超声浸取预处理-流动注射火焰原子吸收法测定大气颗粒物中Pb和Cd

本文提出超声波震荡前处理方法提取大气滤膜样品中待测金属。通过对样品浸取液种类、酸度和干扰方面的研究,确定了颗粒物样品溶液制备的最佳分析条件,结合流动注射在线富集——原子吸收技术,建立了环境中气体样品测定Pd,Cd方法。方法快速、准确,标准样品测定回收率在97％以上,六次测定相对标准偏差小于2.6％。     

微波消解-氢化物发生-原子荧光法测定海蜇中的痕量砷和硒

建立了氢化物发生-原子荧光光谱法(HG-AFS)测定新鲜和腌制海蜇中痕量砷、硒的分析方法。采用冷冻干燥和微波消解相结合的方法处理样品,设定了最佳的样品处理条件和仪器测定条件,解决了消解液中过剩酸对测定的干扰问题,并对共存元素干扰情况进行了研究。利用加标回收试验,对分析方法进行了验证。实验结果表明,该方法具有简便、快速、灵敏、准确等特点,适合于含水量较高的生物样品的测定。     

微波辅助萃取加拿大一枝黄花的花中总黄酮的工艺研究

对加拿大一枝黄花的花进行微波处理,考察微波辅助萃取对加拿大一枝黄花的花中总黄酮提取率的影响.以卢丁为标准品,用硝酸铝做显色剂,采用分光光度法在530nm波长处测定了加拿大一枝黄花的花中总黄酮的含量,探讨了料液比、乙醇浓度、微波功率、微波处理时间等因素对加拿大一枝黄花的花中总黄酮提取率的影响.结果表明,在料液比1:10、乙醇浓度70%、微波功率700W、微波处理时间15min最优条件下,加拿大一枝黄花的花中总黄酮的提取率为17.86%.     

儿童膨化食品中痕量铝的胶束增敏荧光光度法测定

本文采用了铝－8－羟基喹啉－5－磺酸（H2QS）－十六烷基三甲基溴化铵（CTMAB）胶束增敏体系，用荧光光度法对7种儿童膨化食品中痕量铝进行了测定，同时对样品的测定条件和消化处理进行了较详细的研究。方法简单、快速、灵敏度高，测定结果令人满意。     

微波辅助萃取-分光光度法测定卫矛中总黄酮

采用微波辅助萃取法提取,以分光光度法测定卫矛样品中的总黄酮含量。并且通过单因素实验和正交实验设计优化了溶剂浓度、溶剂用量、微波功率和微波辐射时间等微波提取条件,确定了微波辅助萃取法提取卫矛中黄酮类化合物的最佳条件为:使用60%乙醇,在液固比40∶1条件下,以255W的微波功率,微波辐射5min。在上述最优条件下进行了精密度和回收率实验,所得结果的相对标准偏差为1.71%(n=5),回收率在97%~101%之间。与传统的索氏提取法和超声波提取法比较,微波辅助萃取法具有操作简便,经济可靠,重现性好等特点。该实验采用的微波辅助萃取-分光光度法测定法简便高效,可推广应用于各类中草药中总黄酮的含量测定。     

微波-超声波辅助提取枸杞中的多糖工艺

利用微波-超声波辅助提取枸杞中的多糖物质,采用正交试验法考察料液比、浸提温度、微波和超声波功率以及时间等对枸杞中多糖物质提取效率的影响,得到最佳提取工艺:料液比为1∶10(g/mL),微波提取温度为100℃,微波功率为300W,提取时间6min,超声处理时间20min,超声功率80W,温度为70℃.     

微波溶样—ICP／MS法测定稻中15种痕量稀土元素

本文报道采用ＨＮＯ３＋Ｈ２Ｏ２微波溶样，ＩＣＰ－ＭＳ直接测定稻中１５种稀土元素，对微波溶样和等离子体质谱测定条件进行了优化选择。选用Ｒｅ作内标可补偿基体效应。方法检出限为７．０－２５．８ｐｇ／ｍＬ，稻壳加标回收率为９５－１０５％，ＲＳＤ为２．３－４．２％，方法快速、灵敏、准确。     

微波消解-氢化物发生-原子荧光光谱法测定大米中痕量汞

采用微波消解 氢化物发生 原子荧光光谱法对大米中痕量汞进行了消解、测定。以微波消解为样品前处理方法 ,建立了大米微波消解的最佳分析条件。确定了原子荧光光谱仪的参数设置 ,最佳氢化反应条件以及影响汞测定的相关环境参数。检测限 0 0 0 5ng·mL-1 ,测定大米中汞成分分析标准物质 (GBW 0 85 0 8)中汞的含量 ,其结果与证书值相吻合 ,精密度 2 1 % ,回收率 95 2 %～ 1 0 6 4 %。     

微波消解、流动注射-氢化物发生原子荧光光谱法测定三七中硒含量

用微波消解、流动注射－氢化物发生原子荧光光谱法测定三七中硒，通过实验选择最优化的测定条件，方法的检出限为0．30μg.L^-1，相对标准偏差为1．2％，线性范围为0－100μg.L^-1，相关系数为0．9999，回收率为96．7％－100．7％。     

废弃番茄叶中叶绿素超声-微波协同的提取工艺

利用超声-微波协同法提取废弃番茄叶中的叶绿素.通过单因素及正交试验研究了溶剂、乙醇浓度、微波功率、超声温度、超声时间、料液比、微波时间7个因素对叶绿素提取量的影响,再进行正交试验和验证实验.结果表明最佳工艺条件是:乙醇浓度90％、微波功率500W、超声温度70℃、超声时间40min、料液比1∶10(g/mL)、微波时间...     

Speciation of selected metals in aerosol samples by TXRF after sequential leaching

Total reflection x‐ray fluorescence (TXRF) spectrometry was applied after sequential leaching for the speciation of selected elements in particulate matter, in order to complete the knowledge of the mobility of the selected elements and to determine which components are harmful to works of art. Samples were collected on filters in two churches, one situated in a rural area and the other in an urban area. A five‐stage sequential leaching scheme for the speciation of K, Ca, Fe, Zn and Pb was applied, the fractions obtained being as follows: exchangeable elements; elements bound to carbonates; elements bound to Fe and Mn oxides; elements bound to organic matter; and the digested insoluble residue. It was found that, in the case of the church in the urban area, much of the K, Fe and Zn appeared as mobile elements, whereas for the church situated in the rural area, the amounts of Ca and Fe were most mobile. Copyright © 2006 John Wiley & Sons, Ltd.     

电感耦合等离子体原子发射光谱/质谱法在中药微量元素及形态分析中的应用

本文对近年来电感耦合等离子体原子发射光谱法（ICP－AES）和电感耦合等离子体质谱（ICP－MS）在中药微量元素及形态分析中的应用进行了评述，讨论了应用ICP－AES／MS技术测定中药微量元素样品处理和各种分析方法，引用文献58篇。微波消解可作为中药微量元素分析理想的样品处理方法；ICP－AES／MS及各种联用技术在中药微量元素含量及形态分析中将发挥越来越重要的作用。     

Medieval glass from the Cathedral in Paderborn: a comparative study using X-ray absorption spectroscopy, X-ray fluorescence, and inductively coupled laser ablation mass spectrometry

We have investigated four stained glass samples recovered from an archaeological excavation at the Cathedral in Paderborn (Germany) between 1978 and 1980. On two of the samples there are parts of paintings. Concentrations of major elements were determined using two independent techniques: LA–ICP–MS (a UV laser ablation microsampler combined with an inductively coupled plasma mass spectrometer) and synchrotron radiation X-ray excited X-ray fluorescence (SR-XRF). The SR-XRF data were quantified by using the program package PyMCA developed by the software group of the ESRF in Grenoble. Significant differences were found between the concentrations determined by the two techniques that can be explained by concentration gradients near the surface of the glasses caused, for example, by corrosion/leaching processes and the different surface sensitivities of the applied techniques. For several of the elements that were detected in the glass and in the colour pigments used for the paintings X-ray absorption near edge structure (XANES) spectra were recorded in order to determine the chemical speciation of the elements of interest. As was expected, most elements in the glass were found as oxides in their most stable form. Two notable exceptions were observed: titanium was not found as rutile—the most stable form of TiO₂—but in the form of anatase, and lead was not found in one defined chemical state but as a complex mixture of oxide, sulphate, and other compounds.     

Application of Preconcentration and Separation Techniques in Atomic Fluorescence Spectrometry

Abstract

With 135 references, this review presents the recent application of various preconcentration and separation techniques in atomic fluorescence spectrometry for the sensitive determination and speciation of various elements and their species. It focuses on sample pretreatment, separation, and enrichment-related techniques, including liquid–liquid extraction, solid-phase (micro)extraction, microwave/ultrasound-assisted extraction, pressurized liquid extraction, as well as chemical vapor generation. In this review, the historical development and overview of these preconcentration and separation methodologies are briefly discussed, together with a comprehensive collection of application of these methods in combination with atomic fluorescence spectrometry for determination of ultratrace amounts of elements and their species in various sample matrices (liquids and solids).     

微波消解-ICP-MS测定胃癌和癌旁组织中的微量元素

采用微波消解技术,建立了人体胃组织中22种微量元素含量的ICP-MS测定方法.样品经恒温干燥后,采用硝酸-过氧化氢体系微波消解,优化ICP-MS得到最佳工作参数,测定时以Ge,Rh作为内标来校正由于基体效应和信号漂移对测量造成的影响.该方法的回收率为94.7％-105.6％,相对标准偏差为2.9％-13.4％,检出限为...     

绿茶和红茶中微量元素初级形态含量的研究

本文采用沸水浸泡法对茶叶的初级形态进行分离 ,原子吸收光谱法测定了绿茶和红茶初级形态中 8种微量元素含量 ,计算并讨论了微量元素初级形态分析参数 ,获得茶叶中微量元素初级形态的有关信息。结果表明 ,绿茶和红茶中 8种微量元素初级形态含量各有差异 ,初级形态分析参数自符合程度为87.2 0 %— 10 3.73% ,样品的回收率为 87.1%— 10 2 %。     

ICP-MS用于新疆紫草的无机元素初级形态分析及其溶出特性研究

应用电感耦合等离子体质谱技术(ICP-MS),分析了新疆紫草中20多种无机元素的初级形态;并研究了不同提取溶剂对其溶出特性的影响.结果显示:在消解方法上,高温密封消解较之微波辅助消解(MAP)能更彻底地消解样品,达到分析要求;在溶液中,除了K,Zn以溶解态为主要存在形式外,其余绝大部分元素主要以悬浮态存在;不同提取溶剂的极性与所分析的无机元素密切相关.Mg,K,Ca,Mn,Tl,Co和Pb等7种元素的提取得率与其提取溶剂极性呈完全的正比例关系,其余元素尽管略有差异,但基本上呈线性关系.     

微波消解-ICP-MS法测定肺癌患者肺组织中33种元素

建立了冷冻干燥微波消解ICP-MS法测定肺癌患者肺组织中33种元素的方法.样品经真空冷冻干燥,采用纯化硝酸-过氧化氧体系微波消解,稀释定容后用ICP-MS对溶液进行元素的测定,在优化仪器工作参数后,以铑(Rh)和铼(Re)双内标进行校正.测定结果表明,元素榆出限为0.01～0.45 ng·mL~(-1),测定了国家标准物质GBw(E)080193牛肝中的元素,测定值与标准值或参考值一致,元素精密度(RSD)为2.1%～14.3%,回收率为90.1%～117.5%.用该法测定了6例肺癌患者的肿癌、痛旁和正常组织中33种元素的含量.所建立的方法快速、简便、准确,适于肺组织等生物样品中多种元素的测定.     

参术汤中8种元素的初级形态分析

对一中药复方参术汤以及组成该复方的4种单味药水煎液中8种元素进行初级形态分析,探讨了复方与单味药中元素含量之间的关系,火焰原子吸收光谱法测定元素含量。测定结果表明:复方中铁、锌、钙的含量分别是单味药中元素含量之和的2.44、2.27、1.26倍;锰为0.84倍;镁、铜、钠、钾相差无几(0.97—1.04倍)。对于可溶态亦具有同样的规律。说明复方水煎液中各成分发生相互作用导致有些元素形态发生改变。     

高分辨率MPT全谱仪的研制及性能测试

研制了采用模块化设计的高分辨率MPT全谱仪.新研制的MPT全谱仪采用了全内置连续可调微波功率源、中阶梯光栅分光和紫外增强面阵CCD检测等多项先进技术,该仪器具有分辨率高、检测波长范围宽、灵敏度高、模块化等优点.对该仪器对26种元素检出限、光谱分辨率、多元素同时检测及实际样品测定等的考察表明其结果令人满意.