Journal of Analytical Chemistry, Vol. 57, No. 7, 2002, pp. 651–657. Translated from Zhurnal Analiticheskoi Khimii, Vol. 57, No. 7, 2002, pp. 773–780. Original Russian Text Copyright © 2002 by Blank.
ANALYTICAL LABORATORIES
Analytical Chemistry at the Institute of Single Crystals of the National Academy of Sciences of Ukraine A. B. Blank Institute of Single Crystals, National Academy of Sciences of Ukraine, pr. Lenina 60, Kharkov, 61001 Ukraine Received November 22, 2001
Abstract—The paper describes the history and main lines of inquiry of the Analytical Laboratory at the Institute of Single Crystals (Kharkov, Ukraine) organized in 1955.
The Institute of Single Crystals was organized as the Kharkov branch of the Moscow Institute of Chemical Reagents and High-Purity Substances in 1995. The institute soon became a leading scientific center in the field of production and study of scintillation materials, optical and laser single crystals, functional ceramics, organic luminophores, and high-purity inorganic compounds. The analytical laboratory was among the three scientific divisions organized at the institute in the year it was established. Almost all staff members of the laboratory had just graduated from the Kharkov State University, where they studied the fundamentals of analytical chemistry under the supervision of Professor N.P. Komar. They faced difficult problems in the determination of extra low concentrations (10–6 to 10–5%) of trace impurities in inorganic crystals and raw materials, as well as in the high-precision determination of activating dopants, whose distribution in single crystals depends on the growth conditions and strongly affects the properties of resulting products. The laboratory was directed by A.P. Kilimov (1955– 1959), A.M. Bulgakova (1959–1980), and Ya.A. Obukhovskii (1980–1985); A.B. Blank has been the head of the laboratory since 1986 up to the present day. In 1992, the institute entered the National Academy of Sciences of Ukraine under the name of the Institute of Single Crystals and the laboratory was reorganized to the Department of Analytical Chemistry of Functional and Environmental Materials. In the early years, the equipment of the analytical laboratory included only domestic photocolorimeters and pH-meters. More recently, SF-4, SF-16, SF-26, and SF-46 spectrophotometers were acquired, including instruments with temperature-controlled cells. This equipment was used in the early 1960s to develop extraction–photometric procedures for the sequential determination of copper, nickel, iron, and manganese traces in a single test portion and total heavy metals in the same analytical form, e.g., copper(II) or mercury(II) diethyldithiocarbamate (Blank, Bulgakova,
and N.T. Sizonenko). The sensitivity of the developed extraction–photometric procedures was improved using microcells with a small ratio of volume of the solution to the thickness of the absorbing layer (Blank, 1960s). Some errors typical of photometric analysis, protonation equilibria, complexation, and distribution in the systems to be analyzed were studied; the results obtained were used to optimize the conditions for determining trace impurities in high-purity substances (Blank, 1960s–1970s). Among the new analytical forms proposed for photometric analysis, we should note such complexes extractable with organic solvents as iron(II) complexes with 1-nitroso-2-naphthol (Blank, Bulgakova, and L.E. Belenko, 1960s), complexes of some rare and dispersed elements with morin (Blank, I.I. Mirenskaya, Belenko, and L.P. Eksperiandova, 1970s–1980s), as well as a Rivanol diazotization product for the determination of nitrite and nitrate ions, and water-soluble boron-bearing macrobicyclic iron(II) nioximate for the determination of boron (R.P. Pantaler and T.I. Ivkova, 1990s). Photometry and spectrophotometry of solutions (molecular absorption spectra) have remained working techniques for the determination of some impurities, in particular, inorganic anions and rare elements, all the years the laboratory has existed. Pantaler and coworkers have developed kinetic methods of analysis at the laboratory. In 1960s–1970s, new indicator reactions catalyzed by the trace components under study were proposed and studied. Among them are the oxidation of rubeanic acid with hydrogen peroxide catalyzed by tungsten, molybdenum, tantalum, zirconium, and thorium compounds (Pantaler); the catalytic decomposition of hydrogen peroxide in the presence of some iron(III), manganese, and cobalt complexes (Pantaler, R.A. Geits, and L.D. Alfimova); and the formation of chromium(III) complexes with Xylenol Orange catalyzed by carbonate ions (Pantaler and I.V. Pulyaeva). In contrast to the majority of the similar reactions known previously, the latter indicator reaction is a complexation reaction rather than a redox
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buffer, a week complexing agent, served as the background solution, and the overlapping peaks of lead and thallium were resolved using EDTA. Voltammetry was successfully applied to the simultaneous determination of elements in different oxidation states, e.g., Eu(II) and Eu(III) or Cr(III) and Cr(IV). The polarographic determination of Fe(II) formed in the reaction of tungsten in lower oxidation states present in tungsten(VI) oxide with Fe(III) was used to determine the stoichiometric coefficient of oxygen in this oxide, which is a starting material for the synthesis of scintillation materials such as CdWO4 and PbWO4 .
Photo 1. In the atomic spectrometry group: E.S. Zolotovitskaya (left) and L.V. Glushkova (1975).
one. In 1990s, Pulyaeva and L.I. Mikhailova proposed new reactions of this class for the catalymetric determination of phosphate and carbonate ions. To lower the determination limit in catalymetry, Pantaler and Alfimova proposed to measure temperature changes, instead of measuring color changes of the reaction product with time. Using the determination of sulfite and thiosulfate ions as an example, Pulyaeva and N.L. Egorova have shown that the measurement of the rate of a slow noncatalytic reaction involving trace analytes ensured significantly lower determination limits than the measurement of the yield of the reaction product. Since the early 1960s, voltammetry has been widely applied at the laboratory to determine trace impurities, alloydopants, and even for the substance analysis of some materials. The works in this area were performed under the supervision of G.A. Babich and with the participation of E.P. Kisil, K.F. Kravtsova, L.I. Fillipovich, and L.I. Pashneva. A PLS universal voltammetric unit and a PU-1 polarograph were developed by R.M.-F. Salikhdzhanova and showed good performance under long-term use. A procedure for the highprecision determination of thallium (an alloying element in scintillation single crystals of alkali iodides), which involved sample preparation to remove possible interferences and classical polarography, should first be noted. Different versions of voltammetry and sample preparation techniques allow to determine thallium in single crystals in the concentration range covering six orders of magnitude (from 10–6 to several wt %), as well as in the air of the working area and settlements, technological and washout solutions, surface and potable waters, filtering and packing materials, industrial oils, sludge, desiccants, etc. It was shown that stripping voltammetry could be used for the simultaneous determination of Bi, Cd, Cu, Pb, Tl, Sb, and Zn in functional materials in the range between 10–7 and 10–6%; acetate
In the late 1950s, investigations in the area of atomic emission analysis of materials were launched under the supervision of E.S. Zolotovitskaya (Photo 1). The classical technique of spectrographic analysis was used: spectra were photographed using STE-1 and DFS-8 diffraction spectrographs; an SP-1 spectrum-projector and an MF-4 microphotometer were used for their interpretation and photometric measurements. M.Z. Nesanelis, Z.V. Shtitelman, L.V. Glushkova, A.P. Mirnaya, V.K. Shevchenko, and O.P. Il’chenko were involved in this work. High-temperature processes in the channel of a sample-carrying carbon electrode and in arc plasma were studied, as well as the effect of macrocomponents (alkaline earth metal fluorides; chalcogenides; phosphates; and simple and complex oxides of aluminum, yttrium, magnesium, and other elements), additives of carbon powder, readily dissociating reagents, and the parameters of the arc discharge on the kinetics of evaporation and emission spectra of elements. Based on the results obtained, procedures were elaborated for the simultaneous determination of 20 impurity elements. It was shown that the determination limits of elements cmin without preconcentration are in the range between 10–6 and 10–3 wt % and usually increase in the same order as the thermal heats of dissociation of compounds: chalcogenides < halide < niobates < oxides < carbonates. For spectrochemical techniques, the determination limits are lower by one–two orders of magnitude. In the early 1990s, an arc double-jet plasmatron designed by A.P. Tagil’tsev appeared in the laboratory. Zolotovitskaya and Shtitel’man showed that this spectrum excitation source is efficient for the direct analysis of powdered nonconductive functional materials whose matrices are characterized by few-line emission spectra and low ionization potentials of elements and which are readily ground to a finely dispersed state (LiF, KCl, KH2PO4 , Al2O3 , CaCO3 , SrCO3 , and BaCO3). It was found that the selection of the torch zone where the useful atomic and ionic lines are the most intense is highly important. The determination limits for some elements, especially for nonvolatile (Ti, V, and Mo) and widespread (Ca, Al, and Si) ones, can be lowered by 5 to 30 times (to 10–6 × 10–5%), compared to the arc source. The dispresion of the results was also significantly
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lower (at element concentrations of ~5cmin, RSD was 3– 6% for the plasmatron and 12–15% for the arc source). An advantage of plasmatron over inductively coupled plasma is the possibility of the direct analysis of powdered samples without their solubilization. In 1998, we acquired a Trace Scan Advantage ICP AES spectrometer (Thermo Jarrell Ash, USA). To optimize the operating conditions, N.I. Shevtsov and K.N. Belikov studied the signal-to-noise ratio as a function of the plasma power and the carrier gas pressure. It was found that, for different elements, maximum signal-to-noise ratio correspond to different ratios between the parameters studied. To lower the detection limits without an appreciable increase in the time of analysis, it was proposed to classify elements into groups based on the ratios found. The examination of the standard addition method as applied to ICP AES showed that larger amounts of additives within the linear calibration range should be used to minimize the determination error. The ICP AES technique was used for determining trace impurities, alloying elements, and major components of optical and scintillation single crystals, materials used in chemical current sources, soil extracts, biological samples, noble metal alloys, and electronic wastes containing noble metals. Sample preparation procedure is also important. It includes solubilization of samples and sometimes the preconcentration of the impurities to be determined. To determine the major components, calibration curves were constructed by the external standard method using model mixtures of the elements to be determined. The standard addition method was used to determine trace impurities and alloying components. The optimization of the measurement conditions eliminated the mutual interference of analytes and minimized matrix effects. The procedures developed were free from significant systematic errors and exhibited sufficient precision (RSD ≤ 1% for matrix elements and alloying additions). The limits of direct determination (cmin) differed among analytes and matrices; they are between 5 × 10–6 and 1 × 10–5 wt % for the majority of impurities in inorganic functional materials but were usually higher by one order of magnitude for lead impurities. In distinction to multielemental AES methods with arc or plasma excitation sources, flame AES and AAS are generally used for the determination of single elements. Nonetheless, these methods occupy an important place in the analytical chemistry of functional materials. In the early 1960s, Zolotovitskaya began to use flame emission spectrophotometry, first for the determination of alkali and some alkaline earth metal impurities in various materials, including alkali metal salts. An installation composed of an ISP-51 spectrograph and an FEP-1 photoelectric device was first used. When a Saturn spectrophotometer (which was just produced by the Severodonetsk OKBA, USSR) was acquired in the early 1970s, all investigations in emission and atomic absorption flame photometry were JOURNAL OF ANALYTICAL CHEMISTRY
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performed using this instrument. Electrothermal atomic absorption analysis was first carried out with a PerkinElmer 403 spectrophotometer equipped with an HGA-74 atomizer; a Saturn spectrophotometer with a Grafit-2 atomizer designed by L.A. Pelieva has been used since the early 1990s. B.M. Fidel’man, V.G. Potapova (Chepurnaya), N.V. Bondareva, T.V. Druzenko, and N.N. Grebenyuk participated in the work on flame spectrophotometry and atomic absorption spectrometry. To optimize the analytical conditions, the effect of the nature and concentration of major components and trace impurities on the analytical signals was studied. An example of successful solution is the addition of an appreciable amount of calcium to eliminate the interference of attendant impurities with the results of electrothermal atomic-absorption determination of magnesium. The sensitivity of electrothermal atomic-absorption analysis (ET AAS) is better than that of ICP AES. Grebenyuk has recently proposed approaches to remove the known restrictions of this method. In particular, a new method for the chemical modification of silicon (a hardly determinable element) was proposed. New opportunities for introducing corrections for nonselective light absorption, which is a significant source of systematic errors, were opened up based on the idea of using a priori data on molecular absorption spectra of the gas phase above different substances; these spectra can be recorded on an electrothermal atomic absorption spectrometer in wide ranges of temperatures and wavelengths. A VRA-2 crystal-diffraction XRF spectrometer (Carl Zeiss, Jena) was got in the early 1980s; its improved version VRA-30 and a portable SPARK Xray spectrometer (Burevestnik) were acquired more recently. In the history of the laboratory, less accurate methods of X-ray fluorescence (XRF) analysis were changed to more accurate ones: the analysis was first conducted using powdered samples and aqueous solutions, next using compact samples, and finally using sintered, quasi-solid, and thin-film specimens as well as the nondestructive examination of solid samples. It was found that crystal-diffraction XRF spectrometry is an efficient method for the precise determination of alloying elements and the major components of complex single crystals; its relative error is equal to few hundredths of percent for medium and high concentrations of elements under favorable conditions. Using one of the procedures developed, we have found a slight change in the tungsten-to-cadmium ratio along the growth direction of cadmium tungstate scintillation single crystals, which was due to the partial evaporation of cadmium from the melt (Shevtsov and Mirenskaya). Eksperiandova showed that the relationship between the analytical signal and the crystallographic orientation of the sample should be taken into account in the nondestructive XRF analysis of alloying titanium dopant to corundum single crystals. Belikov used a
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heavy metal (barium) additives and thus minimized the systematic errors due to the interference of concomitants in the XRF determination of available toxicants in soils. In 1980s, XRF analysis found wide application for the analytical control of high-temperature superconductors (Shevtsov, Z.M. Nartova, and S.Yu. Sumarokov). Eksperiandova et al. developed some extraction XRF and crystallization XRF procedures for the determination of toxic elements in waste, natural, and potable waters. Along with the crystal-diffraction XRF instruments, an X-ray energy-dispersion analyzer designed at the Kiev State University and improved at our laboratory (Shevtsov and Belikov) was used for the multielement analysis of aerosols. The use of Bragg reflectors from a curved LiF (200) single crystal and a cylindrical reflector composed of segments of the same single crystal lowered the determination limits of elements in air samples by an order of magnitude. Electron probe microanalysis of solids is a customary method of physicists who disregard the metrological aspects of analysis. In this context, it is of interest to consider the results of Eksperiandova, who studied the accuracy and precision of the local determination of matrix elements and alloying elements in some functional materials with an MAR-3 electron probe microanalyzer in the mid-1990s. In addition, the study of the layer-by-layer distribution of matrix elements in the CdWO4 single crystal sections supplemented the XRA data and showed that the cadmium and tungsten distributions are highly nonuniform at the trace level. We studied high-temperature superconducting materials by chemical phase analysis, which proved to be indispensable for the determination of impurity phases at levels below their detection limits in X-ray diffraction techniques (X-ray phase analysis). The simplest version of this analysis (selective dissolution) was used to isolate free copper(II) oxide from a superconducting yttrium–barium cuprate ceramics and to detect and determine bound (ionic) silver in a YBaCuO/Ag composite. The total phase composition of this superconducting ceramics was studied, and it was shown that the main and all impurity phases (except for CuO) can be determined from the curves of sample dissolution in diluted acetic acid, when each portion of the solution contains elements from several phases. Sumarokov was involved in the phase analysis of high-temperature superconducting materials. Sample preparation, which is an essential step of every method of the analysis of materials and environmental samples, has been an important area of investigation at the laboratory over the whole period of its activity. Much attention was given to the preconcentration of trace impurities. In order to prevent the loss of impurities to be determined and their introduction into the sample from the reagents, apparatus materials, and environment, we
used a SEM MDS-9000 microwave oven or analytical autoclaves developed by V.A. Orlova and Yu.A. Karpov. At the same time, methods based on interactions between poorly soluble compounds and complexing agents (under heating on electric hot plates with ceramic bases and heaters covered with an aluminum sheet) were developed. Condensed phosphoric acid proved to be an efficient reagent for the decomposition of many simple and complex refractory oxides in the form of single crystals and powder blends for their growth (Zolotovitskaya and Druzenko, 1996). A solution of boric and nitric acids, which forms soluble fluoroborate complexes, has found wide application for the dissolution of fluorinecontaining functional materials (MgF2 , CaF2 , LiBaF3 , etc.). In the early 1990s, Shevtsov et al. proposed to use lithium metaphosphate as a flux and a glassy carbon crucible as a mold for the high-performance XRF analysis of oxides. In this case, emitters are manufactured as homogeneous glassy moldings that do not require long annealing and subsequent mechanical processing. Recently, Eksperiandova, Ya.N. Makarovskaya, and I.I. Fokina developed original methods for the preparation of liquid samples, including process and waste waters and analytical concentrates on their basis, to XRF analysis. It was shown that when gelling agents (e.g., gelatin or agar-agar) were added to the aqueous solutions under study, homogeneous quasi-solid emitters of the specified size and shape with perfectly smooth surface were obtained. To manufacture quasisolid emitters from organic extracts (impurity concentrates to be determined), it was proposed to obtain organic gels by treating extracts with small volumes of aqueous gelatin and surfactant solutions. Another method proposed by Eksperiandova et al. for preparing organic extracts to XRF analysis consisted in the fabrication of thin-film emitters from the carbosil-70 polymer used in medicine. When a small volume of an aqueous solution (e.g., a concentrate obtained by the directional crystallization of the test water) was analyzed, the preparation of a saccharose-based glassy organic polymeric emitter from this solution was efficient. An appreciable decrease in cmin in the XRF determination of impurities in the wastewater from the production of functional materials was attained recently by combining this method with the extraction preconcentration of analytes and the preparation of quasi-solid or thin-film emitters from the concentrates obtained (Eksperiandova and Makarovskaya). The ultrasonic treatment of samples on a UZDN-A disperser was used by the same authors to decompose humic substances masking heavy metal ions in natural waters. Various methods of analyte preconcentration are used at the laboratory to lower the determination limits of impurities in functional materials and, in some cases,
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to improve the representativeness of test samples or the precision of the results of analyses. Between the 1960s and 1970s, extraction preconcentration was predominant. Along with extraction– photometric procedures, multielement spectrochemical procedures using of sodium diethyldithiocarbamate as an extraction group reagent were developed (Zolotovitskaya, Sizonenko, Mirnaya, Belenko, and E.I. Yakovenko). In these procedures, different groups of elements were extracted at specified pH values. Under the supervision of Yu.A. Zolotov, Sizonenko studied a new extraction group reagent, 1-phenyl-3-methyl-4-benzoylpyrazolone-5. For a long time, spectrochemical methods have formed the basis for the analytical control over the purity of functional materials. However, in the 1980s–1990s they became less significant because of the appearance of such highly sensitive methods as multicomponent stripping voltammetry, ICP AES, and ET AAS (Photo 2). Distillation preconcentration is used at the laboratory for the determination of some aerogenic impurities. In 1980s–1990s, Pulyaeva et al. developed combined distillation–coulometric procedures for the determination of total and bound carbon and carbonate ions in various functional materials and sulfate ions in aluminum oxide. These methods were intended for single crystals. To determine halogenide ions in single crystals and raw materials, A.K. Khukhryanskii used an improved version of pyrohydrolysis (reaction between superheated water vapor and a powdered test sample with the formation of gaseous halogen hydrides absorbed by water or an alkali solution). Along with conventional preconcentration methods (extraction, sorption, distillation, precipitation, and coprecipitation), Blank and coworkers (L.I. Afanasiadi, Shevtsov, Potapova, Eksperiandova, and N.I. Komishan) have developed a new preconcentration procedure based on the redistribution of an impurity in the directional crystallization of a substance analyzed. This method (crystallization preconcentration) expands the possibilities of analytical preconcentration techniques, because it efficiently preconcentrates various impurities, including alkali metal cations, chemical matrix analogues, and anionic and organic impurities. The method does not require reagents and, hence, possesses a low total background; it can be readily automated and saves expensive test materials, which are returned to the process after sampling the concentrate. Different versions of crystallization preconcentration were studied, and the results obtained were used for solving some important analytical problems. In particular, the lowtemperature crystallization preconcentration of different impurities, including thermally unstable, reactive, anionic, organic, and isomorphic ones, was efficiently combined with various instrumental methods of analysis (AES, AAS, spectrophotometry in microcells with small cross-section areas, potentiometry with an ionselective electrode, pH-potentiometry, and kinetic analJOURNAL OF ANALYTICAL CHEMISTRY
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Photo 2. K.N. Belikov works with an inductively coupled plasma atomic emission spectrometer (2001).
ysis). This allowed cmin for impurities to be lowered by two orders of magnitude in most cases. In recent years, Eksperiandova and Blank have also studied the regularities and potentialities of the low-temperature crystallization preconcentration of impurities in the wastewater from functional material-producing plants. A combined sorption–scintillation method for determining small concentrations of radionuclides in water has recently been proposed by Shevtsov and A.Yu. Andryushchenko: radioactive impurities were adsorbed on a solid composite served simultaneously as scintillator. A new area was developed at the laboratory in the last decade: the elaboration of simple and rapid testmethods for the detection and semiquantitative determination of harmful impurities in water, vegetables, fruits, and process solutions, as well as for the detection of illegal narcotics and psychotropics. Ivkova, L.V. Gudzenko, and O.V. Gaiduk were involved in these investigations under the supervision of Pantaler (Photo 3). The analytical signal is usually the coloration, color change, color intensity, or, more rarely, induction period, i.e., the time interval between the test and the appearance of coloration. Along with the reactions described in the literature, new indicator reactions and methods for enhancing the analytical signal were proposed. They lowered the detection limits and improved the test selectivity. In some cases, the new indicator reactions allowed us to exclude the use of expensive or toxic reagents. The detection limits were estimated by the Komar method based on the statistical evaluation of the parameters of the unreliable reaction zone, where some samples gave positive reactions and other samples gave negative reactions. This method exemplifies a metrological approach to the results of measurements and analytical procedures typical of the Komar school. This approach was practiced at the laboratory. To improve the reliability of the analytical control of functional materials, known meth-
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Photo 3. The test-method development team, seated: T.I. Ivkova (left) and O.V. Gaiduk, standing left to right: R.P. Pantaler, L.V. Gudzenko, and A.B. Blank (2000).
ods of statistical data processing are widely used at the laboratory and new idea were advanced. These ideas were considered, e.g., in the works of Blank on the evaluation of the detection and determination limits (1962, 1979) and metrological aspects of the analytical control of functional materials (1997), as well as in the papers “About the Estimation of Errors of Indirectly Measured Quantities” (1971) and “The Assurance of Chemical Composition Measurements and the Iodine Unit” (2000) by Blank and A.A. Bugaevskii, Professor of the Department of Chemical Metrology at the Kharkov State University. An original research area was the use of analytical methods and results for solving problems in materials science. It was shown (Blank, 1996) that the discussion of analytical results in some cases can reveal new physical laws and that analytical methods represent models of processes that are accomplished during the synthesis of new materials. Thus, the results of the phase analysis of the yttrium–barium cuprate/silver superconducting composite elucidated the problem of the state of silver in this composite; the detection of sodium in the unalloyed single crystals of cesium iodide resulted in the development of a new efficient scintillator, and the decomposition of refractory oxides with condensed phosphoric acid served as a model for a new method of chemical etching of sapphire single crystals in studying their corrosion resistance. Until the early 1990s, the most significant results obtained by the laboratory personnel were published predominantly in the Zhurnal Analiticheskoi Khimii or,
more rarely, in Zavodskaya Laboratoriya. Several thematic collections of articles have also been published, e.g., “Methods of Analysis of High-Purity Substances and Single Crystals” (1962, 1966, 1969) and “Methods of Analysis of Alkali and Alkaline-Earth Halogenides” (1971, vols. 1, 2). Blank was a coauthor of the collective monograph Controlled Crystallization in a Tubular Container under the general editorship of A.N. Kirgintsev and V.A. Isaenko (Novosibirsk: Nauka, 1978) and the author of the monograph “Analysis of Pure Substances Using Crystallization Preconcentration” (Moscow: Khimiya, 1986). In recent years, the results of our studies were published not only in Zhurnal Analiticheskoi Khimii, but also in Analytica Chimica Acta, Talanta, Fresenius’ Journal of Analytical Chemistry, X-Ray Spectrometry, Advances in X-Ray Analysis, Journal of Trace Microprobe Techniques, Analytical Letters, Physica C, Nuclear Instruments and Methods in Physics Research, and Polymer and Colloid. We believe that it is important to cover the developed analytical methods and techniques by inventor’s certificates and patents. Totally, more than 30 patents and inventor’s certificates of the USSR, Ukraine, and Russia have been received over the period the laboratory exists. The role of Komar in the organization and development of our laboratory has already been mentioned. Eminent analysts A.K. Babko, Zolotov, V.A. Nazarenko, D.P. Shcherbov, and K.B. Yatsimirskii visited our laboratory and actively helped us in our work. Laboratory staff members have actively participated in international and regional scientific conferences and workshops. Note the recent All-Ukraine conferences on analytical chemistry in the memory of Babko, Nazarenko, and Komar. The latter conference was organized by the laboratory staff in Kharkov in May, 2000. Our personnel participated in the Soviet–Japan Symposium on Analytical Chemistry (Moscow–Kiev, 1984), International Seminar on Critical Currents in Superconductors (Austria, 1994), international symposiums on the use of synchrotron radiation (Poland, 1995, 1998), International Congress on Analytical Chemistry (Moscow, 1977), Russia–Ukraine–Germany Symposia on Analytical Chemistry (Odessa, 1999, Baikal’sk, 2001), international conferences on the environmental protection (Galle, 1999; Athens, 2001), and Conference “Analytical Chemistry in the Black Sea Countries” (Odessa, 2001). International contacts of our laboratory were established at these conferences. Along with the long-standing close relations with Russian analysts (Scientific Council on Analytical Chemistry of the Russian Academy of Sciences; Vernadsky Institute of Geochemistry and Analytical Chemistry, Russian Academy of Sciences; Kurnakov Institute of General and Inorganic Chemistry, Russian Academy of Sciences; Institute of Problems of Chemical Physics, Russian Academy of Sciences; Institute of Inorganic Chemistry, Siberian Division, Russian Academy of Sci-
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ences; Institute of the Earth’s Crust, Siberian Division, Russian Academy of Sciences; Moscow State University; St. Petersburg State Technical University; and many other scientific organizations and higher education establishments of Russia), scientific contacts have recently been established with German, Greek, and Polish scientists. The laboratory is involved in the international project on the study of the technogenic contamination of natural and potable waters, which is performed in cooperation with scientists from the Ioannina University (Greece) and supported by the Ministry of Environmental Protection of Greece.
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Any scientific team has no future without an afflux of talented youth people and training highly skilled personnel. One doctoral and 21 candidate dissertations were defended over the period the laboratory exists. Almost every year young scientists after postgraduate courses and graduate students of Kharkov institutes come to the laboratory. The laboratory begins its 41st year of activity with good traditions, highly skilled personnel, fairly good material resources, new ideas, and wide scientific and production relations. This is the keystone of our future success.
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