微波等离子体原子发射光谱法(MP-AES)测定地质样品中的常量和微量元素

建立了微波等离子体原子发射光谱法(MP-AES)测定地质样品中的常量和微量元素的方法,四酸(盐酸+硝酸+高氯酸+氢佛酸)消解样品,得出了使用4200 MP-AES仪分析地化认证参考物质中常规金属元素(Ag,Cu,Ni,Pb和Zn)的结果,测定样品结果的相对标准偏差落在±10%范围内,另外,IEC和FLIC模型可成功校正光谱干扰。MP-AES仪无需使用乙炔等危险气体,极大提高了实验室安全性并显著降低了运行成本。MP-AES仪已成功应用于地化样品的分析中,结果准确可靠。     

微波等离子体发射光谱法同时测定特色南药中多种元素

特色南药样品利用硝酸微波消解后,在优化的还原剂浓度下,采用多模式样品导入系统和微波等离子体原子发射光谱法(MP-AES)对样品溶液中Al,As,Hg,Ca,Cu,Cr,Pb,Zn等17种元素进行同时分析,考察了其在特色南药材中的含量。结果表明,MP-AES对目标元素有较好的检出限,2种标准物质的分析结果与ICP-MS分析结果及标准值一致,其中可蒸气发生元素(As,Hg,Sb和Se等)未检出。方法对金属元素的检出限为0.05~0.53μg/g,对于氢化物可蒸气发生元素和Fe的检出限为0.93~5.40μg/g。通过该方法进行测定,发现南药样品中Cd和Cu含量低于中国药典的限值,而Cr和Pb含量明显高于欧洲草药材的限值,As和Hg需优化方法降低检出限后方可用于样品质量控制。本方法检出限较低,线性范围较宽,分析结果准确、快速,可进行多元素同时分析,能满足对南药材中多种元素的分析要求。     

Evaluation of Atomic Fluorescence Spectrometry for Determination of Mercury Using a Low-Powered Argon Microwave Plasma Torch (MPT)

The Microwave-Induced Plasma (MIP) has received considerable attention during the past decade since theintroduction of the Becnakker Cavity. It has been commonly used as an atomization cell for atomic emission spectrometry (AES) and atomic absorption spectrometry (AAS), and a great success was achieved for both techniques. More     

微波等离子体原子发射光谱法(MP-AES)测定米粉中的常量、微量和痕量元素

采用4200型微波等离子体原子发射光谱法(MP-AES)分析米粉中的镉和其它常量、微量以及痕量元素。对标准样品(CRM)的测定值与标准值十分吻合,检出限(MDL)足以满足分析需求,并且具有出色的长期稳定性。实验中无需使用改性剂或离子抑制剂,从而简化了样品前处理过程。4200 MPAES具有出色的分析性能,可分析火焰原子吸收法(FAAS)无法分析的磷元素、能够进行多元素无人值守操作、拥有更高的安全性和易用性,是期望获得新技术的FAAS用户的理想选择     

Analysis of Borosilicate Catalysts by Inductively Coupled Plasma Atomic Emission Spectroscopy

Abstract

A method was developed for the analysis of borosilicate catalysts. Samples were prepared by fusion technique with potassium hydroxide and analyzed by inductively coupled plasma atomic emission spectroscopy (ICP-AES). The method was applied to a borosilicate NIST SRM 93 which was analyzed for major and minor elements (aluminum, sodium, silicon and boron). Despite the presence of relatively high concentration of the potassium, no matrix interferences were observed. This method provides precision and accuracy better than ±4% and ±6%, respectively.     

微波等离子体炬发射光谱法测定高温合金中非金属元素

研究了微波等离子体炬原子发射光谱(MPT-AES)法测定高温合金中非金属元素(As、B、P、Si)的分析方法,考察此方法对高温合金行业非金属检测需求的适应性。对镍基高温合金样品进行酸溶解处理,选择适用的微波等离子体炬分析谱线,进行检出限、精密度测定。4种非金属元素的检出限在0.03~0.12μg/mL,10次数据的相对标准偏差(RSD,n=10)为0.88%~1.9%,此方法可用于高温合金中非金属元素的测定。     

Elemental Analysis of Tarhana by Microwave Induced Plasma Atomic Emission Spectrometry

Elemental analysis of tarhana, a traditional Turkish cereal soup, has been conducted. A new method was developed for the determination of calcium, iron, magnesium, manganese, potassium, and sodium, in tarhana by microwave induced plasma atomic emission spectrometry. A sample of 0.1?g were mineralized by microwave digestion in 10?mL of 65% HNO₃. A wheat flour standard reference material (GBW 08503) was used for validation. Linear calibration using standards prepared in acid was conducted for all determinations. The limits of detection were 1.21?µg?g^?1 for Ca at 393.366?nm, 0.43?µg?g^?1 for Fe at 259.940?nm, 11.5?µg?g^?1 for K at 766.491?nm, 0.12?µg?g^?1 for Mg at 285.213?nm, 0.04?µg?g^?1 for Mn at 403.076?nm, and 0.04?µg?g^?1 for Na at 588.995?nm. Ca, K, Fe, Mg, Mn, and Na were determined in tarhana with values from 0.73 to 1.61, 0.016 to 0.061, 2.02 to 4.09, 0.473 to 1.414, 0.019 to 0.043, and 0.26 to 1.83?mg?g^?1, respectively.     

电感耦合等离子体原子发射光谱(ICP-AES)法测定进口酸泥中砷和汞

本文采用硝酸和盐酸的混合酸低温溶解酸泥后,运用ICP-AES法同时测定进口酸泥中砷和汞。建立了最佳实验方法,确立各项分析条件,砷的测定范围：0.01%~10%,汞的测定范围：0.005%~10%。测定值相对标准偏差小于3%,加标回收率在97%~105%之间,该方法简单快速,准确度高,完全满足酸泥中砷和汞的测定要求。     

微波消解-冷原子吸收光谱法测定消毒剂中的汞

建立了微波消解-冷原子吸收光谱法测定消毒剂中汞的方法。将消毒产品经过微波消解后,其中的汞被氧化为离子状态的汞,利用冷原子吸收光谱测汞仪对样品进行测定,结果表明汞在0~10ng/mL范围内呈良好的线性关系,线性相关系数r=0.999 7(n=6),平均加标回收率为97.08%,相对标准偏差(RSD)为4.0%(n=9)。方法简便、准确、灵敏度高、重现性好,可用于测定消毒剂中的汞。     

微波等离子体炬原子发射全谱仪测定粮食中微量金属元素

大米和面粉主要成分为碳水化合物，同时还含有Ca、Cu、Fe、Mg及Mn等人体必需的微量元素。大米和小麦中微量元素的测定主要有原子吸收法、ICP-AES及ICP-MS等方法。原子吸收法虽然灵敏度高，但一次只能测一种元素。ICP-AES及ICP-MS法均可同时测定多种元素，灵敏度高，线性范围宽，但仪器设备昂贵，运转费用高。本实验采用流动注射-微波等离子体炬原子发射(FI-MPT-AES)在线标准加入法同时测定粮食中的Ca、Cu、Fe、Mg及Mn等金属元素。该法操作简单方便，成本及运转费用低，快速并可同时得到检测波长范围内的全部光谱信息。     

气相色谱—微波等离子体发射光谱法研究农药1605与人唾液的相互作用

用ＧＣ－ＡＥＤ联用技术研究了农药１６０５，得到１６０５所含六种元素的元素色谱图，并用该方法研究了人唾液与１６０５的相互作用。     

A Study on the Determination of Copper by Microwave Induced Plasma Atomic Emission Spectrometry (MIP-AES)

The determination of copper by MIP-AES was investigated in detail. Aqueous samples were introduced from an ultrasonic nebulizer and the solvent was removed by a desolvation device before introduction of the aerosol into the MIP. The desolvation system consisted of a condenser associated with a concentrated H2SO4 absorption cell. Various experimental conditions and interferences from easily ionised elements (EIEs) were also studied and some practical samples were analyzed.     

流动分析技术在微波等离子体炬原子发射光谱分析中的应用

本文系统地介绍了微波等离子体煤（MPT）原子发射光谱分析技术从基础研究到商品化仪器的发展过程中流动分析技术所起的作用。论证了几项较简单技术的联用对于解决分析工作者所面临的一些复杂问题的可能性。     

在线标准加入法在微波等离子体炬原子发射光谱法中的应用

在线标准加入法在微波等离子体炬原子发射光谱法中的应用叶冬梅，张寒琦，于惊雷，金钦汉（吉林大学化学系，长春，１３００２３）关键词在线标准加入法，微波等离子体炬，原子发射光谱法微波等离子体炬（ＭＰＴ）是新发展起来的激发光源［１，２］，由于它具有利于样品引...     

Determination of Carbon by Means of Microwave Plasma Torch Atomic Emission Spectrometry

lntroductionIngenera1,microwaveplasmaatomicemissionspectrometry(MWP-AES)isanexcel1enttechniqueforthedeterminationofnonmetalelements.AlthoughtheMWP-AEShasbeenextensivelyappliedtothedeterminationofnonmetals,suchasS,P,Cl,BrandI[1],therehavebeenonlyafewreportsonthedeterminationforcarbon.Mitchelletal.[2Jreportedafurnace-microwaveplasmasystemtode-termineorganicandinorganiccarbon.Samplesweredispensedintoplatinumboatsandinsertedintoafurnace.TheresultantvaporwasfedtoanArMWPandcarbonemissionatl…     

微波等离子体炬原子发射光谱法测定铁增敏效应

针对在低功率下工作的微波等离子体炬原子发射光谱法(MPT-AES)存在对一些元素检测灵敏度较低和抗基体干扰能力弱的问题,以氩气为载气和工作气,研究了表面活性剂及镧盐对MPT-AES测定铁的增敏效应,考察了铁测定的工作条件和共存元素对铁测定的影响.实验结果表明,非离子表面活性剂对铁的测定有抑制作用,而阳离子表面活性剂和镧盐对铁的测定有增敏作用,其中镧盐增敏效果最好.以镧盐为增敏剂,不仅可提高MPT-AES测定铁的灵敏度,还可增加共存元素的允许量.当体系中镧浓度为0.500 mg/m L时,至少可使40倍的锌,30倍的钴,20倍的镍、锰,15倍的钙,10倍的镁、铜和钠不影响铁的测定.与不加镧时相比,铁的发射强度提高了2.4倍,检出限由原来的27.5×10~(-3)μg/m L下降为8.5×10~(-3)μg/m L.将本方法应用于原油样品中铁的测定,所得结果与火焰原子吸收光谱法测定结果一致.     

天然水中痕量无机汞和有机汞的氢化物原子荧光光谱法分析

建立了天然水中溶解的痕量无机汞和有机汞的氢化物原子荧光光谱法分析方法,该方法经标准物质(PACS-1)和加标回收实验研究表明重现性好、准确度高。在此基础上,应用该方法分析了该校人工湖水中的无机汞和有机汞,发现无机汞和有机汞的含量均低于0.1 礸/L。     

电感耦合等离子体原子发射光谱(ICP-AES)法测定车用尿素水溶液中的8种杂质元素含量

将1g尿素水溶液样品置于烘箱105℃下浓缩,在1 100℃马弗炉中加热灰化;取出冷却,使用盐酸(1+1)溶解灰分。采用Al 237.312nm、Ca 393.366nm、Cr 267.716nm、Cu 324.754nm、Fe 238.204nm、Mg 279.553nm、Ni 231.604nm、Zn 213.856nm作为分析线,建立了使用电感耦合等离子体原子发射光谱(ICP-AES)法测定尿素水溶液中铝、钙、铬、铜、铁、镁、镍和锌8种杂质元素的方法。结果表明,铝、钙、铬、铜、铁、镁、镍和锌的线性范围在0.02~2μg/mL时,校准曲线的线性相关系数均不小于0.999 5;方法中各元素的检出限为0.001~0.010μg/mL。将方法应用于尿素水溶液样品中8种杂质元素的测定,结果的相对标准偏差(RSD,n=7)均小于5.0%,加标回收率为91%~108%。方法可一次性完成对多种元素的测定,准确度、精密度较高,方法简便快速,适用于各级检验机构进行多批次、多项目产品的元素检测。     

Mercury(II) Binding to Metallothionein in Mytilus edulis revealed by High Energy-Resolution XANES Spectroscopy

Of all divalent metals, mercury (Hg^II) has the highest affinity for metallothioneins. Hg^II is considered to be enclosed in the α and β domains as tetrahedral α-type Hg₄Cys_11-12 and β-type Hg₃Cys₉ clusters similar to Cd^II and Zn^II. However, neither the four-fold coordination of Hg nor the existence of Hg–Hg atomic pairs have ever been demonstrated, and the Hg^II partitioning among the two protein domains is unknown. Using high energy-resolution XANES spectroscopy, MP2 geometry optimization, and biochemical analysis, evidence for the coexistence of two-coordinate Hg-thiolate complex and four-coordinate Hg-thiolate cluster with a metacinnabar-type (β-HgS) structure in the α domain of separate metallothionein molecules from blue mussel under in vivo exposure is provided. The findings suggest that the CXXC claw setting of thiolate donors, which only exists in the α domain, acts as a nucleation center for the polynuclear complex and that the five CXC motifs from this domain serve as the cluster-forming motifs. Oligomerization is driven by metallophilic Hg⋅⋅⋅Hg interactions. Our results provide clues as to why Hg has higher affinity for the α than the β domain. More generally, this work provides a foundation for understanding how metallothioneins mediate mercury detoxification in the cell under in vivo conditions.     

Determination of Phosphorus by Inductively Coupled Plasma Atomic Emission Spectroscopy after Hydride Generation

Thehydridegenerationtechniquehascontributedmuchtotheimprovementofthesensitivityinatomicabsorption,emissionandfluorescencespectroscopyofAs.Sb.Bi.Se.Te.Ge.SnandPh"=.ManyworkershavesuccessfullyappliedthistechniquetodeterminationofCu.Zn.Cd3'4'5.KazukoMatsumotostudiedphosphinegenerationcoupledwithICPatomicemissionspectrometry,wherephosphateinaqueoussolutionwasfirstprecipitatedbyaddingCaCI,ascalciumphosphate,whichwasthenreducedtoCa,P,byheating(ca,1100'C)togetherwithaluminumpowder'.Thedetecti…