Rotating Coiled Columns Research Articles

A Comparative Study of the Dynamic Fractionation of Rare-Earth Elements in Soils Using a Rotating Coiled Column and a Microcolumn

Rare earth elements (REEs) are currently used in fertilizers, but their behavior in the soil–plant system remains poorly studied. The assessment of the binding of REEs to various organomineral phases of soils remains an important task. Using soddy-podzolic soil and typical chernozem as examples, we performed a comparative study of the dynamic fractionation of REEs in a rotating coiled column (RCC) and a microcolumn (MC). We isolated the exchangeable fraction, specifically adsorbed fraction, and fractions bound to manganese oxides, bound to organic matter, and bound to amorphous and weakly crystallized iron and aluminum oxides using, 0.05 M Ca(NO3)2, 0.43 M CH3COOH, and a 0.1 M NH2OH·HCl solution (pH 3.6), a 0.1 M K4P2O7 solution (pH 11.0), and a 0.1 M (NH4)2C2O4 solution (pH 3.2), respectively. Concentrations of elements in the initial samples and eluate fractions were determined by atomic emission spectrometry and inductively coupled plasma mass spectrometry. The results suggest that the main extractable REE form (up to 40% of the total content) is provided by organometallic complexes extracted with a 0.1 M K4P2O7 solution. For chernozem (soils with a high content of organic matter), fractionation in the RCC and MC yielded comparable results. For soddy-podzolic soil, some differences were observed in the isolation of the first three fractions: exchangeable, specifically adsorbed, and bound to manganese oxides. Both RCC and MC can be successfully used for the dynamic fractionation of REE in soils; however, it is preferable to use an MC in analyzing many samples as a simpler and more affordable device.

Separation of Pt(IV), Pd(II), and Rh(III) from Chloride Solutions by Multistage Extraction Using Nitrogen-Containing Extractants

This article demonstrates possible separation of Pd(II), Pt(IV), and Rh(III) ions from chloride solutions by solvent extraction in rotating coiled columns (RCC). The most common reagents used for extraction of platinum metals were selected as extractants: trioctylamine (TOA), methyltrialkylammonium chloride (MTAA), tributyl phosphate (TBP), and relatively new reagent—N,N,N',N'-tetra-n-octyldiglycolamide (TODGA). The completeness of extraction of platinum metals from individual and mixed hydrochloric acid and chloride solutions has been analyzed as a function of the essence and concentration of extractant, acidity of the analyzed solutions, and other factors. Optimum conditions of quantitative extraction of the metals from model hydrochloric acid and chloride solutions into the extractant phase have been determined, including subsequent selective separation at the re-extraction stage. A flowchart has been proposed for multistage extraction of Pd(II), Pt(IV), and Rh(III) using 0.05 M MTAA solution in toluene as a stationary phase in RCC. The flowchart includes extraction of Pd(II) and Pt(IV) ions from the solution (0.1 M HCl + 30 g/L Cl–) into the organic phase upon simultaneous separation of Rh(III) remaining in the aqueous phase and consecutive re-extraction of Pd(II) and Pt(IV) from the organic phase using 0.01 M solution of thiourea in 0.1 M HCl and 1 M solution of thiourea in 0.5 M HCl, respectively. The flowchart has been verified for separation of platinum metals in the production process of preset composition. The degree of metal extraction after processing by 0.05 M solution of MTAA in in toluene and consecutive re-extraction by solutions of thiourea is 99.5% for rhodium(III), 99.9% for palladium(II), and 97.4% for platinum(IV). The extracted aqueous phases of rhodium and platinum after output from the column did not contain impurities of other platinum metals. In the aqueous fraction of palladium, the platinum content was 0.5%.

Study of the Mobility of Cerium Oxide Nanoparticles in Soil Using Dynamic Extraction in a Microcolumn and a Rotating Coiled Column

Currently, nanomaterials are widely used in various fields of human activity, which inevitably leads to their release into the environment, and soils are one of the main reservoirs for nanoparticles. As nanoparticles can be particularly toxic to living organisms, the development of new approaches to the assessment of their behavior and mobility in soils is an important task. In this paper, the analytical possibilities of the dynamic extraction of CeO2 nanoparticles in a microcolumn (MC) and a rotating coiled column (RCC) are studied to evaluate the behavior of nanoparticles in soil. Differential and integral elution curves of CeO2 nanoparticles from the soil were obtained based on the data of eluate analysis by inductively coupled plasma–mass spectrometry. After pumping 100 mL of water through a microcolumn and a rotating coiled column, 0.15 and 1.37 µg of CeO2 nanoparticles are leached from the soil, respectively, which is 0.2 and 1.6% of the nanoparticles introduced. The ratio of CeO2 nanoparticles and soil mineral particles is two times higher in the MC eluate. It is found that the rotating coiled column enables the estimation of nanoparticles maximum mobility of nanoparticles in soil because of the minimization of the effect of its structure on their transport. The microcolumn, preserving the soil structure, ensures the estimation of the mobility of nanoparticles in a real soil column most accurately. We also studied the effect of the modification of the surface of CeO2 nanoparticles with citric acid on their mobility in soil. CeO2 nanoparticles modified with citric acid have higher mobility in soil compared to unmodified nanoparticles.

SEPARATION OF P t (IV), P d (II) AND R h (III) FROM CHLORIDE SOLUTIONS BY MULTISTAGE SOLVENT EXTRACTION USING NITROGEN-CONTAINING EXTRACTANTS

The possibility of Pd (II), Pt (IV), and Rh (III) separation from chloride solutions by solvent extraction in rotating coiled columns (RCC) is demonstrated. The reagents most frequently used in extraction of platinum metals were selected as extractants: trioctylamine (TOA), methyltrialkylammonium chloride (MTAA), tributylphosphate (TBP), N, N, N',N'-tetra-re-octyldiglyTOlamide (TODGA). The completeness of extraction of the platinum group metals from individual and mixed hydrochloric acidic and chloride solutions was studied depending on the nature and concentration of the extractant, acidity of the test solutions and other factors. Optimal conditions for the quantitative extraction of metals from model hydrochloric acidic and chloride solutions and subsequent selective separation at the stripping stage are specified. A scheme of multistaged extraction separation of Pd (II), Pt (IV), and Rh (III) from chloride solutions using a 0.05 M solution of MTAA in toluene as a stationary phase in RCC is proposed. The scheme includes extraction of Pd (II) and Pt (IV) ions from a chloride solution (0, 1 M HCl + 30 g/liter NT) into the organic phase with simultaneous separation of Rh(III) remaining in the aqueous phase, and sequential stripping of Pd (II) and Pt (IV) from the organic phase with a 0.01 M solution of thiourea in 0.1 M HCl and a 1 M solution of thiourea in 0.5 M HCl, respectively. The scheme was tested in separation of the platinum group metals from the technological solution of a given composition. The degree of metal extraction with a 0.05 M MTAA solution in toluene and sequential stripping with thiourea solutions is 99.5% for Rh (III), 99.9% for Pd (II), and 97.4% for Pt (IV). The separated water fractions of rhodium and platinum after leaving the column did not contain impurities of other platinum metals whereas the water fraction of palladium contained 0.5% Pt.

Assessment of elemental composition and properties of copper smelter-affected dust and its nano- and micron size fractions

A comprehensive approach has been developed to the assessment of composition and properties of atmospherically deposited dust in the area affected by a copper smelter. The approach is based on the analysis of initial dust samples, dynamic leaching of water soluble fractions in a rotating coiled column (RCC) followed by the determination of recovered elements and characterization of size, morphology and elemental composition of nano-, submicron, and micron par ticles of dust separated using field-flow fractionation in a RCC. Three separated size fractions of dust (<0.2, 0.2-2, and >2 μm) were characterized by static light scattering and scanning electron microscopy, whereupon the fractions were analyzed by ICP-AES and ICP-MS (after digestion). It has been evaluated that toxic elements, which are characteristics for copper smelter emissions (As, Cu, Zn), are accumulated in fraction >2 μm. At the same time, up to 2.4, 3.1, 8.2, 6.7 g/kg of As, Cu, Zn, Pb, correspondently, were found in nanoparticles (<0.2 μm). It has been also shown that some trace elements (Sn, Sb, Ag, Bi, and Tl) are accumulated in fraction <0.2, and their content in this fraction may be one order of magnitude higher than that in the fraction >2 μm, or the bulk sample. It may be assumed that Sn, Sb, Ag, Bi, Tl compounds are adsorbed onto the finest dust particles as compared to As, Cu, Zn compounds, which are directly emitted from the copper smelter as microparticles.

Comparative study of methods for evaluating the mobility of element species in contaminated soil and technogenic sand under batch and dynamic extraction

A comparative study of the batch and dynamic extraction methods used to evaluate the physicochemical “mobility” of element species in environmental samples was carried out using samples of contaminated soils and technogenic sands of the Dzhida Tungsten–Molybdenum Factory. In determining the total concentration of mobile species of Cu, Zn, Pb, Cd, Mn, and Mo, they were extracted with an acetate–ammonium buffer solution (pH 4.8) in the batch mode. Fractionation of the most mobile and environmentally relevant element species, that is, exchange and acid-soluble, was carried out in a dynamic extraction mode in a rotating coil column using calcium nitrate and acetic acid. Element concentrations in the initial samples and extracts were determined by inductively coupled plasma atomic emission spectrometry and mass spectrometry. It is shown that the concentrations of mobile species of Cd, Mn, and Mo, isolated with an acetate–ammonium buffer solution, correspond to the sum of these elements in the exchange and acid-soluble fractions, while the concentration of lead in the acetate–ammonium extract is 2–4 times higher. The convergence of the results of dynamic and batch extraction of copper and zinc depends on the type of sample: for sand, the results are in satisfactory agreement, while for soil, the concentration of copper and zinc in the acetate–ammonium extract is 2–4 times lower than their concentration in the exchange and acid-soluble forms. Nevertheless, the data obtained confirm that the conventional method of batch extraction with an acetate–ammonium buffer solution (pH 4.8) can be considered acceptable for the rapid assessment of the physicochemical mobility and potential bioavailability of elements in soil and technogenic sand. For a more detailed study of highly contaminated samples and the assessment of their danger to the environment, it is advisable to separate exchange and acid-soluble fractions.

A combined method of sample preparation for the determination of the total element composition of oils

A comprehensive approach to the determination of the elemental composition of oils (including those with a viscosity of 5000 mm2/s) is proposed. It ensures the determination of the most elements present in oils using two versions of sample preparation, autoclave decomposition of oil samples and extraction preconcentration of elements from oil into an aqueous solution on rotating coiled columns (RCCs). The application of RCCs in the elemental analysis of oil ensures the preconcentration of a number of trace elements from oil (including rare-earth elements) and the determination of their concentrations at a level of ng/kg. The preconcentration factor of trace elements from oil using an RCC depends on the volume of oil sample pumped through a constant volume of the stationary phase (acid solution) retained in the column and on the speciation of elements in the oil.

Assessment of elemental composition and properties of copper smelter-affected dust and its nano- and micron size fractions.

A comprehensive approach has been developed to the assessment of composition and properties of atmospherically deposited dust in the area affected by a copper smelter. The approach is based on the analysis of initial dust samples, dynamic leaching of water soluble fractions in a rotating coiled column (RCC) followed by the determination of recovered elements and characterization of size, morphology and elemental composition of nano-, submicron, and micron particles of dust separated using field-flow fractionation in a RCC. Three separated size fractions of dust (<0.2, 0.2-2, and >2μm) were characterized by static light scattering and scanning electron microscopy, whereupon the fractions were analyzed by ICP-AES and ICP-MS (after digestion). It has been evaluated that toxic elements, which are characteristics for copper smelter emissions (As, Cu, Zn), are accumulated in fraction >2μm. At the same time, up to 2.4, 3.1, 8.2, 6.7g/kg of As, Cu, Zn, Pb, correspondently, were found in nanoparticles (<0.2μm). It has been also shown that some trace elements (Sn, Sb, Ag, Bi, and Tl) are accumulated in fraction <0.2, and their content in this fraction may be one order of magnitude higher than that in the fraction >2μm, or the bulk sample. It may be assumed that Sn, Sb, Ag, Bi, Tl compounds are adsorbed onto the finest dust particles as compared to As, Cu, Zn compounds, which are directly emitted from the copper smelter as microparticles.

Field-flow fractionation of microparticles in a rotating coiled column for the preparative separation of sorption materials

It is demonstrated that field-flow fractionation using a rotating coiled column (RCC) can be used for the separation and purification of the polydisperse sorbents based on polystyrene–divinylbenzene. The behavior of the sorbent at different operating parameters of RCC was studied. The mobile phase composition, column rotation speed, and the initial flow rate of the mobile phase were selected, optimized for the isolation of a monodisperse fraction with the particle size 4.5 µm and the separation of particles 0.5–2 µm in size, particle fragments, and residues of sorbent synthesis. It is shown that a 15-mL analytical RCC ensures the efficient fractionation of 100 mg of the sorbent in one experiment taking less than one hour with the yield of the desired fraction greater than 95%. The perspectives for scaling up the fractionation in RCC are evaluated; the possibility of using the method for the preparative separation of particles of different nature is discussed.

Field-flow fractionation of nano- and microparticles in rotating coiled columns

Field-flow fractionation (FFF) is a very powerful and versatile set of liquid chromatography-like elution methods. However, conventional FFF separations occur in thin channels and the sample weight injected is usually less than 1mg to avoid overloading. The fractionation in a rotating coiled column (RCC), which can be attributed to sedimentation FFF, enables the handling sample weight to be increased at least up to 1g. An uneven distribution of particles in RCC was first observed by Y. Ito et al. in 1966. The work in this direction was continued by P.S. Fedotov et al. in 2000. Regularities of the behaviour of nano- and microparticles of different size and origin in RCCs with different design parameters were systematically studied taking as example silica particles, latex beads, quartz sand, clay minerals, and other samples. The basic principles of the new FFF method were established. The developed method was applied to the speciation analysis of polydisperse environmental samples, in particular, for the separation of soils into silt, clay and sand fractions. For the first time, nano- and submicron particles of street dust have been separated, weighted, characterized by electronic microscopy, and quantitatively analyzed by ICP-MS (after digestion). The elements that may be of anthropogenic origin (Zn, Cr, Ni, Cu, Cd, Sn, Pb) were found to concentrate mainly in <0.3 and 0.3–1μm fractions. It has been shown that the concentrations of Cr, Ni, Zn in the finest fraction (<0.3μm) of street dust can be one order of magnitude higher than the concentrations of elements in bulk sample. The fractionation in RCC was also used for the recovery of a nearly monodisperse fraction (4.5μm) of a chromatographic sorbent based on polystyrene-divinylbenzene; impurities remaining from the synthesis and smaller particles (1–2μm) being removed. Study on the fractionation of synthetic samples has demonstrated the applicability of the method to the preparative separation and purification of polydisperse materials.

Possibilities for the harmonization of methods of the dynamic fractionation of elements in soils and bottom sediments

The paper presents the first comparative study of the fractionation of heavy metals, arsenic, antimony, and selenium in soils, sludge and bottom sediments using two systems for dynamic extraction, rotating coiled columns (RCC) and cylindrical microcolumns (MC). It has been revealed that the results of the fractionation of the forms of elements are related with the physicochemical properties of soils, sludge, and bottom sediments and the special features of mixing the sample and eluent in RCC and MC. In particular, it has been demonstrated that, as compared to MC, RCC provides more efficient recovery of the most mobile (ecologically relevant) forms of arsenic, antimony, and selenium from samples rich with organic matter. However, in the majority of cases, despite the different efficiency of the recovery of individual fractions, RCC and MC provide comparable diagrams of the distribution of the extracted forms of elements. The influence of the rate of the eluent flow on the processes of the dynamic extraction of heavy metals, arsenic and antimony in RCC and MC has been estimated. The directions of research for the further harmonization of the methods of dynamic fractionation of forms of elements in soils, sludge, and bottom sediments with different physicochemical mobilities and potential biological availabilities are outlined.

New Possibility for REE Determination in Oil

A novel approach of rare earth elements (REE) determination in crude oil is suggested. Special application of countercurrent chromatography (CCC) is used as a sample pretreatment tool. An oil sample is continuously pumped through the rotating coil column (RCC) as a mobile phase, while an aqueous phase (nitric acid solution) is retained as a stationary phase. Two phases are kept well mixed and agitated, but there is no emulsion at the interface under the chosen conditions. Special features of CCC give an opportunity to vary the volume of oil samples to be analyzed from 10 mL to 1 L or more. Trace metals are preconcentrated into 10 mL of stationary phase (acidic solutions) pumped out of the column so that analysis can be easily determined with inductively coupled plasma mass spectrometry (ICP-MS) without additional sample preparation procedures. Optimal concentration of nitric acid in the stationary phase for preconcentration of REE from oil by CCC has been investigated. The combination of CCC with ICP-MS gives the possibility to develop a rapid, reliable, and accurate method of trace metal including rare earth elements (REE) determination in crude oils and oil products. Such method could be an alternative for unexpanded and expensive neutron-activation analysis (NAA).

Rotating coiled columns in the speciation analysis of natural samples: Dynamic fractionation of element forms in soils, sludges, and bottom sediments

The potentials of dynamic extraction in rotating coiled columns (RCCs) for the speciation analysis of soils, sludges, and bottom sediments is discussed on an example of the fractionation of element forms. A comparative study of the results of the fractionation of the forms of heavy metals differing in physicochemical mobility and bioavailability (Zn, Cd, Pb, Cu, Ni, Cr), obtained using a number of procedures of sequential extraction, is performed. Particular attention is paid to mercury, which is quite different from other metals in biogeochemical properties. Conditions are described for the dynamic fractionation of arsenic species occurring in natural samples in anionic forms. It is revealed that, in contrast to batch extraction, the continuous renewal of the eluent in a rotating column eliminates the problem of readsorption and overlapping of isolated fractions and enables the correct assessment of the concentration of the most mobile and bioavailable forms of toxic elements. A hyphenated method for the fractionation and determination of certain forms of elements (based on the ICP-AES detection of elements in the column eluate in the on-line mode) is described, ensuring the processing and a real-time control of the dynamic extraction of the forms of elements. The kinetic aspects of selective leaching are considered. It is shown that a comparison of the elution curves of micro- and macrocomponents makes possible a judgment about the selectivity of the leaching reagent, optimization of the conditions for the isolation of each fraction, and the investigation of the features of the binding of heavy metals and matrix elements in soils and bottom sediments. Some recommendations are given for the dynamic fractionation of the forms of elements in soils, sludges, and bottom sediments in RCCs.

Fractionation of Sb and As in soil and sludge samples using different continuous-flow extraction techniques

The fractionation of Sb and As in soil and sludge samples had been comparably studied using two continuous-flow systems: a microcolumn (MC) and a rotating coiled column (RCC). The leachants were applied in correspondence with a five-step sequential extraction scheme addressing water-soluble, non-specifically sorbed, specifically sorbed, and bound to amorphous and crystalline Fe/Al oxide fractions of Sb and As. Inductively coupled plasma atomic emission spectroscopy was applied to determine antimony, arsenic, and major elements in the effluent and in the residual fractions after their digestion. Resemblances and discrepancies of the two methods were evaluated by the fractionation of Sb and As in forest soil, river sludge, and dumped waste (soil) samples. For the forest soil sample, which is very poor in organic matter, RCC and MC extractions yielded similar quantitative values of As and Sb contents in individual leachable fractions. However, for the river sludge sample with a moderate concentration of C (org) (3.3 %), the results obtained by both continuous-flow methods are in satisfactory agreement. RCC extraction enabled water-soluble and non-specifically sorbed As fractions to be recovered, whereas after MC leaching, these environmentally relevant forms of As were not detected. For the soil rich in organic matter (C(org) = 11.5 %), the discrepancy between the data of RCC and MC fractionations is significant. RCC extraction provides about six times higher recoveries of As and Sb bound to amorphous Fe/Al oxides. More efficient leaching of As and Sb in RCC may be attributed to the migration of organic-rich particles with low density inside the column that might enhance the mixing of the solid and liquid phases.

Behaviour of metalloids and metals from highly polluted soil samples when mobilized by water – Evaluation of static versus dynamic leaching

The mobilization behaviour of metalloids and metals when leached by water from highly polluted soil/sediment samples was studied using static and dynamic approaches employing batch methodology and rotating coiled columns (RCC), respectively. Increasing the solution-to-solid ratios during batch leaching resulted in different enhanced mobilization rates, which are element-specific and matrix-specific. When dynamic leaching is employed with continuous replacement of the eluent, a higher portion is mobilized than when using batch elution with an identical solid-to-water ratio.Using RCC the time-resolved leaching of the elements was monitored to demonstrate the leaching patterns. For the majority of elements a significant decrease could be shown in the mobilized portion of the elements with ongoing leaching process. The data were discussed targeted at solid liquid partitioning coefficients of the metal(loid)s. The capabilities in application of Kd values was demonstrated for dynamic leaching which is relevant for environmental processes.

Continuous-flow fractionation of selenium in contaminated sediment and soil samples using rotating coiled column and microcolumn extraction

Dynamic fractionation is considered to be an attractive alternative to conventional batch sequential extraction procedures for partitioning of trace metals and metalloids in environmental solid samples. This paper reports the first results on the continuous-flow dynamic fractionation of selenium using two different extraction systems, a microcolumn (MC) packed with the solid sample and a rotating coiled column (RCC) in which the particulate matter is retained under the action of centrifugal forces. The eluents (leachants) were applied in correspondence with a four-step sequential extraction scheme for selenium addressing “soluble”, “adsorbed”, “organically bound”, and “elemental” Se fractions extractable by distilled water, phosphate buffer, tetramethylammonium hydroxide, and sodium sulphite solutions, respectively. Selenium was determined in the effluent by using an inductively coupled plasma atomic emission spectrometer.Contaminated creek sediment and dumped waste (soil) samples from the abandoned mining area were used to evaluate resemblances and discrepancies of two continuous-flow methods for Se fractionation. In general, similar trends were found for Se distribution between extractable and residual fractions. However, for the dumped waste sample which is rich in organic matter, the extraction in RCC provided more effective recovery of environmentally relevant Se forms (the first three leachable fractions). The most evident deviation was observed for “adsorbed” Se (recoveries by RCC and MC are 43 and 7mgkg−1, respectively). The data obtained were correlated with peculiarities of samples under investigation and operational principles of RCC and MC.

Remobilization of pentavalent antimony and vanadium from a granular iron hydroxide material – A comparative study of different leaching systems

The remobilization of antimony and vanadium from previously loaded commercial granular ferric-hydroxide GEH material (intended for water treatment) was examined by using a sequential extraction procedure and three different leaching systems to evaluate their physicochemical mobility and potential availability under different simulated environmental conditions. A classical batch extraction, an extraction cell (EC) and rotating-coiled columns (RCC) were used as extraction systems.For each system it could be shown that the content of ion-exchangeable antimony and vanadium in previously loaded material is negligible (<1.5%). The oxyanions were sorbed strongly and could be predominantly remobilized through reducing agents, which means through dissolution of the iron (hydr)oxide matrix.The major advantages of dynamic systems in comparison to batchwise fractionation technique are the drastically reduced extraction time and the possibility of generating information to the leaching kinetics. It is shown that the efficiency of the three leaching systems is quite different employing Wenzel's sequential fractionation protocol. Only by working with RCC, the iron (hydr)oxide matrix was completely dissolved within four steps resulting in the total mobilization of antimony and vanadium. EC seems to be less suitable for leaching studies of Sb and V sorbed on iron(hydr)oxide. The remobilizable proportion of the several fractions was lower in comparison to batch and RCC and seems to be a result of an agglomeration of the GEH in the EC device.

Behavior of Oil–Aqueous Solution Systems in Rotating Coil Column

Behavior of oil-aqueous solution systems used for oil analysis in rotating coil column (RCC) has been studied. An RCC can be used as effective tool for pre-concentration and isolation of trace metals from crude oil and oil products into acidic solutions. An oil sample is continuously pumped through column as a mobile phase whereas an aqueous acidic solution is retained in the column as a liquid stationary phase. The main dependences of the stationary phase retention on construction and operating parameters as well as on the physicochemical properties have been investigated. Optimal values of density and viscosity of crude oil and oil products that could be analyzed with an RCC were estimated. Theoretical dependences of the stationary phase retention on density and viscosity differences between stationary and mobile phases were obtained. These studies allow predicting the retention of the different oil/oil product-aqueous solution systems in an RCC.

Sample preparation in the determination of metals in oil and petroleum products by ICP MS

Comparative elemental analysis of the Tengiz oil and diesel fuel is performed by inductively coupled plasma mass-spectrometry with autoclave digestion, digestion, dilution with organic solvents, and also rotating coiled columns (RCCs). The advantages and drawbacks of each of the listed sample preparation techniques for the separation of microelements are discussed. In contrast to the other versions, the use of RCCs is shown to provide a unique opportunity to preconcentrating microelements from oil and petroleum products into tiny volumes of aqueous solutions (10 mL of 0.5 M HNO3). The eluate prepared can be used in the subsequent analysis by ICP MS with no extra sample preparation steps. The RCC preconcentration of elements from oil and petroleum products makes it possible to determine metals in concentrations from μg/kg to ng/kg.

Novel Approach to the Elemental Analysis of Crude and Diesel Oil

A novel approach to the elemental analysis of crude and diesel oil permitted preconcentration of trace elements is presented. An oil sample is continuously pumped through the rotating coil column as a mobile phase while an aqueous nitric acid solution is retained as a stationary phase. Two phases are kept well mixed and agitated but there is no emulsion on the interface at chosen conditions. Preliminary investigation of features of stationary phase retention of two-phase liquid systems (oil/oil products-aqueous solution) in rotating coil column has been shown. Special features of CCC give an opportunity to vary the volume of oil samples to be analyzed from 10 mL to 1 L or more. Trace metals are preconcentrated into 10 mL of stationary aqueous acidic phase which pumped out of the column for analysis can be easily determined with inductively coupled plasma mass spectrometry (ICP-MS) without additional sample preparation. Optimal concentration in the stationary phase of nitric acid for preconcentration of elements from oil by CCC has been investigated. Combination of CCC with ICP-MS gives the possibility to develop a rapid, reliable and accurate method of trace metal including rare earth elements (REE) determination in crude oils and oil products. Combination of preconcentration method by CCC and highly sensitive determination method (ICP-MS) for quantitative detection of the trace elements (without any additional sample preparation) has been suggested for the first time.