| Faculty of Natural Sciences / Comenius University / Prirodovedecka fakulta - S o u r c e : Title of Journal: Acta Geologica Universitatis Comenianae Published by: Comenius University - Faculty of Natural Sciences Bratislava Year: 1999, Number: 53 - ACTA GEOLOGICA UNIVERSITATIS COMENIANAE Nr. 53, Bratislava 1999 DEVELOPMENT OF ATOMIC SPECTROSCOPY METHODS IN GEOLOGICAL INSTITUTES OF FACULTY OF NATURAL SCIENCES COMENIUS UNIVERSITY AND SLOVAK ACADEMY OF SCIENCE Jan Medved Geological Institute, Faculty of Natural Sciences, Comenius University, Mlynska dolina G, 842 15 Bratislava, Slovakia Key words: Atomic emission spectroscopy, atomic absorption spectroscopy, geological materials Abstract: Development of atomic spectrochemistry methods in Geological Institute of Faculty of Natural Sciences, Comenius University (GI FNS CU) is connected with its establishment in 1957. Its instrumental equipment and location resulted from the already existing Laboratory in the Chair for Mineralogy and Crystallography of FNS CU. In Geological Institute of Slovak Academy of Science (GI SAS) the development of atomic spectroscopy methods started later, only since 1963, when the Member of Academy, Prof. RNDr. B. Cambel, DrSc. became its director. In both Institutes the methods of atomic emission spectrography were used as first. A new quality in the development started since 1969 when the Institutes moved to common buildings in Petrzalka, the first atomic absorption spectrometers were acquired and the Institutes were "strengthened" by coming of Prof. Ing. E. Plsko, DrSc. In the following years the Institutes started to collaborate with some other organisations which were equipped with new facilities, e.g. in 1975 with X-ray fluorescence spectrometer, electron microprobe and in 1985 with inductively coupled plasma atomic emission spectrometer. This enabled to improve essentially the quality of research activities of both Institutes in the chemical characterisation of geological materials, as well as in pedagogical work (students practice, diploma works and dissertations). In the present time characterized by new economic conditions a reduction of GI SAS laboratory activities has been realised. The laboratories of the GI FNS CU have, thanks to their director Ing. V. Stresko, PhD. shown also henceforward a rich research, pedagogical and society activities what can be documented by numerous publications, citations, obtained awards, representations in professional societies and commissions, local and foreign advisory boards, accreditation boards etc. ACTA GEOLOGICA UNIVERSITATIS COMENIANAE Nr. 53, 59 - 65 Bratislava 1998 The beginning of the atomic spectrochemistry application in Slovakia - namely, of the optical emission spectrography in the field of geological sciences may have been dated since 1946, when the first spectrograph (large autocollimation, for the wavelength region 280 - 470 nm, Hilger E 492, Great Britain) was obtained in the framework of help of UNRRA by the former Slovak Geological Institute (at present Geological Survey of Slovak Republic). The mentioned method was here adopted in a short time by RNDr. G. Kupco, PhD. and applied to the analysis of geological materials. Thanks to his merits first quantitative determinations of elements in Slovakia based on know-ledge of GERLACH'S (1933) and KAISER'S (1947, 1949) results (use of reference elements and transformation of spectral lines blackening to corresponding logarithmic intensity values) were performed. Further development of atomic spectrochemistry methods in years 1953 - 1960 was achieved in the Chair for Mineralogy and Crystallography FNS CU and Institute of Inorganic Chemistry SAS in Bratislava (MATHERNY 1991). The institutions were equipped with middle dispersion spectrographs ISP - 22 (USSR) and Q - 24 (Carl Zeiss Jena GDR) inclusive of complete accessories. In the Chair for Mineralogy and Crystallography FNS CU, the research headed by Prof. Ing. M. Matherny, DrSc. was mostly of application character, oriented on geological prospecting using semi - quantitative evaluation by means of so called standard paper density (s.p.d.) scale (introduced later by RNDr. I. Matula in the Geological Survey laboratories in Spisska Nova Ves), as well as on quantitative powder and solution methods for the analysis of ore samples and silicate rocks. Apart from that, Prof. Matherny organised practice for students of the Faculty and later lectured "Microchemistry" and "Laboratory methods for research of minerals" till his move to Kosice in January 1961, where he became the head of Chair for Chemistry at the Metallurgical Faculty of Technical University (FLORIAN 1991). Spectroscopic research at the Institute of Inorganic Chemistry SAS, performed by Prof. Ing. Plsko was, DrSc. oriented towards the possibilities of practical utilisation of spectrography (PLSKO - MATIASOVSKY 1954), problems of powdered samples transportation into excitation medium (PLSKO 1962 a), further towards the complex investigation of evaporation processes at the spectral excitation in different excitation sources (PLSKO 1962 b, 1963 and 1964), homology valuation and choice of analytical spectral line pairs (PLSKO 1963 a), etc. The publishing of Prof. Plsko s book "Practical fundamentals of optical methods in chemistry" (PLSKO 1963 b), practically the first Slovak spectrochemical monography, represented a great contribution to students, andergraduate and graduate students and all workers in the field of spectrochemistry. This stage of the development of Slovak atomic spectrochemistry culminated in the organisation of the 2nd Czechoslovak Spectrographic Congress in Tatranska Lomnica on 5 - 10 Oct. 1959, performed under the patronage of Comenius University in Bratislava, at which 236 specialists including 76 foreigners participated. Lectures including discussions of this congress were published in special Proceedings (Acta Geol. - Geograph. Univ. Commenianae, Geologica, No. 6, 1959). They were valued very positively in foreign professional press. The presentation of this introductory information was necessary, since the orientation of the later created laboratories of GI FNS CU and SAS has directly followed activities of the mentioned institutions. The development of scientific research work in Chair of Comenius University oriented on geological sciences claimed to create a common documentation, laboratory and technical base. Consequently, in 1957 the Geological - Geographical Institute of Comenius University (at present GI FNS CU) was established. For the establishing of the new Institute some chemical and physical laboratories of the Chair for Mineralogy and Petrography with their facilities, rooms and staff served as the basis. The Member of Academy, Prof. RNDr. D. Andrusov, DrSc. was nominated as its first director. Since 1958 the Member of Academy Prof. RNDr. B. Cambel, DrSc. filled the function of director with exception of the period 1959 - 61, when he served as Dean of the Faculty and was substituted by Prof. RNDr. A. Gorek, PhD. (HOVORKA 1991, Collective of autors 1992). In 1959 Assoc. Prof. RNDr. J. Jarkovsky, DrSc. from the Dionyz Stur Geological Institute joined the Institute and together with Prof. Cambel started a comprehensive chemical characterisation of some sulphide iron ores (pyrites, pyrrhotite) of different genetic types and from different parts of Slovakia, as well as from foreign regions, followed by geochemical interpretation. For quantitative determination of trace elements Assoc. Prof. Jarkovsky worked out and applied at that time up-to-date method of optical emission spectrography by using a more powerful grating spectrograph PGS 2 (Carl Zeiss Jena, Germany) acquired by the Institute in 1963. The obtained results are summed up in several papers (JARKOVSKY 1964, CAMBEL - JARKOV- SKY 1966, JARKOVSKY 1966) and two books (CAMBEL - JARKOVSKYAMBEL - JARKOVSKY 1969). Apart from that, he worked also on spectrographic determination of trace elements in further sulphide minerals - galenites (JARKOVSKY - POLAKOVICOVA - STRESKO 1970), chalcopyrites (JARKOVSKY - PLSKO - STRESKO 1979), as well as in other geological materials (JARKOVSKY 1969, JARKOVSKY 1970). In the period after 1966 the Department of Analytical Chemistry GI FNS CU organised numerous conferences, symposia and seminars even with foreign participation. Let us mention at least some of them: Four conferences in Smolenice (1966, 1969, 1973, 1990) and one seminar in Tatranska Lomnica (1979), two Czechoslovak spectroscopic conferences (4th in Strbske Pleso, 1970 and 6th in Nitra, 1980) organised in collaboration with Czechoslovak Spectroscopic Society in Prague. Lectures presented in some of these conferences were published e.g. in Acta Geol. - Geograph. Univ. Commenianae, Geologica, Bratislava, Nr. 15, 1968 or in special Proceedings: "Symposium on Methods for determination of low concentrations of elements in mineral raw materials" published by Comenius University, Bratislava 1971. All these conferences contributed essentially to the development of spectrochemistry in Slovakia and to international propagation of our scientific results. Practically simultaneously with the establishing of the GI FNS CU the GI SAS was founded. Merits connected with its foundation and first ten years of its existence belonged to Prof. D. Andrusov, who had become the chairman of the Commission for geology at the Section of mathematical and natural sciences of SAS and after the establishing of Geological Laboratory of SAS (later GI) in 1955, worked as the first director till 1963. In this year Prof. B. Cambel was nominated as the director. Beside the existing geological departments, a new Department for Geochemistry, Mineralogy and Petrology was established (CAMBEL 1994). Thanks to the professional foresight, position and abilities of the new director, different laboratories started very quickly to be built, mainly for chemical analysis of rocks and minerals, spectrochemical laboratory, laboratory for thermal analysis, for separations, for sedimentology and others. He has entered into fruitful relations with the University Institute (J. JARKOVSKY, V. STRESKO and later E. PLSKO) where future co-workers of the GI SAS e.g. J. Kristin and J. Medved have been chosen among the students and prepared during the special practice and in the segregate diploma works. After having finished their study they entered laboratories of the GI SAS. RNDr. J. Medved, PhD devoted himself under the supervision of Assoc. Prof. RNDr. J. Jarkovsky, DrSc. and in collaboration with Ing. E. Martiny, PhD. to spectrochemical determination of trace elements in carbonate rocks (MEDVED - JARKOVSKY 1971, MEDVED - MARTINY 1971). The elaborated methodical procedures were used for analyses of hundreds calcite and dolomite samples from different regions of Western Carpathians and the results have been used also by Prof. J. Veiser and RNDr. R. Demovic in their dissertations. During Prof. Cambel's service as the rector of the University in 1966 - 1969 it succeeded to acquire and to adapt to laboratories the late Jelinek's barracks in Petrzalka, where the Military Chair of the University was situated. Into these rooms all laboratories of the GI FNS CU and SAS, as well as the Chair for engineering geology and hydrogeology moved. More pretentious instruments and technical personnel have increased. A great contribution was gained by the acquisition of the first atomic absorption spectrometer Unicam SP-90 (Great Britain) at the beginning of 1969 in Slovakia and a half year later of the second instrument Perkin - Elmer 303 (U.S.A.). Already experienced analytical chemical engineers V. Stresko, PhD. and E. Martiny, PhD. started to devote themselves to this new analytical technique - atomic absorption and they obtained fast the necessary skill and published their results (STRESKO - MARTINY 1972, MEDVED - MARTINY 1971). After a short time the Institutes served as teaching centre in this field for the whole Slovakia and even for abroad. In this way it was possible to create good conditions for the development of analyses of geological materials and their mineral and geochemical research for cca 15 years, till the erection of the new geological pavilion of FNS CU in Mlynska dolina. An expressive break in development and application of spectrochemical methods in the field of chemical characterisation of rocks, minerals, waters and similar materials was manifested in 1970 by the arrival of Prof. E. Plsko and his co-worker RNDr. J. Kubova, PhD. to the services of GI FNS CU. Prof. Plsko became the Head of the newly created Department of Analytical Chemistry and the Head applied fully scale applied his rich theoretical knowledge and practical experiences, as well as his broad international contacts. Besides the continuation and improvement of concrete routine analytical work performed for the needs of geologists, analytical research consisting in systematic study of some basic problems aimed at elaboration, valuation and finally application of new, more effective analytical procedures has been started. These tasks were reflected for the first time in the so- lution of own research problems officially accepted and included in two projects of the State plane of basic research ensuring necessary funds for the development of the Department and in one international project of Comecon "Intergeotechnika". In addition to this the Department took regularly part in analysing of geological reference materials for their certification (Germany, France, U.S.A., U.S.S.R. and naturally CSSR). All these activities increased recognition of Department and leading position among similar working places not only in local but also in international scale and enabled an uncommon professional growth and prestige of its coworkers. Thanks to all activities of Prof. E. Plsko, who became the "professional and spiritual father of the whole group of associates, a wide range of research tasks was solved and published (STRESKO - PLSKO 1977, PLSKO - Kubova 1973, Medved - Plsko - Cubinek 1974, Kubova - Plsko 1977, Medved - Kubova - Plsko 1979, Plsko - Martiny 1979 etc.), laboratory equipment was fully used for the needs of University and Academy and on the basis of results obtained from tests and analyses a great number of books (Hovorka - Rojkovic 1976, Hovorka 1978, Cambel - Jarkovsky 1979, Cambel - Kamenicky 1982, Cambel - Vilinovic 1987) and papers (Cambel - Kamenicky - Medved 1979, Cambel - Medved 1981, Cambel - Medved - Pitonak 1981) were published. Prof. Plsko's pedagogical work can also be rated as very significant. His lectures always created extreme interest in audience by his ability to contact students what often led to collaboration, working the diploma works, dissertations and to personal lasting friendship. Besides of that his co-workers became by his support and under his patronage active in the Czechoslovak Spectroscopic Society at the Czechoslovak Academy of Science in Prague (Plsko - chairman 1970- 1973 and many years 1st vice-chairman, Stresko - 1st vice-chairman and member of the Main Committee, Kubova - head of the group for spectroscopy of non-conducting materials and member of the Main Committee, Martiny, Medved - members of the Main Committee). The period after 1975 was signified by an extension of some financially pretentious branches of spectroscopy - X ray fluorescence (preferentially for determination of main components in rocks) and electron microprobe analysis (for investigation of spot and space - topographic distribution of elements in geological materials). The working and utilisation of these techniques has already been shared by more institutions. In this vay elaborated methodical procedures co- vered the determination of main, secondary and trace components in a relatively broad scale of geological materials (silicate rocks - acidic, basic, ultrabasic, weathered, soils; carbonates - calcites, dolomites, magnesites, siderites; sulphides - pyrites, pyrrhotites, chalcopyrites, antimonites, galenites sphalerites; different other materials). In all these procedures special stress was dedicated to the reliability of obtained results by using several independent analytical methods, as well as certified reference materials (Plsko - Medved 1981, Medved - Plsko 1982, Kubova - Plsko 1983, Medved - Kubova - Plsko - Budic 1986). Good conditions for education of students were created too and they were enabled to participate directly in laboratory research activities of the institutes or chairs in compiling working of their diploma works or dissertations. The listed, really informal co-operation existed not only on the basis of official agreements signed between the Comenius University and the Presidium of the Slovak Academy of Science but in particular thanks to both managements of the mentioned institutes, as well as all their scientists and technicians. Significant was also international collaboration especially with E. Kardel University and B. Kidric Chemical Institute in Ljubljana (Slovenia), M. Luther University in Halle (Germany) and Institute for Geochemistry, petrology, geology and mineralogy in Moscow (Russia), in the frame of which several mutual , even long term study stays were realised. Since March the 1st 1981 the Department of Mineral Raw Materials of GI SAS has started its activities in Banska Bystrica (headed by Doc. RNDr. M. Haber, PhD). The establishment and instrumentation of the new laboratory, as well as instructing of its future co-workers (RNDr. P Andras, PhD; RNDr. M. Hrnciarova and others) was secured very intensively by scientists from both Institutes in Bratislava, so that the laboratories were in a short time able to perform pretentious analytical work in which basic analytical methods were represented by AAS and in OES. This contributed to an essential way to early and successful solution of basic geological, to metallogenetical and petrological - volcanic problems connected with the formation of ore deposits and complex utilization of their ores (CAMBEL 1994). Since 1970 the Department of Analytical Chemistry has been deeply involved in the successful course of "seminars" organised by the Chair for Chemistry, Metallurgical Faculty, Technical University in Kosice which have become important professional events not only in the former Czechoslovakia. Till now, they have been organised 13 times (the last one in 1996 in Podbanske) and it is laudable that they have been conserved also in contemporaneous difficult conditions of managing and financing of the science. Owing to the construction of a new dwelling area in Petrzalka, laboratories situated there were in 1986 wound up and moved to the new pavilions of FNS CU and to the GI SAS in Patronka. In spite of this territorial separation their traditional cooperation continued mainly in research field. The interest was concentrated chiefly on the possibility of gold determination in rocks by using of appropriate preconcentration procedures (Stresko - Toman - Kolcava 1987, Stresko - Martiny 1987, Medved - Martiny - Plsko - Feriancik 1987), on the preconcentration of trace elements from mineral waters (Polakovicova - Stresko - Kubova - Plsko 1987, Zemberyova - Vackova - Stresko 1989) and on the determination of rare earth elements in geological materials (Plsko 1986, Kubova - Hvozdara - Plsko - Polakovi- cova 1988). In the field of development and application of chemical decomposition of geological materials , as well as utilisation of preconcentration procedures for determination of very low contents of elements significant contribution of Ing. J. Polakovicova, PhD. has to be appreciated. In 1985 the University Institute acquired atomic emission spectrometer with inductively coupled plasma AES-ICP (Plasmakon S-35, KONTRON, Germany). Prof. E. Plsko and Dr. J. Kubova were busy with the new method and J. Kubova has become at present the best specialist in this field in the whole Slovakia. In a short time after the setting of the instrumenting working first papers in different journals have already appeared (Kubova - Plsko 1986, Stresko - Kubova - Polakovicova - Plsko 1986, Plsko 1987, Plsko - Stresko - Kubova 1988 and others). Special interest was evoked by the results representing possibilities to correct background and spectral interference occurring in AES- ICP. (Plsko 1989, Plsko 1990, Plsko 1991) and to analyse solid samples (PLSKO 1988, Plsko 1993). Some changes occurred in 1990 when Prof. E. Plsko retired from active work, Dr. J. Kubova succeeded him in the advisory board of prestige spectroscopic journal (Journal of Analytical Atomic Spectroscopy, Great Britain) and Dr. J. Medved took up the post in the GI FNS CU, Ing. V. Stresko became the head of the Department of Analytical chemistry and two years later he won the competition and was nominated as the director of the Institute. Under his directorship the institute has in hard economic conditions not only "kept on", but even advanced. A recent type of atomic absorption spectrometer Perkin-Elmer 1100 enabling to get faster and more reliable analytical results was hired. The professional work of laboratories was in this period of time focused chiefly on determination of trace elements in soils by using of atomic spectroscopy methods (Medved - Stresko - Kubova - Polakovicova - Curlik 1992), on determination of extremely low concentrations of elements in waters, on determination of beryllium, rare earth elements and mercury in mineral waters (Polakovicova - Medved - Stresko - Kubova 1992, Kubova - Nevoral - Stresko 1994 a, Kubova - Nevoral - Stresko 1994 b, Stresko - Polakovicova - Kubova 1994), on optimisation of conditions and reliability of the used analytical methods (Medved - Stresko - Kubova - Polakovi- cova 1994), on determination of tantalum and niobium and low gold contents in geological materials (Kubova - Polakovicova - Stresko - Medved 1993, Polakovicova Medved - Kubova - Stresko - Celkova 1996, Stresko - Medved - Polakovi- cova - Kubova - Celkova 1996), on determination of elements in environmental samples (Kubova - Stresko - Celkova - Medved - Agrawal 1996, Kubova - Hanakova - Medved - Stresko 1997) and on hydride techniques (HG-AAS) for the determination of As, Se, Sb (Celkova - Stresko - Medved - Kubova - Polakovicova 1995). The further research was recently oriented on effectiveness the valuation of effectiveness of decomposition for the determination of various elements in soils (Medved - Stresko - Kubova - Polakovicova - Celkova 1996, Kubova -Medved - Stresko - Polakovicova 1997). The work of authors Medved - Stresko - Kubova - Polakovicova - Celkova (1996) "Evaluation of the efficiency of the decomposition procedure for the determination of some elements in soils by atomic spectroscopy methods" presented on international conference EUROANALYSIS IX held on 1 - 9 Sept. 1996 in Bologna (Italy) was awarded by bronze medal "Giovanni Canneri" of the Italian Chemical Society, by a professional book and annual subscription of the journal "Accreditation and Quality Assurance" published by Spriger-Verlag (Germany). After the split of the Czechoslovak federation in 1993 the division of J. Marcus Marci Spectroscopic Society was actual, too. In our country Slovak Spectroscopic Society was established. Thanks to activities of the Main committee members of the Czechoslovak Society, Ing, V. Stresko and Dr. J. Kubova, it was possible to gain funds necessary for starting of these activities in Slovakia. Ing. V. Stresko became the first chairman of the Society, Dr. J. Kubova its secretary and Dr. J. Medved the committee member. The society already organised several professional events and courses. At present time, the Society counts 115 individual and 8 collective members. At the conclusion it is necessary to state that in this brief review it is extremely difficult to list all the most important activities of the GI FNS CU and SAS. 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STRESKO, V. - MEDVED, J. - POLAKOVICOVA, J. - KUBOVA, J. - CELKOVA, A. (1996): Determination of gold in geological materials by atomic spectroscopy methods after preconcen- tration. CANAS 95, Colloquium Analytische Atomspektrokopie. Uberlingen, 455-460. ZEMBERYOVA, M. - VACKOVA, M. - STRESKO, V. (1989): Stanovenie Cu, Pb a Cd v mineralnych vodach za pouzitia extrakcie. Hydrochemia, 89, 3-17. - S o u r c e : Title of Journal: Acta Geologica Universitatis Comenianae Published by: Comenius University - Faculty of Natural Sciences Bratislava Year: 1999, Number: 53 - Faculty of Natural Sciences / Comenius University / Prirodovedecka fakulta | |
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