有机试液ICP光谱技术的发展

电感耦合等离子体(ICP)光谱法测定无机水溶液样品已得到广泛应用。由于试样处理简便和具有多元素同时测定能力,近十年来它在有机试液的分析方面也有许多实际应用,并已成为ICP光谱分析的一个重要专题。目前有机试液ICP光谱技术的研究主要集中在四方面:1.各种油类中金属杂质的测定。如燃料油及食用油中无机杂质的测定;润滑油中磨损金属的测定。2.有机溶剂萃取技术与ICP光谱法联     

电感耦合等离子体原子发射光谱法分析中有机溶剂效应

综述近年来电感耦合等离子体原子发射光谱法分析中有机溶剂效应,内容包括有机溶剂对等离子体物理特性的影响,有机溶剂对等离子体雾化进样系统的影响,有机溶剂对等离子体光谱特性的影响以及有机溶剂效应干扰消除,引用文献41篇.     

ICP-MS法测定电子级高纯硝酸中的金属杂质

用ICP-MS的不同状态（标准状态、冷等离子体技术、碰撞池技术）直接测定电子级高纯硝酸中的34个痕量金属杂质,用铟作内标可补偿基体效应,方法检出限为0.1-70ng/L,加标回收费率为90%-110%,相对标准偏差为4.0%,样品测定结果与ICP-AES测定结果基本一致。     

膜去溶进样高分辨电感耦合等离子体质谱法测定半导体级氢氟酸中杂质元素

利用高分辨电感耦合等离子体质谱法测定半导体级高纯氢氟酸中的痕量金属杂质,用膜去溶进样系统直接进样检测,无需前处理、快速,避免了在样品前处理时的污染问题。高分辨电感耦合等离子体质谱法可以消除多分子离子干扰,降低检出限,提高定量准确性。方法的检出限为0.09～37.07ng/L,加标回收率为92.3%～116.8%。方法简单,结果可靠,适用于高纯氢氟酸中痕量元素的快速测定。     

金属有机化合物中过渡金属的原子吸收分光光度法测定

本文报导应用火焰原子吸收分光光度法对金属有机化合物中过渡金属铜、镍、钴、铁、钼及铬的定量测定。我们将金属有机化合物溶解在适当的有机溶剂或水中,不必分离基体,即可用标准加入法直接进行测定。操作简单,速度快,相对误差<0.4％。     

铟(Ⅲ)-铬天青S-烷基三甲基溴化铵-含氧有机溶剂多元配合物显色反应中的有机溶剂化效应

系统研究了有机溶剂对多元配合物In-铬天青S-烷基三甲基溴化铵显色反应的溶剂化效应.发现与水混溶的乙醇、异丙醇、丙酮等含氧有机溶剂可以使多元配合物的分析性能优异化,大幅度地提高多元配合物显色反应的灵敏度和选择性.用这类体系测定了纯铝及铅中的微量铟.测定了配合物组成、有机溶剂化数、真正(?)值及表观稳定常数K.探讨了有机溶剂化效应的机理.     

电感耦合等离子体质谱法检测农作物土壤中的镉、锡、锰、锑、钒、钛、锶金属污染物残留

建立全自动石墨消解- 电感耦合等离子体质谱(ICP-MS)法检测农作物土壤中的镉、锡、锰、锑、钒、钛、锶金属污染物残留的分析方法.随机采集农作物土壤,取约200 g,置于烘箱中烘干,烘干后的样品用粉碎机粉碎,精密称取粉碎后的样品约0.25 g,置于聚四氟乙烯材质的消解罐内,按既定消解程序进行自动消解处理,得样品溶液,上...     

DMF和DMSO配位的金属十聚钨酸盐在非水溶剂中光致变色性质的研究

研究了某些DMF和DMSO配位的金属十聚钨酸盐在 3 种有机溶剂中的光致变色性质,通过ESR、NMR和可见吸收光谱的研究及对五价钨的测定,说明了光致变色性质的产生与金属阳离子无关,而取决于十聚钨酸根W₁₀O₃₂^4-、金属离子的配体及所采用溶剂。     

电感耦合等离子体发射光谱法测定地质样品中的钨、钼、锡

改进了电感耦合等离子体发射光谱法(ICP-AES)同时测定多金属矿石等地质勘查样品中钨、钼、锡的溶样方法。采取酸溶和碱熔结合,先用硝酸和高氯酸及氢氟酸溶样,用盐酸(1+1)浸取再过滤,滤渣及滤纸灰化后再碱熔,最后用电感耦合等离子体发射光谱法(ICP-AES)测定钨、钼、锡。克服了传统的酸溶法导致锡的测定结果偏低和碱熔法易堵塞ICP-AES矩管和雾化器的两大弊端,方法经国家一级标准物质验证,精密度和准确度均能达到日常分析的要求。     

毛细管色谱-质谱法测定环境大气中挥发性有机污染物

毛细管色谱-质谱法测定了环境大气中挥发性污染物。用液氧冷冻法和常温吸附法(TenaxGC)分别采集大气样品,然后用两种系统进行浓缩,并进入毛细管色谱-质谱体系,完成了有机污染物的定性定量分析。解决了一些色谱-质谱联用中的问题。并且还讨论了无分流进样问题,比较了两种采样方法。用此方法测定了某炼油厂环境大气中的污染物。     

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.     

Effects of trace levels of copper,chromium, and zinc ions on the performance of activated sludge

The effects of copper, chromium, and zinc ions, at trace levels, on the performance of a simulated activated sludge process were investigated. The results of batch adsorption experiments showed that the adsorption of copper, chromium, and zinc ions followed both the Langmuir and Freundlich isotherms. The presence of trace levels of these three metals not only reduced the adsorption rate of organic matters but also the chemical oxygen demand adsorption capacity (CAC) of the activated sludge. Metal ions competed with the organic substrate for adsorption binding sites on the surfaces of activated sludge bioflocs and reduced the CAC. Studies performed in a sequential batch reactor (SBR) showed that the presence of trace levels of heavy metal ions in wastewater affected the SBR performance to different extents depending on the hydraulic retention time (HRT). When the reactors were operated at short HRTs of 2.5 d or less, the presence of trace levels of heavy metal ions reduced substantially the CAC of activated sludge, which, in turn, affected significantly the performance of the SBR. However, under longer HRTs (e.g., 5d), the heavy metal ions in the wastewater reduced the CAC but had not significant effect on the chemical oxygen demand removal efficiency.     

Determination of trace elements in petroleum products by inductively coupled plasma techniques: A critical review

The fundamentals, applications and latter developments of petroleum products analysis through inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are revisited in the present bibliographic survey. Sample preparation procedures for the direct analysis of fuels by using liquid sample introduction systems are critically reviewed and compared. The most employed methods are sample dilution, emulsion or micro-emulsion preparation and sample decomposition. The first one is the most widely employed due to its simplicity. Once the sample has been prepared, an organic matrix is usually present. The performance of the sample introduction system (i.e., nebulizer and spray chamber) depends strongly upon the nature and properties of the solution finally obtained. Many different devices have been assayed and the obtained results are shown. Additionally, samples can be introduced into the plasma by using an electrothermal vaporization (ETV) device or a laser ablation system (LA). The recent results published in the literature showing the feasibility, advantages and drawbacks of latter alternatives are also described. Therefore, the main goal of the review is the discussion of the different approaches developed for the analysis of crude oil and its derivates by inductively coupled plasma (ICP) techniques.     

Exploring the Performance Improvement of the Oxygen Evolution Reaction in a Stable Bimetal–Organic Framework System

Despite wide applications of bimetallic electrocatalysis in oxygen evolution reaction (OER) owing to their superior performance, the origin of the improved performance remains elusive. The underlying mechanism was explored by designing and synthesizing a series of stable metal–organic frameworks (MOFs: NNU‐21–24 ) based on trinuclear metal carboxylate clusters and tridentate carboxylate ligands. Among the examined stable MOFs, NNU‐23 exhibits the best OER performance; particularly, compared with monometallic MOFs, all the bimetallic MOFs display improved OER activity. DFT calculations and experimental results demonstrate that introduction of the second metal atom can improve the activity of the original atom. The proposed model of bimetallic electrocatalysts affecting their OER performance can facilitate design of efficient bimetallic catalysts for energy storage and conversion, and investigation of the related catalytic mechanisms.     

活化污泥强化工艺对重金属的去除效果研究

重点研究了活化污泥法强化一级处理对城市污水中重金属离子的去除效果。以实际生活污水和Cd、Cu、Zn、Cr6+、Pb、Mn六种城市污水中常见的重金属离子配水,采用活化污泥法的正常工艺条件,发现这几种金属离子去除的难易顺序为:Cd>Pb>Cu>Zn>Mn>Cr6+。水中的重金属离子与有机物间存在竞争吸附作用,共存时双方的去除效果都有所下降,但对Cd、Pb来说,有机物的存在则可以提高其去除效果。     

Determination of phosphorous in organic compounds and metal complexes by inductively-coupled plasma atomic emission spectrometry

Phosphorus is determined by inductively-coupled plasma atomic emission spectrometry at 213.618 nm. Different types of organic and inorganic phosphorus compounds and metal complexes were examined after direct dissolution in water, aqueous ethanol or acid, or after decomposition by oxygen flask combustion or Kjeldahl digestion; results were within the usual limit of precision and accuracy for such determinations. The effect of small (<20%) ethanol concentrations in the aqueous solution on the signals obtained from a low-power (1200 W) argon plasma is examined and discussed.     

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。     

Cellulase Hydrolysis of Unsorted MSW

A recent development in waste management and engineering has shown that the cellulase can be used for the liquefaction of organic fractions in household waste. The focus of this study was to optimize the enzyme hydrolysis of thermally treated municipal solid waste (MSW) by the addition of surfactant. Concurrently, the enzyme performance was analysed on pure cellulose in a solution of MSW wastewater. Results showed no effect of surfactant addition to the hydrolysis media as measured by viscosity and particle size distribution. MSW treatment wastewater was found to contain a high amount of calcium, potassium, sodium, chloride and others that may affect cellulolytic enzymes. Cellulase performance showed no effect of adding the metal ion-chelating agent EDTA to the solution. The cellulases were stable, tolerated and functioned in the presence of several contaminants.     

Oxalic acid cross-linked sodium alginate and carboxymethyl chitosan hydrogel membrane for separation of dye/NaCl at high NaCl concentration

Dye desalination is a challenge in the treatment of textile wastewater with high salt concentration. It is imperative to develop salt resistance membrane that is from sustainable materials to effectively treat dye/salt mixtures. And most polymer membrane materials are non-renewable petrochemical resources.In this paper, a green hydrogel membrane(CMCS-OA-Na Alg) was prepared by non-metallic ions of oxalic acid(OA) cross-linking of two natural macromolecules of sodium alginate(Na Alg) and carboxym...