,对Ｉｒ１０,Ｉｒ２０两个试样进行了测定。其相对标准偏差（ｎ＝９）Ｉｒ为０．５８％～１．３６％,Ｒｕ为０．５４％～０．７６％;回收率Ｉｒ为９７％～１０３％、Ｒｕ为９６％～１０３％。     

Analytical Determination and Bio-Monitoring of Platinum Group Elements in Roadside Grass Using Microwave Assisted Digestion and Electrothermal Atomic Absorption Spectrometry

The analytical conditions that enable the determination of traffic related platinum group elements (PGEs) in roadside grass using microwave digestion and electrothermal atomic absorption spectrometry were evaluated as an alternative to the biomonitoring of traffic related PGEs and Pb levels in urban areas. To optimize the analytical conditions and account for matrix effects that could import error in the analysis, method optimization was based on matrix simulation through analyte recovery from spiked unpolluted samples against a matrix blank. A mixture of nitric and hydrofluoric acid under progressively increasing microwave irradiation was optimized to afford the quantitative extraction of platinum group elements from plant matrix. Due to the low levels of platinum group elements in real samples, preconcentration was accomplished using sample evaporation followed by dissolution in dilute nitric acid prior to deliverance to the atomic detector. Quantitation limits below 1 ng g^?1 for Pd and Rh and lower than 2 ng g^?1 for Pt, were accomplished, enabling the monitoring of platinum group elements bioaccumulation in roadside grass with satisfactory recoveries, as determined from the analysis of spiked samples. The results from method application in an annual monitoring survey of PGEs and Pb levels in urban flora and other roadside media are presented and discussed.     

环境和生物样品中铂族金属的分析研究进展

评述了近年来环境和生物样品中痕量铂族金属的分析研究进展，重点介绍了样品的预处理和分离富集技术以及检测手段等。     

用微波消解气相色谱法测定鱼肉中的有机氯农药

研究了微波消解 -有机溶剂提取 -气相色谱法测定鱼肉样品中有机氯农药的分析方法。对消解液、微波辅助加热条件及提取溶剂进行了优化实验 ,选择冰醋酸 -高氯酸 (体积比4∶1)在600W微波功率下接受辐射2min分解鱼肉样品 ,用30 % (φ)苯的石油醚溶液提取 ,对各种有机氯农药的回收率除 p,p′_DDT为60.3 %外 ,其余均在83.4 %～109.6 %之间 ,与水浴加热分解的国家标准方法相当。该法具有快速 ,灵敏度、精确度、准确度高等优点 ,适用于大批量食品和生物样品中有机氯农药的分析测定。     

A New Family of Binary Layered Compounds of Platinum with Alkali Metals (A = K,Rb, Cs)

By reacting platinum with alkali metals (A = K, Rb, Cs) a new family of binary alkali metal platinides has been synthesized and characterized by chemical analysis, X‐ray powder diffraction, thermal analysis (DTA and DSC), and magnetic measurements. All three compounds exhibit similar XRD‐patterns with strong reflections that can be indexed on the basis of a rhombohedral crystal system (K_xPt: a = 2.6462(1), c = 17.123(1); Rb_xPt: a = 2.6415(1) Å, c = 17.871(1) Å; Cs_xPt: a = 2.6505(1) Å, c = 18.536(1) Å; x < ½. The a lattice constant is independent on the alkali metal used and of value close to the Pt–Pt distance in NaPt₂ (2.645Å). The c parameter increases monotonically with the growing atomic radius of the alkali metal. The average structure of the alloys consists of cubic close packed layers of platinum atoms with layers of disordered alkali metals in between. For all compounds besides the strong reflections small satellites are observed which cannot be indexed together with the rhombohedral peaks in any rational 3‐dimensional lattice. However, these satellites can be indexed as incommensurate modulations within the ab plane (found propagation vectors k = (0.1011, 0.2506, 0) for Cs_xPt, and k = (0.0168, 0.2785, 0) for Rb_xPt).     

Voltammetric Analysis of Trace Levels of Platinum Group Metals – Principles and Applications

The compelling use of autocatalytic converters, containing platinum group metals (PGMs), has been the cause, in the environmental and biological matrices, of an increasing concentration of such metals. For this reason, in the last decade, the literature has reported several papers regarding analytical procedures for the determination of Pt(II), Pd(II) and Rh(III) in real samples, generally employing spectroscopic methods. The present review intends to highlight the contribution of the voltammetric techniques for the determination of these metals, including also those less investigated, i.e. Iridium, Osmium and Ruthenium.     

Diversity of Luminescent Metal Complexes in OLEDs: Beyond Traditional Precious Metals

Organic light-emitting diodes (OLED) have attracted increasing attention due to their excellent properties, such as self-luminosity, high color gamut and flexibility, and potential applications in display, wearable devices and lighting. The emitters are the most important composition in OLEDs, mainly classified into fluorescent compounds (first generation), metal phosphorescent complexes (second generation), and thermally activated delayed fluorescence (TADF) materials (third generation). In this review, we summarize the advances of novel emitters of organic metal complexes in the last decade, focusing on coinage metals (Cu, Ag, and Au) and non-precious metals (Al, Zn, W, and alkali metal). Also, the design strategy of d¹⁰ and Au(III) complexes was discussed. We aim to provide guidance for exploring efficient metal complexes beyond traditional phosphorescent complexes.