Trace anion determination in concentrated hydrofluoric acid solutions by two-dimensional ion chromatography II. Method performance study with a hydroxide eluent and a low noise suppressor

The two-dimensional ion exclusion chromatography/ion chromatography (ICE-IC) approach is considered to be the method of choice for the determination of trace anions in concentrated hydrofluoric acid (48-50%, w/w). In order to achieve lower detection limits, this method was for the first time used with electrolytically generated and purified hydroxide eluents in combination with a low noise electrochemical suppressor. Compared to carbonate based eluents, the achieved gain in peak height sensitivity for chloride, sulfate, nitrate and phosphate is a factor of 6, 7, 16 and 13, respectively. The instrumental detection limits, based on the background noise, are 2, 0.2, 0.4 and 1.4 microg/kg HF 50% (w/w) for the same anions. Their method detection limits, calculated according to SEMI, are all within the 6-10microg/kg HF 50% (w/w) range and thus at least 10 times lower than the current Tier C grade requirements. The chromatographic run time could be shortened with some 10 min by the use of a relatively fast high-capacity hydroxide selective anion exchange column.     

Chemical separation and inductively coupled plasma–atomic emission spectrometric determination of seventeen trace metals in thorium oxide matrix using a novel extractant – Cyanex-923

Comprehensive studies have been carried out on the extraction behaviour of thorium matrix vis-a-vis 17 trace metallic elements using a novel extractant viz. Cyanex-923. The near total extraction of thorium and quantitative separation of these metals has been established using inductively coupled argon plasma–atomic emission spectrometry (ICP–AES). The recovery of few representative elements has been confirmed by radio-active tracer studies. The studies carried out here have enabled determination of μg/l amounts of all analyte elements with a precision of better than 1% RSD with prior chemical separation from as low as 1 g thorium sample in just five chemical extractions.     

Analysis and Speciation of Traces of Arsenic in Environmental,Food and Industrial Samples by Voltammetry: a Review

Voltammetric approaches for the determination of arsenic and speciation at trace levels are critically appraised in a review covering the literature from 1970 to 2002. Special attention is devoted to stripping modes and to issues related to the choice of working material and supporting electrolyte. A section is dedicated to the management of real samples and aspects of sample preparation. An extensive compilation, organized by real sample type, gathers essential experimental conditions. Potentiometric stripping analysis is introduced for sake of comparison. The coupling of voltammetric detection or preaccumulation with FIA, chromatography, capillary electrophoresis and ICP techniques is also addressed.     

A new method for the quantitative analysis of organochlorine pesticides and polychlorinated biphenyls

A simple method is described for the quantitative determination of organochlorine pesticides and polychlorinated biphenyls (PCB's) in water at the sub-ppb level. A micro gas-phase extractor advantageously replaces other preconcentration and purification techniques. The extract is analyzed by capillary gas chromatography without further enrichment. The recovery at the ppb level was nearly 100% for organochlorine pesticides and more than 80% for PCB's. The complete procedure including sample preparation, steam distillation-extraction, and capillary gas chromatographic analysis is carried out in less than four hours.     

Zur Anreicherung der stabilen Isotope des Schwefels durch Fest-Flüissig-Austausch unter Verwendung von Ionenaustauschern

An verschiedenen Systemen chemischer Verbindungen wurden Versuche zur Anreicherung des stabilen Isotopes ³⁴S unter Verwendung der Ionenaustauscher Wofatit L 150, SBW und SBK nach den Methoden der Frontalchromatographie und der Bandenverdrāngungschromatographie ausgeführt. Beim Isotopenaustauschsystem Hydrogensulfit (am Ionenaustauscher)/Schwefeldioxid (in wäβriger Lösung) wurden Verfahrensweise und Betriebsparameter hinsichtlich des Anreicherungsgrades optimiert. Mit Hilfe einer einfachen Methode gelang es, aus den Versuchsergebnissen Werle für den elementaren Trennfaktor und die Trennstufenhöhe zu berechnen.     

ICP—AES法测定人体胎盘血清中15种微量元素

用ICP-AES法测定了人体胎盘血清中15种微量元素。本法具有灵敏度较高,校正曲线的线性范围宽,基体效应小,尤其是进样量少等优点。本法可同时测定多种元素。     

高纯金属镨中痕量稀土杂质的电感耦合等离子体原子发射光谱分析及光谱干扰的校正

本文提出了PGS-2型平面光栅光谱仪(色散率0.18纳米,二级光谱)与PlasmaTherm ICP-5000D射频发生器联用,乙醇预去溶方式进样,同时直接测定高纯金属镨中5个痕量稀土杂质元素的方法。并讨论了基体浓度对检出限的影响以及光谱干扰及其校正方法。当样品溶液中镨的浓度为5毫克/毫升时,测定下限分别为镧、钕和钐0.002%,铈0.003%和钇0.0005%。获得了良好的实验结果,其相对标准偏差为1.2-6.2%。     

Cardinality enrichment of flexible cross correlation (FCC) code for SAC-OCDMA system by alleviation interference scheme (AIS)

In this paper, we propose an alleviation interference scheme (AIS) for spectral amplitude coding (SAC) – optical code division multiple access (OCDMA) coding system approaches. The AIS SAC-OCDMA systems is demonstrated by utilizing the new flexible cross correlation (FCC) code. The FCC code has advantages, such as flexibility in-phase cross-correlation at any given number of users and weights, as well as effectively reduces the impacts of phase-induced intensity noise (PIIN) and has the multiple-access interference (MAI) cancelation property. The results indicated good performance whereas the FCC (W = 4, K = 150) AIS SAC-OCDMA coding system offers 66%, 172%, 650% and 900% percentage of cardinality enrichments as a contrast to DCS (W = 4, K = 90), MDW (W = 4, K = 55), MFH (W = 4, K = 20) and Hadamard (W = 8, K = 15) codes, respectively. Finally, the FCC AIS SAC-OCDMA coding system has low effective receive power Psr = −21 dBm which is expected to be more significant for future SAC-OCDMA coding systems without requiring any amplification at the receiving plant.     

ICP-AES测定7种花茶中8种微量元素的含量和溶出率

采用微波消解样品,电感耦合等离子体-原子发射光谱法测定了金银花、玫瑰茄、玉蝴蝶、仙人草、菊花、薰衣草、腊梅等7种花茶中Fe、Mn、Cu、Zn、Ni、Cr、Cd和Pb等元素的含量及其溶出率。结果表明,花茶中Fe含量较高,重金属Cr、Cd和Pb含量普遍较低,花茶中Cu、Zn、Mn和Ni的溶出率相对较高,Fe的溶出率较低,有害的重金属Cd、Pb和Cr的溶出率很低,此测定结果可为探讨花茶的保健作用与微量元素的相关性提供科学数据。     

ICP-MS法测定不同采收时间宽叶荨麻中微量元素含量

采用微波消解,ICP-MS法分析不同采收时间宽叶荨麻中18种微量元素Al,Ba,Ca,Co,Cr,Cu,Fe,K,Li,Mg,Mn,Mo,Na,Ni,P,Pb,S和Zn的含量。该方法的相对标准偏差在1.2%～5.3%之间,加标回收率在95.4%～101.2%之间。结果表明宽叶荨麻中K,P,S,Ca,Na含量较高;Fe,Mg,Mn,Zn含量次之;有潜在生理毒性的元素Al,Cr,Pb的含量较低,并且在宽叶荨麻中微量元素呈现明显的季节性动态变化,此结果为进一步研究宽叶荨麻药理药效与微量元素的关系以及更好的开发这一资源提供理论数据。