ࡱ> Y[TUVWXnM ibjbj== WWu]lpppptlΤ,tlFz(Щ$J j#޲#XppЩ*XXXp|8ЩXXX0V n ς8l| y $(0FTd:dXllpppp SEDIMENTS FROM SAVINJA, VOGLAJNA AND HUDINJA RIVERS (SLOVENIA), REFLECTING ANOMALIES IN AN OLD METALLURGIC AREA Stanislav Fran iakovi-Bilinski1*, Halka Bilinski1, Darko Tibljaa2 and Darko Han~el3 1Institute  Ruer Boakovi , POB 180, 10002 Zagreb, Croatia 2Department of Mineralogy and Petrology, Faculty of Science, University of Zagreb, Horvatovac bb, 10000 Zagreb, Croatia 3Institute  Jo~ef Stefan , Jamova 39, 1001 Ljubljana, Slovenia SUMMARY Stream sediments from Savinja and its tributaries, Voglajna and Hudinja rivers, which drain an old metallurgic area of Slovenia, have been studied by detailed mineralogical, chemical, Mssbauer and geostatistical methods. It is a case study, which provides an example for a possible chemical threat to aquatic ecosystems, such as toxic contamination with Zn, Cd, Cu, Ni, Pb, Ag, Hg and As, in the Celje area. Concentrations of 53 elements were determined in fractions <63 m by ICP-MS. Cluster analysis of Q-mo- dality, applied on total geochemical data set, was used to dis-aggregate it into three subsets. The geochemistry of stream sediments belonging to the largest cluster has been used to identify the background geochemical signatures, related to geology of the drainage basin area. 57Fe Mssbauer spectroscopy at room temperature was used to study iron, which is a major element, partly present in poorly crystalline compounds (oxides and hydroxides). Spectra were fitted with two to four doublets. Hyperfine parameters were obtained and Fe(III)/Fe(II) ratio was cal-culated. The ratio is higher in Voglajna than in Savinja and Hudinja. Fe(III) is retained in silicates, or as finely dispersed iron oxide. Fe(II) is assumed to be retained in calcite, dolomite and chlorite. Regarding contamination of the studied region, some improvement was observed. Anthropogenic association due to iron metallurgy in the recent past, detected lately on attic dust, was not detected in recent sediments. Anthropogenic association Ti-Nb, reflecting titanium oxide production, is still observed in recent sediments. Highly correlable high concentrations of Zn, Ag and Cd show that these elements still reflect metallurgic activity in Celje region. In spite of elevated concentrations of toxic elements within the Celje region, only in two locations concentrations of several toxic elements are above the values, which can cause serious toxic effects with respect to recommended sediment quality criteria. KEYWORDS: stream sediments, Savinja, Voglajna, Hudinja, mineral composition, chemical composition, anomalies` determination. INTRODUCTION Celje region in central Slovenia attracted scientific interest during the past and recent times as an industrial district. There is metal-manufacturing and chemical industry in Celje region, which affected water and sediments of the Hudinja, Voglajna, Savinja and Sava rivers. Several papers were written on sediments of this region. Some of the most important will be mentioned in chronological order: In 1976, tern and Frstner [1] performed the first preliminary geochemical investigations of stream sediments of the Sava River basin in Slovenia. According to them, one of the most polluted water flowing in Slovenia was Voglajna. They found in one studied sample that, in the Voglajna River sediment, chromium and zinc were enriched by a factor of more than 100, copper, lead and cadmium by a factor of 2550, compared with the geochemical background. It was assumed that effluents from the old waste dumps of zinc-works, from iron-works near tore, from a TiO2-factory, and from an enamel pottery factory, are the contributors to the unusually high metal contamination in Voglajna. In 2002, Fran iakovi-Bilinski et al. [2] presented preliminary results of characterization of sediments from Voglajna and Savinja Rivers (samples 1-6 in this article). According to these preliminary results, S, P, Cr, Ni, Pb, Cu, Mo, Sb, W and Hg show the highest concentrations in sediment of Voglajna near tore (sample 4), while the highest concentrations of Zn, Cd, Ag and Au are present in sediment of Savinja River at Tremerje (sample 5), about 5 km downstream from Celje. These results indicate continuation of an industrial pollution in this region. }ibret [3] investigated the mass balance of heavy metals in Celje area, using samples of attic dust and soil. His results showed that the environment is contaminated with heavy metals, especially with zinc and cadmium, which is the consequence of 100 years of smelting the sphalerite ore in the Cinkarna Celje factory. It was possible to calculate the emissions of heavy metals in the environment. These calculations show for Celje region that emission of Zn is 1712 tons, and the natural background has been estimated to be 207 tons. Similar proportion between anthropogenic and natural emissions can be seen for Cd (9.1 tons of anthropogenic and 1.4 tons of natural Cd). The opposite ratio was observed for elements whose presence is influenced mainly by lithology (for example Al). `ajn [4] used the same sampling media as }ibret [3] for the identification of anthropogenic and geogenic element sources in Celje region. He assumed one natural geochemical association (Al-Ce-K-La-Li-Rb-Sc-Th) and three anthropogenic geochemical ones. The anthropogenic associations are: (Ag-As-Cd-Cu-Hg-Mo-Pb-S-Sb-Zn), which is the result of zinc and sulphuric acid production in the past; (Co-Cr-Fe-Mn-Ni), which is the result of iron metallurgy; and the third athropogenic association (Nb-Ti), which is the result of titanium oxide production. The aim of the present work The aim of the work is to present levels and sources of major and trace elements in stream sediments of Savinja, Voglajna and Hudinja rivers, belonging to the Sava River basin. They are still heavily impacted with different metallurgical activities, which are decreasing in recent years. One of the aims is to establish if this decrease resulted in reduction of sediment pollution. Statistical analysis applied on these data will be used to detect anomalies in this region, and to identify background geochemical signature related to the geology of the drainage basin. Possible toxicity of some elements will be discussed according to the existing sediment quality criteria. STUDY AREA The study area of Savinja, Voglajna and Hudinja drainage basins with numbers of sampling locations is presented in Figure 1. This area is located in the eastern part of Slovenia. The geology of Slovenia is very interesting, because of its high diversity, as described by Pirc [5]. The geology of the Voglajna region was described in detail by Nosan [6]. The northern border of the Lako syncline east the Savinja River was studied by Hamrla [7]. For more recent geological data, the reader is referred to Buser [8]. The studied area represents a young tectonic basin, which is filled with Quaternary deposits of Savinja, Voglajna and Hudinja rivers. In the northern part, there are Pleistocene clays, quartz gravel and sand. In the SE part, Miocene sand, sandstone, marly limestone and lithothamnian limestone are also exposed as part of the Celje syncline. The oldest rocks crop out in the southern part. These rivers were poorly studied in terms of geochemistry. However, Slovenian averages of elements in soil can be used for comparison (Pirc, [9]; Andjelov, [10]; ajn, [11]).  FIGURE 1 - Study area with numbers of sampling stations. EXPERIMENTAL Sampling and sample preparation Sampling of stream sediments was performed on three occasions. Samples 1-6 were taken on 27th August 2001, and samples 4750 were taken on 27th August 2002, both during low water regime, whereas samples 7984 were taken on 19th November 2002, during high water flow. Sampling was performed further away from the river bank to avoid contamination from the soil. Sediments were wet-sieved and then dried at 80 C. Sediment fractions containing silt and clay (<63 m) were further analyzed. Mineralogical analysis Mineral composition of sediments (fraction <63 m) was determined by X-ray powder diffraction method using a Philips X-Pert MPD diffractometer (Cu tube, graphite monochromator, generator settings: 40 kV, 40 mA, range scanned 4-63 2). Crystalline phases were identified by comparison with Powder Diffraction File [12] using the computer program X Pert High score [13]. Chemical analysis Chemical analysis was performed in ACTLABS commercial laboratory, Ontario, Canada, in fraction <63 m, using ICP-MS (Inductively Coupled Plasma Mass Spectroscopy), with program  Ultratrace 2 . The procedure was as follows: 0.5 g of sample is dissolved in aqua regia at 90 C in a microwave digestion unit. The solution is diluted and analyzed using a Perkin Elmer SCIEX ELAN 6100 ICP-MS instrument. For analysis, the following reference materials were used: USGS GXR-1, GXR-2, GXR-4 and GXR-6, which were analyzed at the beginning and after analysis of each series of samples. Although this digestion is not total, its use is justified because the international standard methods for determining action limits are based on aqua regia leach [14]. Mssbauer spectroscopy Poorly crystalline iron phases were studied by Mssbauer spectroscopy at 300 K. For all experiments, we used a 57Co source with an activity of ~10 mCi in an Rh matrix. The velocity scale was calibrated by metallic Fe, which was also used as a reference for the isomer shift parameters. The speciations were computer-fitted by assuming Lorentzian or Voigt shapes for the resonance lines. Statistical methods Program Statistica 6.0 [15] was used for preliminary statistical calculations, based on 16 up-to-now collected samples. The total data set was used to determine samples with anomalies and outliers. Cluster analysis of Q-modality was performed using the total data set to determine the subset, not containing significant anomalies [16], from which basic statistical parameters were calculated. Correlation analysis was performed to find out mutual dependence of elements in sediments, which can be compared with anthropogenic associations of ajn [4], obtained on different sampling media. RESULTS X-ray diffraction Mineral composition of sediments (fraction <63 m) from Voglajna, Savinja and Hudinja rivers are presented in Table 1. Quartz predominates as a major mineral in all sediment samples. Among other major minerals, albite was found in locations 1 and 3; muscovite in locations 2, 79 and 82; calcite in locations 4, 5, 6 and 82; and dolomite in locations 6 and 81. As minor minerals, muscovite was found in locations 1, 4, 5, 6, 47, 48, 49, 50, 80, 81 and 84; albite in locations 2 and 48; calcite in locations 3, 47, 49, 50, 79, 80, 81, 83 and 84; microcline in location 81; and chlorite group minerals in locations 79 and 82. Depending on location, there are several trace minerals, mostly from chlorite group, clay mineral group and oxide and hydroxide group. Classification of minerals was according to Klein and Hurlbut [17] and Klockmanns [18]. Among minor and trace minerals, there were those which contain Fe-ion in the structure. These are montmorillonite, clinochlore, muscovite and goethite. It should be mentioned that trace minerals present at concentrations <5% were near the detection limit of XRD. Therefore, they are very probable, but not completely certain. The program XPert gave the numbers of the JCPDF cards, which have the best fit with experimental data. Therefore, for further investigation, Mssbauer spectroscopy will be applied as comparative technique. Elemental analysis of sediments from Savinja River drainage basin Table 2 shows results of elemental analysis (56 elements) of sediments from Savinja, Voglajna and Hudinja rivers. Among the analyzed elements, the most abundant are Fe and Ca. Concentration of Ca was significantly higher in Savinja and Hudinja than in Voglajna. Concentrations of Al and K were similar in samples of Savinja and Voglajna, however, higher concentrations were found in Dobrinjski Potok (sample 47) and in Hudinja (sample 79). The highest concentration of Mn was found in Voglajna (sample 2). Among microelements, the highest concentrations of S, P, Cr, Mo, Sb and W were found in Voglajna (sample 4). The highest concentrations of Zn, Cd and Hg were found in the vicinity of Celje (Zn in samples 5 and 49; Cd and Hg in sample 49). 57Fe Mssbauer spectroscopy To get more information about iron minerals, which are known to be carriers of numerous trace elements and are very abundant in the studied region, 57Fe Mssbauer spectra were taken at room temperature. Spectra of samples 1-6 were already published by Fran iakovi-Bilinski et al. [2]. Mssbauer spectra of other samples (47, 48, 49, 79, 82, 83 and 84) are presented in Figure 2. Spectra were fitted with two doublets in sample 79; with three doublets in samples 47, 82, 83 and 84; and with four doublets in samples 48 and 49. Hyperfine parameters, such as isomer shift (IS) and electric quadrupole splitting (QS), together with the relative resonance area (A, in percent of total iron) are presented in Table 3. In this table are also included already published values of hyperfine parameters for samples 1-6 [2]. Mssbauer spectroscopy can provide quantitative information about the relative population of the iron species, together with specific properties of the individual iron sites. The Fe(III)/Fe(II) ratio was calculated and included in Table 3. The lowest ratio was found in Savinja (sample 6), and the highest one in Lo nica (sample 48). Table 1 - Mineral composition of <63 m sediment fraction from Hudinja, Voglajna and Savinja rivers. No.Location, river (lake)Major mineralsMinor mineralsTrace minerals1Zg. Rakitovec, Slivniko lakequartz (46-1045) albite ordered (09-0466)muscovite (01-1098)montmorillonite (13-135) kaolinite (29-1488) clinoenstatite (35-610)2Gorica, Voglajnaquartz (46-1045) muscovite (7-25)albite ordered (09-0466)kaolinite (29-1488) clinochlore, ferroan (07-0076) montmorillonite (13-135) Mg-calcite (43-0697) calcite (05-0586) dolomite (36-0426)3Vrbno, Voglajnaquartz (46-1045) albite ordered (09-0466)calcite (05-0586)muscovite (01-1098) kaolinite (29-1488) clinochlore, ferroan (07-0076) Mg-calcite (43-0697) dolomite (36-0426) montmorillonite (13-135)4Teharje-tore, Voglajnaquartz (46-1045) calcite (05-0586)muscovite (01-1098)albite ordered (09-0466) clinochlore, ferroan (07-0076) montmorillonite (13-135) kaolinite (29-1488) dolomite (36-0426)5Tremerje, Savinjaquartz (46-1045) calcite (05-0586)muscovite (01-1098)dolomite (36-0426) clinochlore, ferroan (07-0076) albite ordered (09-0466)6Letu, Savinjaquartz (46-1045) calcite (05-0586) dolomite (36-0426)muscovite (01-1098)albite ordered (09-0466) clinochlore, ferroan (07-0076) Mg-calcite (43-0697)47Hrastje, Dobrinjski potokquartz (01-089-8934) calcite (01-081-2027) muscovite (00-001-1098)albite ordered (00-020-0554) clinochlore ferrian (00-007-0078) dolomite (00-036-0426)48Lipovec, Lo nicaquartz (01-070-3755)muscovite (00-070-3755) albite ordered (00-009-0466)vermicullite (01-076-0847) goethite (00-029-0713)49Celje, Voglajnaquartz (01-078-1252)muscovite (00-007-0032) dolomite (01-073-2361) calcite (00-005-0586)clinochlore, ferroan (00-007-0076)50Celje, Savinjaquartz (00-046-1045)calcite (01-089-5862) dolomite (01-089-5862) muscovite vanadian (00-019-0814)albite ordered (00-009-0466)79Celje, Hudinjaquartz (01-070-3755) muscovite (00-006-0263)calcite (01-086-2334) dolomite (00-036-0426) clinochlore ferroan (00-029-0701)anorthoclase (00-009-0478)80Spodnja Hudinja, Hudinjaquartz (00-046-1045)muscovite (00-007-0042) calcite (01-086-2334) dolomite (01-083-1766)clinochlore ferroan (00-029-0701) muscovite vanadian barian (00-046-1409) albite ordered (00-009-0466)81kofja Vas, Hudinjaquartz (01-070-3755) dolomite (00-036-0426)muscovite (00-007-0042) calcite (01-086-2334) microcline (00-001-0705)clinochlore ferroan (00-029-0701) albite ordered (00-009-0466)82Vinja Vas, Hudinjaquartz (00-046-1045) calcite (01-086-2334) muscovite vanadian barian (00-046-1409)dolomite (01-075-1655) montmorillonite-chlorite (00-007-0027) chlorite serpentine (00-052-1044)illite (00-002-0050) albite calcian, ordered (00-041-1480)83Debro, Savinjaquartz (01-085-0457)calcite (01-086-2334) dolomite (00-036-0426)clinochlore ferroan (00-029-0701) muscovite (00-007-0032) albite ordered (00-009-0466)84Rimske Toplice Savinjaquartz (01-085-0457)calcite (01-083-0578) dolomite (01-075-1760) muscovite (00-001-1098)clinochlore feroan (00-007-0076) albite ordered (00-019-1184) Table 2 - Elements in sediments (fraction <63 m) from Hudinja. Voglajna and Savinja rivers (Slovenia). obtained by ICP-MS method. SampleLi (ppm)Be (ppm)B (ppm)Na (%)Mg (%)Al (%)P (%)S (%)K (%)Ca (%)Ti (%)V (ppm)Cr (ppm)Mn (ppm)120.51.1-10.0120.6161.3890.0320.0230.1260.569-0.01041.339.2708.0218.31.2-10.0190.5601.3410.0850.0860.1521.298-0.01043.835.513700.0314.11.1-10.0300.5851.0630.1720.1170.1223.141-0.01035.543.91140.0415.21.12.20.0400.9011.2100.1810.3230.1514.901-0.01034.271.81490.0518.70.725.60.0361.2651.1720.1100.2860.1168.483-0.01024.042.21030.0618.90.7-10.0212.0811.1510.0410.1470.0929.397-0.01025.919.4643.34742.01.310.40.0301.2802.3520.0550.1710.3463.053-0.01047.259.02590.04812.61.45.10.0200.3641.1880.0990.0610.1580.641-0.01078.366.02460.04931.81.1331.40.0801.4631.6580.1070.1880.2535.1740.03037.853.91270.05029.90.822.00.0351.4511.7010.0690.2320.1946.887-0.01026.341.81240.07930.41.1154.50.0451.6042.0180.0840.1360.255.4710.02241.745.0860.58022.70.913.30.0231.7121.6830.0720.1220.2275.4970.01634.535.7774.78123.40.85.40.0211.8191.6180.0680.1060.2445.6730.01533.336.2607.08224.90.85.10.0221.6831.7090.0650.1030.2714.6840.02636.740.2625.48323.60.930.50.0351.5061.5250.0710.1680.1585.5800.01426.841.81160.08423.20.816.80.0281.8341.4750.0780.2290.1476.6670.01127.942.11160.0    FIGURE 2 - Mssbauer spectra of 57Fe taken at room temperature with 57Co source in a Rh matrix: sediment fraction <63 m of selected samples. Table 3 - Hyperfine parameters of Mssbauer spectra of sediments (f < 63 m) from Voglajna, Hudinja and Savinja rivers obtained at room temperature. Nosub-spectraIS (mm/s)QS (mm/s)Heff (kOe)SiteA%Fe(III)/ Fe(II)1du1 du20.3521(19) 1.0966(58)0.6240(31) 2.648(11)0 0Fe(III) Fe(II)81.35(60) 18.65(70) 4.362du1 du20.3536(32) 1.101(15)0.6481(52) 2.686(29)0 0Fe(III) Fe(II)86.75(98) 13.3(12) 6.523du1 du20.3546(31) 1.097(11)0.6828(52) 2.655(22)0 0Fe(III) Fe(II)81.47(86) 18.5(10) 4.404du1 du2 se1 se20.3521(18) 1.0907(65) 0.316(18) 0.652(33)0.6475(30) 2.608(13) 0 00 0 511(13) 459(24)Fe(III) Fe(II) 70.43(45) 18.19(57) 7.38(53) 4.00(53) 3.875du1 du20.3531(52) 1.1207(81)0.6514(84) 2.649(16)0 0Fe(III) Fe(II)68.7(12) 31.3(14) 2.196du1 du2 du30.2503(46) 1.266(11) 1.176(47)0.845(11) 2.400(21) 2.05(22)0 0 0Fe(III) Fe(II) Fe(II)61.7(13) 25.1(68) 13.3(77) 1.6047du1 du2 du30.3620(29) 1.1212(37) 1.154(13)0.6276(52) 2.659(10) 2.019(26)0 0 0Fe(III) Fe(II) Fe(II)70.78(71) 25.0(13) 4.2(11)2.4248du1 du2 du3 du40.3663(31) 0.99(19) 1.126(78) 0.3705(43)0.491(17) 2.42(39) 2.73(15) 0.789(56)0 0 0 0Fe(III) Fe(II) Fe(II) Fe(III)31.0(12) 2.8(27) 5.4(25) 61.0(13)11.2249du1 du2 du3 du40.3906(78) 1.1219(80) 0.928(31) 0.249(10)0.6301(32) 2.646(16) 2.390(60) 0.661(13)0 0 0 0Fe(III) Fe(II) Fe(II) Fe(III)70.5(43) 18.1(15) 4.3(14) 7.2(38)3.4750-------79du1 du20.3677(60) 1.114(10)0.627(10) 2.636(21)0 0Fe(III) Fe(II)73.1(18) 26.9(22)2.7280-------81-------82du1 du2 du30.3573(40) 1.1150(41) 1.112(18)0.6692(69) 2.6450(91) 1.976(36)0 0 0Fe(III) Fe(II) Fe(II)66.48(89) 30.0(13) 3.48(64)1.9983du1 du2 du30.3637(67) 1.021(44) 1.1193(80)0.620(12) 2.213(89) 2.649(17)0 0 0Fe(III) Fe(II) Fe(II)66.2(22) 4.3(30) 29.4(33)1.9684du1 du2 du30.3674(85) 1.120(13) 1.002(43)0.603(14) 2.660(30) 2.247(82)0 0 0Fe(III) Fe(II) Fe(II)66.4(23) 29.0(42) 4.6(33)1.98- not measured IS (mm/s), the isomer shift relative to metallic ion QS (mm/s), the electric quadrupole splitting A (%), relative resonance area in percent of total iron Statistical analysis Q-modality cluster analysis On total set of geochemical data, Q-modality cluster analysis was performed. In the simplest case with three clusters, cluster 1 has only one sampling location (No.2). Cluster 2 included four sampling locations (No. 47, 48, 49 and 5). Cluster 3 consisted of eleven sampling locations (No. 1, 3, 4, 6, 50, 79, 80, 81, 82, 83 and 84). Basic statistical parameters were determined for cluster 3 and are presented in Table 4. For each element, the values are given as arithmetic mean, geometric mean, median, minimal and maximal concentrations, variance (2), standard deviation, skewness and kurtosis. The values for arithmetic mean ( standard deviation can be considered as tentative baseline values for elements studied in this region, until more locations are studied. Determination of anomalous values In Table 5 locations within Savinja River drainage basin, in which concentrations for some elements show anomalous values (extremes and/or outliers), are presented. Anomalous values were obtained using experimental data from Table 2 and two-dimensional scatter box diagrams from program STATISTICA 6.0. In sample 2, Mn showed an extreme value. It can be explained as a possible signature from an old enamel pottery factory in Gorica. In samples 48 and 47, Mn showed first and second outliers. Th had an extreme value in sample 47, and an outlier in sample 48. Anomalous values of Th, Mn, and some other elements (Li, Ga, V, Yb) found in the region without industrial activity (locations 47 and 48) are considered to be of natural geogene origin. Extremes of Mo and Sb, and outliers of numerous trace elements (P, Cr, Cu, Re, Pb, Bi, W) in sample 4, can be explained due to iron metallurgy in tore. The greatest number of elements with anomalous concentrations were found in Voglajna (extremes in sample 49) and Hudinja (outliers in sample 79), within the town of Celje. Zn anomaly was observed also in Savinja sample 5, collected about 5 km downstream of Celje. Furthermore, downstream Zn concentrations are still elevated but not so much. Except for that, sediments in other sampling locations further downstream, as well as those upstream of Voglajna confluence, do not show anomalous element concentrations. Table 4 - Basic statistical parameters for 53 elements in sediments of 11 sampling locations (cluster 3) from Savinja, Voglajna and Hudinja rivers. ElementMeanGeom. meanMedianMinimumMaximumVarianceStd.Dev.StandardSkewnessKurtosisLi (ppm)22.431021.862523.153014.098030.37026.65.15621.5546-0.05814-0.30314Be (ppm)0.91400.90360.86800.67701.1100.00.14360.04330.03518-1.26907B (ppm), i 22.44295.4080-1.0000154.5102027.145.022813.57493.007869.46296Na (%)0.02840.02670.02800.01200.0450.00.00970.00290.15568-0.52197Mg (%)1.43561.32861.60400.58502.0810.30.50740.1530-0.83202-0.60604Al (%)1.50381.47871.52501.06302.0180.10.28460.08580.01598-0.38786P (%)0.08480.07490.07090.03240.1810.00.04780.01441.448681.25293S (%)0.15490.13130.13610.02260.3230.00.08090.02440.673170.89606K (%)0.18020.17080.15800.09200.2710.00.06010.01810.19175-1.41319Ca (%)5.31514.53915.49700.56909.3974.92.21440.6677-0.484772.06223Ti (%)0.00500.0111-0.01000.0260.00.01490.00450.05943-1.98847V (ppm)33.112032.659934.198025.898041.69332.75.72011.72470.10897-1.21685Cr (ppm)41.545939.923441.772019.365071.835149.812.23853.69011.104014.70769Mn (ppm)946.2625903.2894860.5480606.96901490.00091424.4302.364791.16640.41472-1.16494Fe (%)3.68423.59523.33072.83605.6490.80.91850.27691.496311.29096Co (ppm)18.473617.790817.432011.643034.25834.75.88811.77532.062265.74985Ni (ppm)53.354752.056152.945036.336082.851168.512.98153.91411.192711.74216Cu (ppm)56.019446.812843.876819.7680138.7321456.238.159911.50561.444801.22568Zn (ppm)337.2074235.8671198.559266.04901040.00086501.5294.111388.67791.407602.24704Ga (ppm)4.18134.09933.81103.04905.9140.80.89500.26990.75662-0.44989As (ppm)17.327816.270016.343010.872030.46348.26.94292.09341.319100.82407Se (ppm)1.25581.14031.23300.34302.7160.30.56850.17141.520635.07508Rb (ppm)19.571618.721517.719010.063028.04534.85.89791.77830.09030-1.02324Sr (ppm)94.072386.9504101.491023.5740125.786942.230.69539.2550-1.175291.59517Y (ppm)12.154711.940411.24608.928017.0616.22.48720.74990.946280.00724Zr (ppm)0.91230.84821.03500.42601.3980.10.33440.1008-0.29640-1.40397Nb (ppm)0.63580.61050.60200.41400.8990.00.18770.05660.21014-1.74219Mo (ppm)1.56561.24571.10600.70906.2812.51.58970.47933.1287610.06627Ag (ppm)0.80570.6030-0.05003.0210.70.85310.25721.915984.53818Cd (ppm)1.64650.94300.69700.16307.3484.22.06010.62112.454796.73997In (ppm)0.05370.05040.04400.03000.0930.00.02040.00620.74620-0.60309Sn (ppm)2.26981.55571.39300.46708.4936.02.45680.74082.102053.99190Sb (ppm)1.24820.78550.75200.19206.7143.41.83630.55373.1666010.26152Te (ppm)0.06520.06180.07100.03100.0970.00.02080.0063-0.23407-0.97046Cs (ppm)1.42501.38591.52500.86301.8320.10.32810.0989-0.73451-0.70078Ba (ppm)367.9016223.0852161.568064.90001010.000138863.0372.6432112.35620.99182-0.73405La (ppm)16.625216.048015.55508.362023.90019.64.42811.33510.070970.30667Ce (ppm)35.885234.897735.149018.429047.78167.58.21602.4772-0.524031.02592Nd (ppm)16.475216.073016.29609.130022.06313.13.61571.0902-0.396110.52831Sm (ppm)3.65853.59393.57102.32304.6870.50.70370.2122-0.11180-0.02753Eu (ppm)0.75000.73780.74600.49100.9910.00.13870.0418-0.121610.12585Tb (ppm)0.48370.47570.45900.33600.6460.00.09320.02810.45306-0.38906Yb (ppm)0.95570.94010.93000.61101.2250.00.17470.0527-0.314870.24446Lu (ppm)0.11230.1290-0.10000.1610.00.07290.0220-2.914169.12940W (ppm)0.52860.3630-0.20002.7931.01.00050.30171.570811.76296Re (ppm)0.00100.0010-0.00100.0060.00.00200.00061.640864.26286Au (ppb)19.744222.5020-0.200038.357153.912.40633.7406-0.23214-0.66760Tl (ppm)0.24860.23830.22300.15800.4630.00.08420.02541.861334.02385Pb (ppm)57.150849.405252.246017.4440133.3881062.132.59039.82641.248092.11655Bi (ppm)0.42040.40240.36700.28000.7870.00.14530.04381.884653.70792Th (ppm)3.09042.94663.33901.11504.0500.70.82790.2496-1.370122.50435U (ppm)0.94410.92940.94300.58701.2150.00.16540.0499-0.700021.45383Hg (ppb)425.0495343.8310311.9680121.50611086.60197613.9312.432294.20191.407210.93581 Table 5 - Anomalies in the Savinja River drainage basin. Sample No.Location, River (lake)Element with positive anomalyextremeoutlier1Zg. Rakitovec, Slivniko Lake2Gorica, VoglajnaMn3Vrbno, VoglajnaP, Sn4Teharje-tore, VoglajnaMo, SbP, Cr, Cu, Re, Pb, Bi, W5Tremerje, SavinjaZn, AuAg6Letu, Savinja47Hrastje, Dobrinjski PotokThLi, Mn, Ga 48Lipovec, Lo nicaV, Mn, Th, Yb49Celje, VoglajnaB, Na, Co, Zn, Se, Zr, Cd, In, Pb, TlCu, Hg50Celje, Savinja79Celje, HudinjaBCo, Cu, Se, Cd, Sb, Ba, Tl, W80Spodnja Hudinja, HudinjaBa81`kofja Vas, Hudinja82Vianja Vas, Hudinja83Debro, Savinja84Rimske Toplice, Savinja DISCUSSION Mutual correlation of elements can give a possibility to distinguish geogenic from anthropogenically introduced elements. Correlation matrix n x n (n=53) shows mutual relationship among the elements. Due to the limited number of sampling locations, relationship is a tentative one. From 6 major elements, significant correlations (r>0.80) show: Ca with Mg (0.81) and Sr (0.84); Fe with B (0.89), V (0.81), Y (0.95), Sm (0.82), Eu (0.81), Tb (0.92) and Yb (0.89); Al with Li (0.93), K (0.91), Rb (0.91) and Cs (0.81); Mg with Ca (0.81); K with Li (0.81), Al (0.91) and Rb (0.96); and S with Sr (0.86). It can be concluded that Ca, Fe, Al, Mg, K and S belong to geogenic elements, which are little affected by anthropogenic activities. Because there was neither found iron anomaly, nor correlation of Fe with Co, Cr, Mn and Ni, it can be concluded that, anthropogenic association due to iron metallurgy in the past, was not recorded in recent sediments. The result is showing an improvement of the environment in comparison with historical levels [4]. P, Na and Ti belong to minor elements and show the following significant correlations with anthropogenically introduced elements: P with Sn (0.81); Na with B (0.90), Cu (0.81), Se (0.86), Cd (0.92), In (0.90), Tl (0.88) and Pb (0.92); and Ti with Nb (0.81). The Ti Nb association is in accord with findings of ajn [4]. It is the result of titanium-oxide production, which is still in progress. It was found in the present work that Zn shows the highest correlation with Ag (0.80) and Cd (0.78). These elements found in sediments still reflect metallurgic activity in Celje region, although the concentrations are lower than that in the first report by tern and Frstner [1]. Geochemical data can be also used for assessment of contamination of sediments with toxic elements. Existing criteria for sediment quality, issued by the University of Waterloo [19], Canada, will be used. Significant toxic effects are possible only on two locations in the town of Celje. In location 49, significant toxic effects are possible with As, Cd, Cu, Pb, Hg, Ni, Ag and Zn. In location 79, toxic effects are possible with Cu, Ni, Ag and Zn. Results regarding Zn and Cd are in support to }ibret [3]. Mssbauer spectroscopy at room temperature can be used with certainty only to calculate Fe(III)/Fe(II) ratio. Fe minerals, in which Fe(III) and Fe(II) ions are incorporated, are difficult to determine. The highest concentration of Fe(III) is in sample 48, Lo nica stream. It is assumed that Fe(III) is retained in the silicate sites or in finely dispersed iron oxide [20]. The lowest ratio, observed in location 6, can be explained with Fe(II) situated in calcite and/or dolomite. High Fe(II) content was observed in sediments, also containing calcite and dolomite as important constituents, of Hudinja and Savinja below Celje. CONCLUSIONS The described mineralogical, geochemical, statistical and Mssbauer spectroscopy investigations of stream sediments of Savinja, Hudinja and Voglajna Rivers led to the following conclusions: Mineralogical analysis has shown the presence of numerous minerals. The most abundant are quartz, calcite, dolomite, feldspar and muscovite, depending on location. Chlorites and clay minerals (<5%) are trace minerals, which are probable, but not proved, due to the limitation of XRD method. Mssbauer spectroscopy at room temperature could not distinguish iron minerals. Only Fe(III) and Fe(II) can be determined using hyperfine parameters. Q-modality cluster analysis of geochemical data was used to disaggregate the total data set into more ho-mogenous subsets. For the largest cluster, without significant anomalies, it was possible to calculate baseline values for 53 elements in the studied region. Chemical anomalies have been determined. Comparison of concentrations of toxic elements with existing criteria for sediment quality, revealed that Celje region is still contaminated. The most significant contaminants are Zn and Cd. In two locations within the town, serious toxic effects are possible due to several elements. In other locations, only minor toxic effects are possible. ACKNOWLEDGEMENTS This research was funded by the Ministry of Science Education and Sport of the Republic of Croatia, project 0098041 (principal investigator H. Bilinski). Measurements of XRD were funded by project number 0119412. Additional support for sampling in Slovenia was obtained from the bilateral project Croatia-Slovenia (principal investigators H. Bilinski and D. Han~el). REFERENCES [1] `tern, J. and Frstner, U. (1976). Heavy metals distribution in the sediment of the Sava Basin in Slovenia. Geologija 19, 259-274. [2] Fran iakovi-Bilinski, S., Bilinski, H., Tibljaa, D., Han~el, D. and Mertelj, A. (2002). Characterization of sediments from Voglajna and Savinja rivers  preliminary results. Geologija 45(2), 367-372. [3] }ibret, G. (2002). Mass balance of heavy metals in Celje area. Geologija 45(2), 613-618. [4] `ajn, R. (2005). Using attic dust and soil for the separation of anthropogenic and geogenic elemental distributions in an old matallurgic area (Celje, Slovenia). Geochemistry: Exploration, Environment, Analysis 5, 59-67. [5] Pirc, S. (2001). Geology and geochemistry of mercury in Slovenia. RMZ-Materials and Geoenvironment 48, 37-48. [6] Nosan, T. (1963). The geology of the Voglajna River Region and of the Upper Sotla River Region. Geografski Zbornik 8, 67-75. [7] Hamrla, M. (1954). Geological relations along the northern border of the Lako Syncline east the Savinja River. Geologija 2, 118-144. [8] Buser, S. (1977). Basic geological map of SFRJ, sheet Celje 1:100000. Federal Geological Survey, Beograd (In Slovene with English abstract. [9] Pirc, S. (1993). 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STATISTICA (data analysis software system), version 6. www.statsoft.com. [16] Davis, J.C. (1986). Statistic and data analysis in geology. Wiley & Sons, New York. [17] Klein, C. and Hurlbut, C.S.jr., after Dana, J.D. (1985). Manual of mineralogy, 20th Edition. John Wiley & Sons, New York. [18] Klockmanns Lehrbuch der Mineralogie (1978). 16. Auflage, Paul Ramdahr und Hugo Strunz. Ferdinand Enke Verlag Stuttgart, Germany. [19] URL1:  HYPERLINK "http://wvlc.uwaterloo.ca/biology/447/modules/module1/sedaquat1.html" http://wvlc.uwaterloo.ca/biology/447/modules/module1/sedaquat1.html [20] Schwertmann, U. and Cornell, R.M. (1991). In: Iron Oxides in the Laboratory (VCH Ed.), Weinheim, Germany, 14-18. Received: December 21, 2005 Accepted: January 24, 2005 Corresponding author Stanislav Fran iakovi-Bilinski Institute  Ruer Boakovi POB 180 10002 Zagreb Croatia e-mail: francis@irb.hr FEB/ Vol 15/ No 3/ 2006  pages  EMBED CorelDRAW.Graphic.9  by PSP Volume 15  No 3. 2006 Fresenius Environmental Bulletin  PAGE 2 4600' N 48 1 47 2 3 5 6 83 84 49 50 81 83 82 84 bd&*JLjl  /0pqv ! 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