X-ray Fluorescence Determination of Heavy Metals in Solutions after the Preconcentration of Their Pyrrolidinedithiocarbamate Complexes on Cellulose Filters

Conditions of the quantitative extraction of Co, Cu, Fe(III), Ni, Pb, V(IV), and Zn from solutions on cellulose filters in the form of pyrrolidinedithiocarbamates obtained in flow were found. The elements were determined on filters by X-ray fluorescence spectrometry. The detection limits were 0.1, 1.2, 0.4, 0.2, 0.2, 0.4, and 0.3 g on the filter, respectively. The relative standard deviation of the results of the determination was no higher than 8% for the amounts of elements on the filter of 5–50 g. The accuracy of the determination of elements by the proposed sorption–X-ray fluorescence method in river and sea water and in soil extract was verified by the added–found method.     

Preconcentration of Trace Elements in Water for Speciation Studies

Trace element speciation has recently become one of the most important problems in water analysis. Proper combination of preconcentration techniques with instrumental determination methods is essential to speciation analysis, because sensitivity and selectivity of direct determination methods are generally lacking. The present paper describes such preconcentration techniques as filtration, centrifugation, flotation and sorption, which have been developed in the author's laboratory for the speciation of heavy metals in river and pond waters by electron microscopy, X-ray microanalysis and chemical analysis. The application of freeze concentration to the speciation of silica in high-purity waters is also discussed.     

8－羟基喹啉纤维微柱分离富集ICP－AES测定多种痕量元素

制备了８－羟基喹啉纤维滤纸片，作为微柱填充物，同时富集了九种痕量元素，并分离了样品中的高盐组分。富集后的痕量组分采用电感耦合等离子体原子发射光谱法（ＩＣＰ－ＡＥＳ）测定，回收率为９０％～１０２％。     

Preconcentration of Simazine from Aqueous Solutions with an Immunosorbent and Its Quantitative Determination

The optimal conditions were found for sorption preconcentration of Simazine (herbicide of sym-1,3,5-triazine group) from aqueous solution with immobilized antibodies. The main characteristics of immobilized antibodies as sorbents for Simazine were determined.     

Chelating 2,2′-Diaminodiethylamine Cellulose Filters and X-ray Fluorescence for Preconcentration and Trace Analysis of Natural Waters

Abstract

The 2,2′-diaminodiethylamine (DEN) functional group can be expected to have ideal properties for the chelation of transition metals and their collection from aqueous solutions, independent of the alkali and alkaline earth ions concentration. Introducing DEN into cellulose filters allows straightforward preconcentration of trace cations by a simple filtration step, and the DEN-filter constitutes a suitable target for X-ray fluorescence (XRF) analysis. The linearity between the XRF-response on the loaded DEN-filter and the trace cation concentration in the solution appears excellent, up to a total filter capacity of ca. 3 μeq.cm^?2. The detection limits are around 0.5 μg. l^?1 in most practical cases. Accuracy and precision are around 10%. The applicability of the proposed procedure is illustrated on a comparative basis by XRF-analysis of drinking water and surface water, after preconcentration by DEN-filtration and by alternative procedures.     

Biosorption of Toxic Elements from Multicomponent Solutions by Microfungal Biomass

The results of experiments on sorption of toxic elements from multicomponent solutions by microfungal biomass are presented. In the elements group extraction processes the species and strain specificity of micromycetes manifests itself. Talaromyces funiculosus biomass possesses the highest (1.5–3 times higher) sorption indicators compared to Cladosporium cladosporioides and Trichoderma aureoviride. Within each species, the strains, isolated from technogenic substrates, are also characterized by higher sorption indicators. The affinity of chemical elements to fungal biomass as a sorbent corresponds to the following series: Bi ≈ Sn ≈ Pb ≈ Fe > Hg ≈ (Sb) ≥ Cr ≥ Cd > Cu ≈ Se > Zn ≈ V ≥ Co ≈ Mn ≈ As ≈ Ni ≈ Sr ≈ (Sb). The use of the analytical scanning electron microscopy has made it possible to detect particles of various composition and morphology on fungal biomass. The mechanism of their formation is proposed.     

采用吸附树脂Amberlite XAD-4从水溶液中富集痕量元素

本文采用短吸附柱(10×60mm,充填高度24mm)研究了非离子性吸附树脂AmberliteXAD-4从水溶液中对16种金属元素的氢氧化物,二硫代氨基甲酸衍生物的配合物和二甲酚橙配合物的吸附行为。难溶金属化合物在树脂上的吸附率与溶液pH值的关系与采用活性碳作吸附剂的情况十分相似。而含有亲水基团的二甲酚橙螯合物不被树脂吸附。对吸附于树脂上的痕量元素的洗脱以及采用火焰原子吸收光谱法测定丙酮富集液中的金属元素问题也进行了讨论。     

Determination of Phenol and Guaiacol in Aqueous Solutions Using Extraction-Chromatographic Preconcentration

Compositions of stationary phases based on tributyl phosphate and dicyclohexano-18-crown-6 were optimized for the efficient extraction of phenol and guaiacol from aqueous solutions. Procedures were developed for the total and selective determination of these compounds in aqueous solutions, in particular, at trace level.     

Preconcentration of pesticides from waters

Summary A procedure for the preconcentration of pesticides from water is described using the sorption on an organic sorbent with following desorption by means of an organic solvent. The usefulness of a few sorbents (Separon SE, Tenax GC, Porapak Q, Separon SI C 18) was compared on the basis of several factors influencing the sorption. The experiments showed the excellent suitability of Separon SI C 18 for this purpose.

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Anreicherung von Pesticiden aus Wässern

Zusammenfassung Die Anreicherung von Pesticiden aus verschiedenen Wässern und durch Sorption auf einem organischen Sorbent und anschließende Desorption mit einem organischen Lösungsmittel wird durchgeführt. Die entsprechenden Eigenschaften einiger Sorbentien (Separon SE, Tenax GC, Porapak Q, Separon SI C 18) wurden auf Grund von Parametern, die die Sorptionseffektivität beeinflussen, verglichen. Die Untersuchungen erwiesen die vorzüglichen Eigenschaften von Separon SI C 18 für den genannten Zweck.

     

An in-syringe La-coprecipitation Method for the Preconcentration of Oxo-anion Forming Elements in Seawater Prior to an ICP-MS Measurement

A lanthanum (La) coprecipitation method with low sample consumption was explored for the preconcentration of oxo-anion forming elements prior to a measurement by inductively coupled plasma mass spectrometry (ICP-MS). The preconcentration procedure was composed of two main steps: (1) the formation of a coprecipitate with the lowest possible La and (2) the redissolution of target analytes with minimal use of nitric acid, and the elimination of high concentration La from the analysis sample. Each step was performed in a 25 mL-volume syringe to reduce the sample consumption and to avoid contamination from the experimental environment. Various parameters, such as the concentration and volume of La added into the sample solution, the precipitation pH, the aging time, and the volume of HNO(3) were optimized to obtain good recoveries and high detection sensitivities for V, As, Sb, and W, which could be hardly recovered by solid-phase extraction using a chelating resin. The obtained method was evaluated through the analysis of seawater reference materials (CASS-4 and NASS-5). The recoveries exceeded 80%, and the observed values were in good agreement with the certified values.     

Sorption Recovery of Transplutonium Elements from Nitric Acid Solutions with Arsenazo Group Reagents

Sorption recovery of actinides and lanthanides from nitric acid solution with arsenazo group reagents, activated carbon modified with these reagents, and chelating sorbents containing arsenazo functional groups was studied.     

Studies on the Uptake of Rare Earth Elements on Polyacrylamidoxime Resins from Natural Concentrate Leachate Solutions

Synthesis of poly(acrylamidoxime) resin from polyacrylonitrile performed with different crosslinking ratios 2, 5, and 10 wt% of divinylbenzene as crosslinking agent, using methylbenzoate and dioctylphthalate as pore producing solvent, the reaction mixture occurred under nitrogen. Studies carried out on diluted solution from rare earth elements (REEs) concentrate contains impurities as Cu²⁺, Ni²⁺, Zn²⁺, Fe³⁺, Al³⁺, Si⁴⁺, Th⁴⁺, U⁶⁺, Ca²⁺, and K⁺. Changing some parameters as pH of the solution, time of feeding and type of acid as HCl, HNO₃, H₂SO₄. The adsorption efficiency of resin is in the order pH 6 > pH 5 > pH 4 > pH 2 with excluding pH 6 due to the precipitation of some of REEs with the impurities and complete precipitation of Dy ion during pH adjustment, the adsorption in HNO₃ > HCl > H₂SO₄ media.     

Determinations of Some Trace Metals in Dialysis Solutions by Atomic Absorption Spectrometry After Preconcentration

Abstract

A method is presented for the determination of copper, lead, iron, cadmium, cobalt and nickel in dialysis solution at μg/1 level by atomic absorption spectrometry after preconcentration. The preconcentration is based on chelate formation of the investigated metals with ammonium pyrrolydine dithiocarbamate and on retention of the chelates on Amberlite XAD-4 in a short column. The relative standard deviations for the determinations were found to be lower than 0.08.     

流动注射在线柱预富集-电感耦合等离子体原子发射光谱测定痕量金属元素

本文报道了流动注射在线柱预富集ICP光谱测定痕量金属的方法,以meso-四(4-磺基苯)卟啉为柱前衍生试剂,硅胶作固定相和盐酸作洗脱液,对痕量金属离子Cu、Mn、Ni、Fe、Pb、Cd进行在线预富集检测。在给定实验条件下,方法的富集倍数为9.3～11.3,检出限和测定的相对标准偏差(n=6)分别在0.32～26.8ng/ml和1.3％～3.0％范围内。方法用于小牛肝和西红柿叶样品分析,结果与参考值吻合。     

低空白镍锍试金预富集中子活化分析测定地球化学标准物质中的铂族元素

研究了镍锍试金预富集中子活化分析测定岩石样品中的铂族元素。纯化捕集剂氧化镍,大大降低了化学分离全流程铂族元素的空白。取样量为50g时,所需溶剂各元素的空白值为(ng/g):Pt<0.05、Pd<0.05、Os<0.01、Ru<0.05、Rh<0.05、Ir=0.002。用平面锗探测器测定Rh使测定下限降低了两个数量级,对几种国标地球化学标准物质的测定结果与推荐值基本符合。