氢化物发生-电感耦合等离子体质谱联用技术研究

运用自制的接口，实现了氢化物发生与电感耦合等离子体质谱的联用。考察了连续流动氢化物发生器、气动型断流式氢化物发生器及气动型流动注射氢化物发生器与电感耦合等离子体质谱仪的联用性能。确定了仪器的最佳参数，研究了系统的分析性能，实现了能生成氢化物的8种元素的定量测定。     

热喷雾作为电感耦合等离子体原子发射光谱的进样技术

设计并建立了热喷雾器及其去溶装置。用热喷雾作为电感耦合等离子体原子发射光谱的进样技术，并对其性能作了系统研究。与气动雾化器比较，对２３个元素检出限的改善为５￣２０倍。     

Elemental Analysis of Biodiesel by Inductively Coupled Plasma Optical Emission and Flame Atomic Absorption Spectrometries

The extraction of 21 elements from biodiesel using aqueous acid and alkaline solutions was investigated as pretreatment to permit their determination by inductively coupled plasma optical emission spectrometry and flame atomic absorption spectrometry. Al, Ca, Cd, Cu, K, Mg, Mn, Na, V, and Zn were completely extracted from the biodiesel fuel with aqueous acid solution, and Na was completely extracted with alkaline solution. Extraction characteristics varied from element to element; however, 100?±?5% recoveries were obtained with a 30-s extraction procedure. Therefore, although biodiesel is an organic lipophilic material, these elements were determined in aqueous solution. The extracted elements were determined based on traceable Japan calibration service system standards. Accurate analysis of biodiesel was performed using the reported protocol.     

气动雾化进样微波等离子体炬（MPT）原子荧光光谱法测定锌的研究

本文将水溶液雾化进样与微波等离子体炬原子荧光光谱法联用,建立了HCL-MPT-AFS测定Zn的新方法。讨论了实验条件的选择问题以及溶液中共存离子对测定Zn的影响,本文所推荐的方法具有较高的灵敏度和精密度,并将其用于实际样品分析。     

气动雾化进样时微波等离子体炬作为激发光源的性能研究

以气动雾化进样研究了微波等离子体炬（ＭＰＴ）放电作原子发射光谱法激发光源的性能，包括ＭＰＴ的获得、操作参数的影响、样品引入及其分析性能，并与微波诱导等离子体进行了比较，证明ＭＰＴ放电作激发光源有良好的分析性能．     

悬浮液进样电感藕合等离子体发射光谱中颗粒的输运和蒸发行为

以碳化硼为例,研究了悬浮液雾化进样中的粒子在传输和蒸发过程中的行为,并对分析结果出现负偏离的原因进行了详细探讨.对比悬浮液颗粒的原始粒径分布和经过传输过程后的粒径分布,获得到达等离子体的颗粒粒径上限小于10 Am.样品中存在的部分超大粒径的颗粒(d>>10 μm)会严重影响可传输区域颗粒(d<10 μm)的质量运输效率...     

气动雾化进样微波等离子体炬原子发射光谱法研究

本文研究了气动雾化进样低功率微波等离子体炬原子发射光谱法的分析性能,方法对Ag、Al、Ca、Cd、Cu、Fe和Mg的检出限分别为31、17、3.0、6.7、16、5.1和3.1ng/mL,对所研究元素的测定精密度(RSD)在1.7至5.3％之间。另外还研究了易电离元素对测定的影响。     

毛细管电泳氢化物发生等离子体原子发射光谱联用的接口设计

设计了一种毛细管电泳氢化物发生装置。应用该装置将毛细管电泳(CE)分离后的两种硒形态转化为氢化物,然后再将氢化物引入到电感耦合等离子体原子发射光谱(ICP-AES)中进行检测。讨论了盐酸、硼氢化钠的浓度和载气流速对硒氢化物发生的影响,通过两根PTFE管并列方式消除了体系的反压,将优化的条件应用于Se的形态分析,RSD小于5%,检出限低于3μg/L,结果令人满意。     

氢化物发生与ICP/AES联用后等离子体的性质研究

本文通过测量电子密度ｎｅ,电子温度Ｔｅ,激发温度Ｔｅｘｃ及谱线强度,将氢化物进样同水溶液常规气动雾化进样对比,研究了氢化物进入ＩＣＰ后,对等离子体性质的影响。结果表明,由于氢化物的引入,ＩＣＰ的激性能得到了改善。     

Review of Solid Sample Introduction for Plasma Spectrometry and a Comparison of Results for Laser Ablation, Electrothermal Vaporization, and Slurry Nebulization

The relative merits of three solid sample introduction techniques for inductively coupled plasma atomic emission spectroscopy and inductively coupled plasma mass spectrometry have been evaluated. The techniques studied were laser ablation (LA), slurry nebulization, and slurry introduction via electrothermal vaporization. The application of each technique to the quantification of Pa and Pb in geochemical samples has been described and the results obtained for each technique have been compared. To help in assessing the potential of the systems described here a simple classification of the agreement obtained between found and known values has been proposed allowing a comparison of these results with other results published in the literature to be made. Problems encountered during the evaluation of the techniques have been described and, for LA, the associated problems have led to the development of a modified sampling system which was used in an investigation of some fundamental aspects of LA as a method of solid sample introduction. Possible routes for improvement in sampling and transport are suggested, including use of reactive gases, ablation under stopped flow conditions and removal of large particles by gravitational settling.     

氢化物发生新体系-原子荧光法同时测定铅和镉

报道了Pb和Cd同时氢化物发生的K3Fe(CN)6-(NH4)2Ce(NO3)6-NaBH4-HCl新体系,并探讨了相关反应机理。(NH4)2Ce(NO3)6作为氧化剂将Pb(Ⅱ)氧化为Pb(Ⅳ),Fe(CN)63-与Pb(Ⅳ)络合促进了Pb的氢化物发生。同时,体系中的(NH4)2Ce(NO3)6作为Cd氢化物发生过程中的增敏剂使荧光信号显著增强。在该体系中,Pb和Cd的氢化物发生不产生相互干扰。本实验据此建立了顺序注射-氢化物发生-双道原子荧光同时测定Pb和Cd的方法。所采用的实验条件包括NaBH4、HCl、K3Fe(CN)6和(NH4)2Ce(NO3)6的浓度分别为2%、3%、0.6%和0.3%。以125μL/s进样500μL,得到的线性范围分别为0.4~15μg/L(Pb)和0.5~20μg/L(Cd);对应的检出限分别为0.09μg/L(Pb)和0.17μg/L(Cd);方法的精密度为0.5%(6.0μg/L Pb,n=9)和1.0%(6.0μg/L Cd,n=9)。将本法应用于国家标准样品GBW08608中Pb和Cd的检测,检测值与标准值相符;对河水及海水中Pb和Cd进行了同时测定,加标回收率合格。     

氢化物发生-电感耦合等离子体原子发射光谱法同时测定锑锭中氢化物元素和非氢化物元素

运用改进的同心喇叭口双溶液管雾化器，采用连续氢化物发生法，在酸性介质中，对锑锭样品溶液既发生雾化作用，又对可形成氢化物的元素（Ａｓ、Ｓｅ、Ｐｂ）发生氢化作用，使它们的发射强度得到显著提高，而对非形成氢化物的元素（Ｆｅ、Ｃｕ）的发射强度基本不受影响，利用ＩＣＰ－ＡＥＳ同时测定锑锭中形成氢化物的元素和非形成氢化物的元素。对实际样品进行对比检测，结果令人满意。     

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…     

Continuous Hydride Generation with Direct Current Plasma Emission Spectroscopic Detection for Total Arsenic Determinations (HY-DCP)

Abstract

Total arsenic determinations in complex food matrices can be performed with a high degree of accuracy and precision using an initial hydride formation step followed by direct current plasma (DCP) emission spectroscopic detection¹. The hyphenated technique, HY-DCP, uses a continuous flow hydride formation step with dual mixing of the hydride forming reagents, followed by on-line, continuous introduction of the aqueous arsenic sample. The final aqueous solution of arsine, excess sodium borohydride, and sample components, is directly introduced into the conventional spray chamber of the DCP instrument. Calibration plots for both arsenate and arsenite have been determined, together with linearities and minimum detection limits (MDLs) The overall methods for total arsenic determination have been applied to spiked water and tunafish samples. Accuracy and precision determinations have been performed for these total arsenic analyses, and compared with continuous hydride formation-flame atomic absorption (FAA) detection, as well as sequential hydride formation-FAA methods. All of these results are then compared, with the individual advantages and disadvantages o f each approach summarized.     

Optimization of Continuous Flow Hydride Generation Inductively Coupled Plasma Optical Emission Spectrometry for Sensitivity Improvement of Bismuth

Experimental variables in continuous flow hydride generation inductively coupled plasma-optical emission spectrometry (CF-HG-ICP-OES) were optimized for determination of bismuth. Concentrations of NaBH₄, HCl, and NaOH, flow rates of NaBH₄, sample solution, waste and carrier argon, radio frequency power, lengths of reaction, and stripping coils were optimized to obtain lower detection limits. Under optimum conditions, the detection limit was calculated as 0.16 ng mL^?1, and the calibration plot was linear between 1.0–50.0 ng mL^?1. An improvement in detection limit of 5.75 times by CF-HG-ICP-OES was reached vs. ICP-OES. Relative standard deviation (RSD) for ten replicate measurements of 10.0 ng mL^?1 Bi was calculated as 3.9%. Effect of possible interferic ions on Bi signal was evaluated. Accuracy of method was verified by using a standard reference material, SRM 1643e. Results found for Bi were in satisfactory agreement with certified values. The proposed method was then employed to determine trace concentration of Bi in milk samples. Bi amounts in samples were found in the range from lower than the quantitation limit to 14.5 ng mL^?1, whereas Bi concentrations were lower than the detection limit in three samples.     

Spectrophotometric Determination of Ipratropium Bromide in Liquid for Nebulization

ABSTRACT

Three simple and sensitive spectrophotometric methods for the determination of ipratropium bromide (IPB) in liquid for nebulization are described. Method A, is based on the formation of a charge transfer complex with iodine. The reaction product is measured spectrophotometrically at 278 nm. Method B, is based oh the formation of an ion – association complex between the drug and an acidic dye, Bromocresol green (BCG), which is extractable into chloroform and has an absorption maximum at 418 nm. Method C, uses derivative spectrophotometry for the determination of IPB by measuring the D₂-value at 232 nm. Beer's law is obeyed over the concentration range 1-10, 2-16 and 5-30 μg ml^? for method A, B and C, respectively. The optimum conditions for the formation of the charge transfer or ion-association complexes were optimized. The proposed methods were applied for the determination of IPB in liquid for nebulization. Evaporation to dryness and extraction of the residue with isopropanol, were performed before application of methods A & B. Mean percentage recoveries were found to be 99.67 ± 0.79, 99.26 ± 1.06 and 100.21 ± 0.85 for method A, B, and C, respectively.     

超声雾化进样法MPT－AFS的研究

本文对超声雾化进样微波等离子体炬（ＭＰＴ）原子荧光光谱法（ＡＦＳ）的分析性能进行了研究，在实验中详细地考察了各种实验条件和仪器参数对分析性能的影响，并利用此方法对Ｚｎ、Ｃｄ等元素进行了分析测定研究，并对这种等离子体的荧光发射区域作了探讨。     

连续氢化物发生—微波等离子体炬原子发射光谱法测定砷

对连续氢化物发生－微波等离子炬原子履地测定砷进行了研究，对这一方法的分析性能考察结果表明，本法对砷的检出限（３σ）ｎｇ／ｍＬ线性范围达三个数量级，大多数共存离子的干扰很小，对实际样品是一种简便、快速、准确的分析方法。     

Determination of Some Elements by MIP-AAS Spectrometry with Ultrosonic Nebulization Sample Introduction System

Atmospheric pressure plasmas are not only powerful sources for excitation but also very good atomizers. In the early developing stage, the inductively coupled plasma (ICP) was investigated as an atomizer for atomic absorption spectrometry (AAS). A multiple pass system,a T-shaped plasma cell,and a long-path torch was used to increase the absorption path length. But all these ICP-AAS systems gave low sensitivities for most     

Nebulization effects in analytical atomic spectrometry

The effects of solvent vaporization and of element redistribution between the various fractions of an aerosol during sample nebulization in atomic spectrometry are examined. These effects govern the fluctuations of element concentration in the analytical zone of the flame. Sample composition modification can increase random errors to 5–10% in the absence of matrix matching.