有机溶剂与水溶液引入电感耦合等离子体电子密度和电子温度轴向分布的比较

为了研究有机ICP最佳分析条件与水溶液ICP明显不同的原因,本文在不同的等离子体操作条件下测量了Hβ486.133nm Stark变宽,分别计算了有机溶剂和水溶液引入1CP轴向的n_e和Te值,并进行了比较。有机溶剂引入ICP时,在固定的功率,观测高度及载气流量下其轴向ne和Te均比用水溶液引入时低一些。有机ICP的优异分析性能只有在比水溶液ICP有较高的入射功率和较低的载气流量条件下才能展现出来。     

乙醇对感耦等离子体发射光谱分析的影响

前言近几年来已有文献报告了用ICP发射光谱直接测定有机溶液样品如油类、酒类等中的多种元素。还有人用螯合萃取的方法对某些痕量元素预先进行富集,然后将有机相直接喷入ICP中进行分析。由于有机溶剂与水相比,在物理性质方面存在很大差异,因而会对ICP产生影响。Greenfield曾报导了将甲醇及其他有机酸引入ICP时,发射强度与溶液粘度,表面张力、密度等物理特性的相关关系。他还报导在以自激式高频发生器作为ICP电源时,有机溶剂     

有机溶剂在流动注射(FI)-ICP-AES体系中的应用

本文采用特制的双毛细管雾化器引入有机溶剂，产生的气溶胶经预混合，在载气（Ａｒ）的作用下导入ＩＣＰ中激发．比较了有机溶剂在ＦＩ－ＩＣＰ与非ＦＩ－ＩＣＰ体系中的行为，所得实验结果表明：（１）引入微体积的有机溶剂于ＦＩ－ＩＣＰ体系，对待测元素谱线强度有不同程度的增敏作用，但依元素和谱线不同而异；（２）同非ＦＩ－ＩＣＰ体系比较，在ＦＩ－ＩＣＰ体系中，ＩＣＰ对有机溶剂有较强的承受能力，原则上可用于不同类型有机溶剂的引入；（３）在试验过程中，未发现因有机溶剂在高温下分解所造成的碳粒沉积现象。     

ICP—AES中有机溶剂对稀土元素的增敏效应

十几年来,人们对不同性质的有机溶剂对待测元素的增敏机理、基体效应及对ICP操作参数的影响等方面进行了研究,并得到了一些有价值的结论。但有机溶剂对稀土元素的增敏效应报道还不多。本研究在以前工作的基础上,以PMBP为萃取剂,考察醋酸丁酯等五种不同性质的有机溶剂对镧、钇的增敏效应,ICP放电的稳定性和碳沉积情况。在优化条件下,与水溶液相比较,检出限明显改善。     

pH分布—光谱法用于背景与待测物波谱严重重叠灰色体系的…

本文基于残差双线性（ＲＢＬ）的原理并结合数值遗传算法，充分利用这一信息，把ｐＨ分布光谱两维信息引入灰色体系的定量分析中，结果表明，对于背景与待测物波谱严重重叠的体系，本法对待测组分预报有较高的准确度。     

溶液制备过程引入的甲醇对阿特拉津UV光氧化速率和降解机理的影响

在低压汞灯（253.7 nm）光照条件下，研究了样品制备过程中引入的有机溶剂甲醇对目标有机物阿特拉津光氧化降解速率的影响规律，并系统地分析了其影响机理.研究结果表明：反应体系中含有低浓度（<0.1%）有机溶剂甲醇时，不会对阿特拉津在单独UV工艺中的降解动力学产生影响；对UV/H₂O₂工艺中阿特拉津降解动力学的影响较小，但此含量的甲醇却能显著地降低阿特拉津在UV/TiO₂工艺中的降解速率.甲醇对阿特拉津在不同光氧化工艺中降解动力学的影响是甲醇与阿特拉津竞争光量子、改变溶液极性和淬灭活性氧化物种等作用的综合结果，但反应体系中甲醇的存在及含量未改变阿特拉津降解产物的种类及降解途径.本研究的结果可为探索溶液制备时引入到反应体系中的有机溶剂对有机目标物光氧化速率的影响提供新的研究视角，同时也能为文献中目标物配制在不同溶剂中的降解速率差异提供合理解释.     

氟化辅助电热蒸发/ICP-AES直接测定氧化铝粉末中痕量杂质钇

报道了以聚四氟乙烯（PTFE）悬浮体为氟化剂,悬浮体制样／氟化辅助电热蒸发（ETV）／ICP －AES直接测定两种AI2O3粉末样品中痕量杂质钇。考察了影响基体和待测元素蒸发过程的各种因素;对比研究了待测元素和基体的氟化蒸发行为。在优化实验条件下,方法的检出限为0．1μg/g,相对标准偏差为5．6％（n=5,c=8g/L悬浮体）。并与溶样法气动雾化（PN）－ICP－AES的分析结果进行了对比。本法简便、灵敏、无需任何化学前处理,可用于相关陶瓷生产过程中的质量控制。     

氟化电热蒸发／电感耦合等离子体原子发射光谱中的基体效应研究

本文系统研究了氟化电热蒸发／电感耦合等离子体原子发射光谱（ＥＴＶ－ＩＣＰ－ＡＥＳ）测定难熔元素的基体效应。与常规气动雾化（ＰＮ）－ＩＣＰ－ＡＥＳ中的基体效应比较，氟化ＥＴＶ－ＩＣＰ－ＡＥＳ中的基体效应更小。对难熔基体元素，由于基体和待测元素与氟化剂之间的竞争反应，随着基体浓度的增加，待测元素谱线强度降低；对常见基体元素，由于热循环中基体与待测元素之间的选择挥发，对待测元素的蒸发和传输过程无明显影响     

含稀土铕(Ⅲ)配位聚合物的研究

将铕的有机配合物NaEu(TTA)4与聚（苯乙烯-丙烯酸）（PSAA）反应制备了铕配位聚合物[Eu(Ⅲ）-TTA-PSAA]，用电导、DTA-TGA、荧光光谱等对其进行了表征。由于配合物中存在着Eu^3 分别与TTA^-和PSAA分子中羧基的配位作用，并进一步交联，因此配合物样品均不溶于大部分有机溶剂，只能溶于N，N-二甲基甲酰胺和丙三醇/异丙醇的混合溶剂，且耐热性得到提高。配合物为褐色固体，在常温、紫外光下发出红光，主要是由于Eu^3 离子的^5D0→^7F2跃进。讨论了pH值对配合物荧光强度的影响，当pH=10时，合成的配合物具有最好的荧光性。     

基于激光介导富集的表面增强拉曼分析

基于具有优异表面增强拉曼散射(SERS)性能的石墨烯隔离的金纳米晶(GIAN)能够在水-有机相界面自组装, 待测物分子在有机相中的分配系数较大以及GIAN能够通过π?π相互作用与待测物分子结合的优势, 构建了激光介导的待测物分子的高效富集策略, 进而实现了9,10-双苯乙炔基蒽(BPEA)分子的痕量SERS分析. 所构建的新型待测物分子高效富集策略在一定程度上避免了因“咖啡环效应”带来的信号波动, 有望为复杂体系中痕量待测物的SERS分析提供可靠的平台.     

有机试剂雾化进样电感耦合等离子体原子发射光谱特性的研究

利用流动注射技术对有机试剂雾化进样情况下电感耦合等离子体（ＩＣＰ）的特性进行了研究。考察了有机试剂对ＩＣＰ放电外观的影响。对ＩＣＰ的局部热平衡状态作了判定。由Ｍｇ２７８．３０ｎｍ和Ｍｇ３３３．６７ｎｍ二线法对有机试剂负载和水负载情况下ＩＣＰ的激发温度分别作了计算。讨论了试剂分子裂解产物的光谱干扰问题。     

有机试液的电感耦合等离子体原子发射光谱分析 Ⅰ.实际应用的若干方面

本文从七个方面介绍了ICP-AES在有机试液直接分析中的应用:(1) 油类样品分析;(2) 酒样直接分析;(3) 溶剂萃取分离富集-ICP光谱分析;(4) 基于生成挥发性金属有机化合物的ICP进样方法;(5) 有机试液分析中的其它进样方法;(6) 有机介质中非金属元素的ICP-AES测定;(7) ICP-AES作为色谱法的检测器。     

Evaluation of an ultrasonic nebulizer-membrane separation interface (USN-MEMSEP) with ICP-AES for the determination of trace elements by solvent extraction

The introduction of volatile organic solvents and metal organic complexes into an inductively coupled plasma (ICP) is problematic due to overloading and pyrolysis effects. These include carbon built up in the torch and spectral interferences. As a consequence, solvent extraction as a method for preconcentrating trace metals for the determination by ICP has been limited. In this report a commercial ultrasonic nebulizer-membrane separation interface (USN-MEMSEP) for the direct introduction and separation of organic solvents using ICP atomic emission spectrometry (AES) and a sequential spectrometer has been evaluated for solvent extraction of chelated trace metals. The ability of the MEMSEP to separate volatile organic flows from metal aerosols has been demonstrated by determining the recoveries of several transition metals in an oil-based methyl-isobutyl ketone (MIBK) standard relative to an aqueous solution. However, low recoveries of several metal chelates have been found evidently due to the volatilization of the organic metal species at the boiling point of MIBK (160° C). Moreover, the multielement capability and limits of detection have been limited due to sequential atomic emission detection. Advantages of the technique include enhanced limits of detection (LODs) and reduced plasma and spectral interferences.     

Evaluation of an ultrasonic nebulizer-membrane separation interface (USN-MEMSEP) with ICP-AES for the determination of trace elements by solvent extraction

The introduction of volatile organic solvents and metal organic complexes into an inductively coupled plasma (ICP) is problematic due to overloading and pyrolysis effects. These include carbon built up in the torch and spectral interferences. As a consequence, solvent extraction as a method for preconcentrating trace metals for the determination by ICP has been limited. In this report a commercial ultrasonic nebulizer-membrane separation interface (USN-MEMSEP) for the direct introduction and separation of organic solvents using ICP atomic emission spectrometry (AES) and a sequential spectrometer has been evaluated for solvent extraction of chelated trace metals. The ability of the MEMSEP to separate volatile organic flows from metal aerosols has been demonstrated by determining the recoveries of several transition metals in an oil-based methyl-isobutyl ketone (MIBK) standard relative to an aqueous solution. However, low recoveries of several metal chelates have been found evidently due to the volatilization of the organic metal species at the boiling point of MIBK (160° C). Moreover, the multielement capability and limits of detection have been limited due to sequential atomic emission detection. Advantages of the technique include enhanced limits of detection (LODs) and reduced plasma and spectral interferences.     

Alternative organic solvents for HILIC separation of cisplatin species with on-line ICP-MS detection

Several low volatile organic solvents were evaluated as organic modifiers in eluents for HILIC separations of cisplatin species to optimize the on-line coupling of HILIC to inductively coupled plasma MS (ICP-MS). The aim was to identify a solvent giving low solvent vapor loading of the ICP, to maximize analyte sensitivity and minimize carbon depositions on instrumental parts, while retaining chromatographic performance. The best overall performance of the HILIC-ICP-MS system for the analysis of cisplatin was achieved using 1,4-dioxane as eluent, yielding high retention and an HILIC type retention mechanism, at the expense of a 50% drop in column efficiency due to the higher viscosity of 1,4-dioxane compared to the more commonly used HILIC solvent ACN. Using 1,4-dioxane as solvent in HILIC provides the best compromise between carbon deposition and separation efficiency among a series of high-boiling water-miscible solvents tested.     

Modification and optimization of a 50 MHz inductively coupled argon plasma with special reference to analyses using organic solvents

The torch and nebulizer of an existing argon ICP system were modified and the system was (re-) optimized for aqueous and organic liquids. The paper describes the design considerations and construction of(1) a new, streamlined torch including a torch base used in this study, where a demountable rather than a prealigned version of the torch was preferred;(2) a cross-flow pneumatic nebulizer with adjustable teflon capillaries including a spray chamber with flow spoiler, concentric aerosol pick-up tube, and “U” tube with unequal legs to smooth the flow of wasted liquid to the drain.The (re)-optimization of the ICP system for analysis of aqueous solutions with inorganic matter or with both inorganic and organic matter is discussed in the light of earlier work in this laboratory regarding the selection of “compromise conditions” and the choice of representative spectral lines and measurement criteria for establishing such compromise conditions. In this context the authors consider the concepts of norm temperature and “hard” and “soft” lines, as well as recent results of measurements of spatial distributions in ICPs. The authors further describe experiments aimed at the optimization of the operating conditions of an “organic ICP” using methyl isobutyl ketone (MIBK) as organic solvent. Trends of net line and background signals and signal-to-background ratios with the ICP parameters (power; outer, intermediate and carrier gas flow; observation height; liquid feed rate) are reported, and a rational choice of compromise conditions for the ICP is argued.Performance characteristics of the modified ICP system, such as detection limits, precision and interference level, achieved under compromise conditions, have been communicated in a previous report [Spectrochim. Acta36B, 1031 (1981)] to demonstrate the capabilities of the system for analysis of aqueous solutions. Detection limits in MIBK and oil diluted in MIBK are reported in the present work as an illustration of the performance of the system when used for organic liquid analysis.     

Sedimentary siloxanes: A depositional history

A Puget Sound sediment core has been quantitatively analyzed for organic silicon content, as derived from post-1945 release of poly(organo)-siloxanes (silicones). The sedimentary silicone data record and preserve at depth, a smeared event horizon, or first appearance of silicone in the sediment column. Core samples older than 50 years showed no detectable silicone as measured by a new procedure utilizing inductively coupled plasma (ICP) emission spectroscopy after solvent extraction to collect the silicone from gram-sized sediment core samples.     

用于锆稳定同位素测定的化学分离技术

本文采用ＨＤＥＨＰ／环己烷体系萃取锆和钼，并将两 发离以便测定锆的稳定同位素，此外，还研究了作为同 素稀释剂的ＺｒＯ２固体粉末的微波溶样法。     

Excitation temperature and electron density in the inductively coupled plasma—aqueous vs organic solvent introduction

Using a photodiode array spectrometer, spatially resolved Fe I, excitation temperatures and electron densities have been measured for an ICP with both water and xylene solution introduction. The excitation temperature is lower in the ICP with organic aerosol than in the ICP with aqueous aerosol at a fixed power and height. For an ICP with organic aerosol the input power must be increased by approx. 0.5 kW to simulate the temperatures reached in an aqueous ICP.     

FI溶剂萃取与ICP-AES联机的研究水样中微量铜的测定

本文建立了用FI-溶剂萃取-ICP-AES测定水样中微量铜的分析方法。选择了ICP-AES、超声雾化发生器及FIA的最佳工作条件。研究了溶液pH对用打萨腙-四氯化碳体系萃取铜的影响;有机相流速与水相流速之比例;萃取盘管长度等因素对萃取过程及等离子体放电的影响。分析了自来水样品及美国标准局标准水样中铜含量。统计了分析方法的精密度、检出限与实验条件下的富集倍数。