ICP-AES Method Research Articles

Geochemical features and formation conditions of Early-Devonian cherty-argillaceous shales and the underlying basalts in the Ishkildino section (eastern slope of the Southern Urals)

Research subject.The West Magnitogorsk zone of the Southern Urals in the vicinity of the Ishkildino village features a subaerially exposed basaltic sequence superposed by cherts and siliceous-clay shales. The basalts and the overlying shales are assumed to have formed during the Ordovician and Silurian (?)–Early Devonian (up to the conodont zone excavates inclusive) periods, respectively. The aim of this research was to reconstruct, using geochemical data, the conditions under which the rocks present in this geological location were formed.Materials and methods. Five samples of the basalts (XRD and ICP-MS methods), 27 samples of the siliceous-clay shales and 10 samples of the cherts (XRD and ICP-AES methods) were analyzed.Results.According to the ratio of SiO2, Na2O and K2O, the volcanic rocks from the lower part of the section are represented by basalts and trachybasalts. Their geochemical composition corresponds to the N-MORB and is established to be similar to that of the basalts in the Polyakovskaya formation (the Middle–Upper Ordovician). In terms of main elements, the shales under study consist of quartz and illite with a slight admixture of organic matter, goethite, quartzfeldspar fragments, etc. The degree of the sedimentary material weathering according to the CIA, CIW and ICV index values is shown to be moderate. The values of Strakhov’s and Boström’s moduli correspond to sediments without the admixture of underwater hydrothermal vent products. The values of Cr/Al, V/Al and Zr/Al correspond to those characteristic of deposits in deep-water zones remote from the coasts of passive and active continental margins, basalt islands and areas adjacent to mid-ocean ridges. For most samples, the values of Ni/Co, V/Cr, Mo/Mn are typical of deposits formed under oxidative conditions. However, several samples from the upper part of the section, which is comparable to the kitabicus and excavatus conodont zones, demonstrate the Ni/Co, V/Cr, and Mo/Mn values corresponding to deposits formed under reducing atmospheres. An assumption is made that the existence of these deposits can be associated with the Bazal Zlichov event.Conclusion.The investigated pre-Emsian shales have shown no signs of volcanic activity in the adjacent areas. The studied deposits are established to correspond to the central part of the Ural Paleoocean.

Application of Statistical Methods for Classification of Varietal and Regional Origin of White Wines

White wines of four wine-growing regions of Krasnodar region were studied by the ICP-AES method. Nineteen elements were identified in 153 samples of white wines of the Chardonnay, Riesling, and Muscat brands. Methods of statistical analysis demonstrated that, despite the complicated technological cycle of wine production (soil–grapes–juice–wine), information about the grape variety and the region of its origin is preserved in the totality of trace elements. Probabilistic statistical models were constructed to identify the grape variety and the region where it was grown by the concentrations of a certain set of microelements contained in wine. The proposed models are based on the assumption that the soil origin is an important factor determining the microelement composition in wine.

ANALYSIS OF CORROSION-RESISTANT TITANIUM ALLOYS DOPED WITH RUTHENIUM BY ICP-AES

We present a technique of multi-element analysis of new corrosion-resistant titanium alloys doped with ruthenium using Optima 7300 DV ICP-AES spectrometer (Perkin Elmer Corporation, USA) and microwave system Speedwave FOUR (Berghof Products, Germany). Compositions of the acid mixture as well as the temperature and time parameters of the sample preparation of titanium alloys under microwave heating in an autoclave which ensure a complete quantitative transfer of the sample into a convenient analytical form for subsequent ICP-AES analysis without loss of volatile components are substantiated. Optimal conditions of excitation of the analytical signal of analytes for ICP-spectrometer are specified and analytical lines of the elements free of spectral interference are chosen for determination of all critical components in corrosion-resistant titanium alloys. The studies were carried out using samples of experimental melting of industrial titanium alloys of different classes, which, due to volumetric doping with ruthenium, are under development and are not yet commercially available in Russia (grades of alloys PT-7M+Ru, PT-3B+Ru, 5B+Ru, 37+Ru, BT-22+Ru). The samples contained the following alloying elements (% wt.): Al (1.8 – 6.3); V (1.0 – 5.5); Mo (0.7 – 5.5); Zr (0.2 – 3.0); Cr (0.5 – 1.5); Fe (0.5 – 1.5); Ru (0.05 – 0.15). The correctness of the alloying element determination is confirmed by analysis of standard samples using the method of sample variation and spike test for ruthenium determination. The developed technique significantly shortens the duration of the analysis due to combination of the multi-element method of ICP-AES with microwave sample preparation, expands the list of detectable elements in titanium alloys, and increases the accuracy of Al, Si, V, Cr, Fe, Ni, Cu, Zr, Nb, Mo and Ru determination in titanium alloys in critical(rated) ranges of concentrations.

Trace elements in the soils of the Tikves region

The paper presents the results obtained during the investigations carried out for the availability of trace elements (Ni, Cd, Cr, Β) to the soils of the Tikves region. Examination by ICP-AES method were carried out on fifty samples taken in the vicinity of the villages of Begniste, Resava, Vozarci, Drenovo, Sirkovo, Manastirec, Sivec, Rosoman, Sopot, Vatasa, Kavadarci, the Beli Kamenja site as well as a number of samples collected between the places. The results obtained indicate high selenium quantities in the vicinity of Rosoman. Increased nickel concentrations, cadmium and boron along the Crna River course were also determined.

Using reference materials of blast furnace slag, steelmaking slag, converter slag and fused fluxes when developing a procedure for analysis of slag-forming mixtures using inductively coupled plasma atomic emission spectrometry

Introduction . Slag-forming mixtures play an important role in obtaining metal without non-metallic inclusions. Required properties of slag-forming mixtures (SFMs) directly depend on their chemical composition, that is why control of individual component content in a mixture is an important stage in the technological chain of metallurgical production. At the present time, it is a common practice to use inductively coupled plasma atomic emission spectrometry (ICP-AES for analyzing SFMs, requiring sample preparation by alloying with alkali fluxes, which makes it impossible to determine potassium and sodium oxides in a sample. That is why it is necessary to work out a procedure for simultaneous determination of calcium, silicon, magnesium, aluminium, potassium, and sodium oxides by the method of ICP-AES, which would include quantitative transferring of all components into a solution. For that purpose, it is suggested to use microwave digestion of samples in autoclaves. The purpose was to develop a procedure for simultaneous determination of specified components of SFMs using ICP-AES after transferring the sample into a solution in an autoclave under conditions of microwave heating, and to certify it reference materials of slag and fluxes. Materials and methods . Compositional analysis of slag-forming mixtures was conducted using an atomic emission spectrometer with inductively coupled plasma «iCAP 6500 Duo»; sample digestion was conducted with the use of the microwave system «ETHOS PLUS». The following brands of SFMs were chosen as research objects: Melubir 9563 and Accutherm ST-SP/235AL4D; AlsifluxGS-C7; SRCP015, SRCP173P. For calibrating the spectrometer and controlling correctness of determining the specified components, the following reference materials were used: reference materials of blast furnace slag, steelmaking slag, converter slag, and fused fluxes, which have close chemical composition. Research results . An ICP-AES analysis procedure has been developed for calibrating the spectrometer and controlling correctness of determining CaO, SiO2 , MgO, Al2 O3 , K2 O, Na2 O in reference materials of blast furnace slag, steelmaking slag, converter slag and fused fluxes, which allows to establish target components of SFMs quickly and reliably.

Growth and characterization of ammonium nickel-cobalt sulfate Tutton’s salt for UV light applications

We have obtained a set of sample crystals of the family of Tutton’s salt comprise in the isomorphic series with general chemical formula (NH4)2NixCo(1−x) (SO4)2·6H2O, by employing growth from solutions by slow evaporation technique. The samples crystals were characterized by ICP-AES, X-ray powder diffraction analysis, thermogravimetric analysis, UV–Vis-NIR, Raman and FTIR spectroscopy. This type of material has been studied because of its physical and chemical properties not yet understood and they have potential technological applications. Chemical analysis of the samples by ICP-AES method allowed us to investigate the efficiency of the method of growth used. Thermogravimetric analysis provides the information about the thermal stability of the obtained crystals for high temperature applications, and powder X-ray diffraction analysis at ambient and high temperature reveals the structural quality and structural change of the samples respectively. We have used Raman spectroscopy in the range 100–4000 cm−1 and FTIR spectroscopy in the range 400–4000 cm−1 to understand the internal vibrational mode of the octahedral complexes [Ni(H2O)6]2+ and [Co(H2O)6]2+, SO42− and NH4+ tetrahedra. The transmittance of our mixed ammonium nickel cobalt sulfate hexahydrate (ACNSH) crystals is 75% in the UV region, which indicates that they are ideal to use in UV light filters and UV sensors.

Synthesis and catalytic activity of SBA-15 supported catalysts for styrene oxidation

Abstract Cu (II) and Mn (II) metals embedded on mesoporous SBA-15 were synthesized by co-precipitation technique. The support and catalysts were characterized by SEM–EDX, TEM, BET, XRD and ICP-AES methods. The catalytic activity of these catalysts was evaluated for styrene oxidation at various reaction conditions such as styrene to TBHP mole ratio, temperature, catalyst amount by using TBHP as an oxidizing agent. Major reaction products were styrene oxide and benzaldehyde and highest styrene conversion (97.3%) was observed at styrene to TBHP mole ratio of 1:4, temperature at 80 °C and 20 mg of catalyst. Further, the recyclability of the catalysts was observed and found that they can be recycled three times without major loss in their activity and selectivity.

Content and health risk assessment of selected elements in commercially available fish and fish products

ABSTRACTSelected elements (Na, K, P, Mg, Fe, Zn, Cr, Ni, Cu, Mn, Pb, Hg) in fish and fish products bought in supermarkets in Krakow were investigated. Contents of elements were analyzed using AMA 254 apparatus for Hg, and ICP-AES method on JY238 ULTRACE apparatus after samples digestion (HNO3+HClO4 3:1) for other elements. Elements’ concentrations in six fish species and fish products were within the range of (mg/kg w.m.): 2151–6239 for Na; 855–2500 for K; 49.3–183 for P; 353–531 for Mg; 32.6–61.3 for Fe; 4.01–17.6 for Zn; 7.04–12.9 for Cr; 4.25–7.98 for Ni; 1.30–2.27 for Cu; 0.99–1.51 for Mn; 0.09–0.21 for Pb; and 0.01–0.13 for Hg. Human health risk assessment revealed that total non-carcinogenic risk was low to medium with general decreasing order: tuna > salmon > herring> pollock > crab sticks > iridescent shark-catfish. The carcinogenic risk was acceptable for adults and unacceptable for children. Carcinogenic risk values for all subpopulations for Pb were decreasingly ordered as follows: tuna > salmon > herring > pollock > iridescent shark-catfish > crab sticks; and for Cr(VI): tuna > salmon > herring > pollock > crab sticks > iridescent shark-catfish.

Adsorption property of Br-PADAP-impregnated multiwall carbon nanotubes towards uranium and its performance in the selective separation and determination of uranium in different environmental samples

A newer efficient U(VI) ion adsorbent was synthesized by impregnating Br-PADAP [2-(5-Bromo-2-pyridylazo)-5-(diethylamino)phenol] onto multiwall carbon nanotubes (MWCNTs). The effects of various operation conditions on uranium adsorption (i.e., pH contact time, temperature, and initial uranium concentration) were systematically evaluated using batch experiments. The results indicated that the uranium adsorption on modified MWNCTs (5.571 × 10−3g/mg × min) reached faster equilibrium than that on pristine MWNCTs (4.832 × 10−3g/mg × min), reflecting the involvement of appropriate functional groups of Br-PADAP on the chelating ion-exchange mechanism of U(VI) adsorption. Modified MWNCTs (83.4mg/g) exhibited significantly higher maximum Langmuir adsorption capacity than pristine MWNCTs (15.1mg/g). Approximately 99% of uranium adsorbed onto modified MWNCTs can be desorbed by 2.5mL of 1M HNO3 solution. Therefore, Br-PADAP-modified MWNCTs can server as a promising adsorbent for efficient uranium adsorption applications in water treatment. Subsequently, the proposed solid-phase extraction (using a mini-column packed with Br-PADAP/MWCNT) was successfully utilized for analysing trace uranium levels by the ICP-AES method in different environmental samples with a pre-concentration factor of 300-fold. The coexistence of other ions demonstrated an insignificant interference on the separative pre-concentration of uranium. the detection limit was recognized as 0.14μg/L, and the relative standard deviation was approximately 3.3% (n = 7).

Correlations between iron content in knee joint tissues and chosen indices of peripheral blood morphology

Iron as a cofactor of enzymes takes part in the synthesis of the bone matrix. Severe deficiency of iron reduces the strength and mineral density of bones, whereas its excess may increase oxidative stress. In this context, it is essential to determine the iron content in knee joint tissues. The study objective was to determine the level of iron in the tissues of the knee joint, i.e., in the femoral bone, tibia and meniscus. Material for analysis was obtained during endoprosthetic surgery of the knee joint. Within the knee joint, the tibia, femur and meniscus were analyzed. Samples were collected from 50 patients, including 36 women and 14 men. The determination of iron content was performed with the ICP-AES method, using Varian 710-ES. The lowest iron content was in the tibia (27.04 μg/g), then in the meniscus (38.68 μg/g) and the highest in the femur (41.93 μg/g). Statistically significant differences were noted in the content of iron in knee joint tissues. In patients who underwent endoprosthesoplasty of the knee joint, statistically significant differences were found in the levels of iron in various components of the knee joint. The highest iron content was found in the femoral bone of the knee joint and then in the meniscus, the lowest in the tibia. The differences in iron content in the knee joint between women and men were not statistically significant.

Parameter analisis voltammetri pulsa diferensial elektrode grafit pensil untuk penentuan kadmium

Kadmium (Cd) adalah salah satu logam berat non-esensial, yang relatif kecil, tetapi dapat terus meningkat di lingkungan, keracunan kadmium bersifat bioakumulatif dapat menyebabkan penyakit ginjal, gangguan perut, tulang rapuh, penurunan hemoglobin, dan pigmentasi gigi. Oleh karena itu metode analisis untuk menentukan kandungan kadmium harus dikembangkan. Metode untuk penentuan kandungan logam kadmium yang telah banyak digunakan adalah metode AAS dan metode ICP-AES. Dengan sensitivitas dan selektivitas yang sebanding, metode elektrokimia seperti voltammetri telah banyak digunakan sebagai metode yang menarik untuk menentukan kadar kadmium, instrumentasi pada metode ini lebih sederhana dibandingkan dengan metode AAS dan ICP-AES. Tujuan dari penelitian ini adalah untuk mengembangkan metode voltammetri dalam menentukan kadmium menggunakan pensil grafit sebagai elektroda kerja dan parameter analisis metode ini untuk kuantifikasi kadmium. Hasil penelitian ini menunjukkan bahwa metode voltammetri menggunakan pensil grafit elektroda dapat mendeteksi kadmium (II), dengan batas deteksi 0,8 ppm, batas kuantifikasi 2,8 ppm, rentang linearitas dari 2,8 menjadi 4,8 ppm, dan akurasi 0,21-0,58 %.

Alpha-pinene isomerization over Ti-SBA-15 catalysts obtained by the direct method: The influence of titanium content, temperature, catalyst amount and reaction time

This work presents the studies on the isomerization of alpha-pinene in the presence of Ti-SBA-15 catalysts with different titanium contents: 0.75, 0.90, 1.10, and 3.10 wt%, as established by the EDX method, and 0.60, 0.76, 1.08, and 2.53 wt%, as measured by the ICP-AES method. These catalysts were prepared by the hydrothermal method and were characterized by the followed instrumental techniques: XRD, UV-Vis, FT-IR, SEM, ICP-AES, EDX, TEM, and AFM. Additionally, textural parameters were determined by N2 adsorption/desorption. Preliminary studies showed that the most active catalyst was the material prepared from the crystallization gel with the molar ratio of Si:Ti = 20:1. This catalyst was further used for the detailed studies on α-pinene isomerization according to the following parameters: temperature range of 20–200 °C, 0.5–20 wt% catalyst content, and reaction times from 15 min to 24 h. The optimal conditions for α-pinene isomerization were determined on the basis of its conversion and the selectivity of the produced camphene. This study also showed that the process of α-pinene isomerization is complex because subsequent reactions occurred during the process.

Gold nanoclusters as fluorescent sensors for selective and sensitive hydrogen sulfide detection

As a highly toxic environmental pollutant and also an important gasotransmitter in diverse physiological processes, the selective and sensitive detection of hydrogen sulfide (H2S) is very significant. In this work, acetylcysteine stabilized gold nanoclusters (ACC@AuNCs)-based fluorescent sensors had been successfully constructed for H2S perception. The sensing principle was that H2S-induced fluorescence quenching of AuNCs which attributed to both the formation of Au2S between Au(I) in the AuNCs and H2S and the increased particle size. The proposed sensors showed high selectivity toward H2S over other anions, amino acids and thiols, and exhibited a stable response for H2S from 0.002 to 120μmolL−1 with a detection limit of 1.8nmolL−1. In addition, the practical application of the designed sensors was further evaluated with water and serum samples, and the tested results agreed well with those obtained by ICP-AES method. The satisfactory recoveries and good precision show that the proposed fluorescent sensors has potential application in biological and environmental fields.

Corrosion of Austenitic Steels and Their Components in Molten Nacl–Kcl–UCl3

The fused halides can be used for nuclear fuel reprocessing and as working media for molten salt nuclear reactors. However practical implementation of such technologies is limited by the problem of finding suitable corrosion resistant materials capable of long-term working in contact with molten salts. From the economical point of view the application of stainless steels as construction materials for the molten salt media is one of the most prospective ways. In the present study the corrosion behaviour of metallic iron, nickel, chromium, molybdenum, AISI 316L and 12Kh18N10T (analogue of AISI 321) austenitic steels was studied in NaCl–KCl–UCl3(1 wt.% U) melts at 750 ºC. Gravimetric measurements served as a basis for estimating corrosion resistance of studied materials. Quenched melts were analyzed using ICP-AES method. The surface of the alloy samples after corrosion tests was characterised using XRD, SEM and Х-ray microanalysis. The foils of corroded materials were examined by TEM. The corrosion rates of studied metals in NaCl–KCl–UCl3melt decrease in the following order: Cr>Fe>Ni>Mo, which correlates well with the formal standard potentials of metals in chloride melts indicating electrochemical nature of the corrosion processes. Molybdenum is the only corrosion resistant metal in the uranium-containing chloride melts and it can be used as a construction material for molten salt reactors. The major products of stainless steel corrosion in chloride melts are iron, chromium and manganese species. The surface of the corroded samples of austenitic stainless steels was depleted in manganese and chromium and enriched in nickel and molybdenum. Intergranular corrosion was observed for all types of austenitic steels. In terms of intensity and depth of the corrosion layer in NaCl–KCl–UCl3 the studied steels can be ranged in the order AISI 321>AISI 316L that correlates with the amount of excessive phases formed (figure). Figure 1

Factors that Affect the Content of Cadmium, Nickel, Copper and Zinc in Tissues of the Knee Joint

Osteoarthritis causes the degradation of the articular cartilage and periarticular bones. Trace elements influence the growth, development and condition of the bone tissue. Changes to the mineral composition of the bone tissue can cause degenerative changes and fractures. The aim of the research was to determine the content of cadmium (Cd), nickel (Ni), copper (Cu) and zinc (Zn) in the tibia, the femur and the meniscus in men and women who underwent a knee replacement surgery. Samples were collected from 50 patients, including 36 women and 14 men. The determination of trace elements content were performed by ICP-AES method, using Varian 710-ES. Average concentration in the tissues of the knee joint teeth amounted for cadmium 0.015, nickel 0.60, copper 0.89 and zinc 80.81 mg/kg wet weight. There were statistically significant differences in the content of cadmium, copper and zinc in different parts of the knee joint. There were no statistically significant differences in the content of cadmium, nickel, copper and zinc in women and men in the examined parts of the knee joint. Among the elements tested, copper and nickel showed a high content in the connective tissue (the meniscus) compared to the bone tissue (the tibia and the femur).

Određivanje sadržaja nitrita i teških metala u mesu i proizvodima od mesa

The improvement of living standards has a significant impact on food and food production. Meat and meat products, due to their high nutritional value, are an important segment of human nutrition and a rich source of elements such as Fe, Zn, Mn, Ca, K, Mg. On the other hand, meat can accumulate heavy metals such as Cd and Pb. Toxic metal concentrations in the muscles are rare, but the liver and kidneys have an ability of accumulation. Nitrites are very important in the meat industry as additives and preservatives, but downside effects of nitrite addition are the development of toxic and carcinogenic nitrosoamine. In monitoring the quality of meat and meat products, it is important to keep track of metal content, but also the residual concentration of nitrite. The aim of this study was to determine the content of Cd, Cu, Fe, and Zn in samples of pork and beef meat and pig liver and the content of nitrites in samples of pork and beef meat and meat products - patches and sausages. Metals were determined using the ICP-AES method and nitrate by the standard method SRPS ISO 2918/1999. The content of iron in the liver, pork and beef meat is 189.2 μg / kg, 89.78 μg / kg and 87.79 μg / kg respectively. The content of Cu and Zn in all tested samples is below MAC values, and Cd in pork meat sample is 1.2 times more than MAC values. The content of nitrite is below the MAC values and represents the residual concentration of these compounds.

A set of analytical methods for the estimation of elemental and grain-size composition of volcanic ash

A combined approach to the analysis of volcanic ash (VA) was proposed. Ash particles were separated by size using a combination of vibration sieving on sieves (140, 70, 40 μm) and field-flow fractionation in a rotating coiled column (for separation of nano- and submicron particles). Initial samples and obtained fractions were characterized using scanning electron microscopy and static light scattering. Their elemental composition was determined using ICP-MS and ICP-AES methods. The radionuclide composition of the VA was studied by the low-background gamma spectrometry. The studies were carried out by the example of ashes from Puyehue volcano, the Puyehue Cordon Caulle volcanic group, Andes (Santiago, eruption on June, 2011), which were taken immediately after eruption and after first rain. It was shown that up to 15% of major elements (such as P, Ca, and К) and trace elements (such as Be, Hg, Tl, As, Sb, and Bi) could be extracted from the ash by rain and migrate into environment. It was also found that the content of radionuclides (U235, Th234, Pb214, Bi214, Be7) after rain decreases by 30–40%. Of special interest are ash nanoparticles (up to 200 nm), in which the contents of Cu, Pb, Tl, Bi, Sn, As, and Sb are over an order of magnitude higher than the bulk contents of these elements in the ash. This regularity was found in samples taken both prior to and after rain. The proposed methodology of fractionation, study, and analysis of ash particles may be applied for a wide range of soil, ash, and dust samples of different nature.

The Effect of Liming and Sewage Sludge Application on Heavy Metal Speciation in Soil

The aim of this paper is to assess the effect of liming and low doses of municipal sewage sludge (5%, 10%, 15% of the soil mass) on lead, chromium and nickel speciation in soil. The 420-day experiment was carried out in laboratory conditions. In all the samples lead, chromium and nickel concentration was determined with the ICP-AES method, while the content of those metals in different fractions was measured with the seven-step Zeien and Brümmer method, on the 30th and 420th days of the experiment. Sewage sludge doses significantly diversified lead, chromium and nickel amounts in the soil. The highest dose of sludge caused a significant increase, compared to the control, in the content of those metals. In the sludge the dominant forms of metals tested in the experiment were lead and chromium bound to organic matter (F4) as well as nickel bound to amorphous iron oxides (F5). Liming decreased the mobility of the metals in the soil.

The effects of soil liming and sewage sludge application on dynamics of copper fractions and total copper concentration.

The paper deals with effects of liming and different doses of municipal sewage sludge (5, 10, and 15 % of soil mass) on copper speciation in soil. In all samples, pH was determined together with total copper concentration, which was measured with the ICP-AES method. Concentration of copper chemical fractions was determined using the seven-step procedure of Zeien and Brümmer. In the soil treated with the highest dose of sludge (15 %), there was, compared to the control, a twofold increase in the concentration of copper and a threefold increase in the concentration of nitrogen. Copper speciation analysis showed that in the municipal sewage sludge the easily soluble and exchangeable fractions (F1 and F2) constituted only a small share of copper with the highest amount of this metal in the organic (F4) and residual (F7) fractions. In the soil, at the beginning of the experiment, the highest share was in the organic fraction (F4), the residual fraction (F7) but also in the fraction where copper is bound to amorphous iron oxides (F5). After 420 days, at the end of the experiment, the highest amount of copper was mainly in the organic fraction (F4) and in the fraction with amorphous iron oxides (F5). Due to mineralization of organic matter in the sewage sludge, copper was released into the soil with the share of the residual fraction (F7) decreasing. In this fraction, there was much more copper in limed soil than in non-limed soil.

Optimization of capillary electrophoresis method for the determination of rare earth elements in soils and natural waters

Currently, rare earth elements (REEs) in the environmental objects are determined by neutron activation and ICP-MS methods. Capillary electrophoresis (CE) is not used for these purposes because the poor detection limits (LOD). This weakness can be overcome by multiple concentrating of the samples through the high effective sample stacking process of triply charged ions Ln3+. LOD for REEs were received ranged from 0.2 to 1.2μg/l. The following composition of background electrolyte for CE determination of lanthanides was proposed: 12mM benzimidazole, 8mM dipropylglycolic acid, 10mM glycolic acid, pH=3.0. Using this background electrolyte the completely separation of REEs (Y+La+Ln without Pm) is possible for 12min. The sample preparation procedure for CE determination of lanthanides in soil and natural water was improved and the analysis of these analytes was performed. The validity of experimental results was confirmed by AES and ICP-AES methods.