ISSN 1408-7073 RMZ - MATERIALS AND GEOENVIRONMENT PERIODICAL FOR MINING, METALLURGY AND GEOLOGY RMZ - MATERIALI IN GEOOKOLJE REVIJA ZA RUDARSTVO, METALURGIJO IN GEOLOGIJO RMZ-M&G, Vol. 58, No. 2 pp. 101-240 (2011) Ljubljana, June 2011 Historical Rewiev More than 80 years have passed since in 1919 the University Ljubljana in Slovenia was founded. Technical fields were joint in the School of Engineering that included the Geologic and Mining Division while the Metallurgy Division was established in 1939 only. Today the Departments of Geology, Mining and Geotechnology, Materials and Metallurgy are part of the Faculty of Natural Sciences and Engineering, University of Ljubljana. Before War II the members of the Mining Section together with the Association of Yugoslav Mining and Metallurgy Engineers began to publish the summaries of their research and studies in their technical periodical Rudarski zbornik (Mining Proceedings). Three volumes of Rudarski zbornik (1937, 1938 and 1939) were published. The War interrupted the publication and not untill 1952 the first number of the new journal Rudarsko-metalurski zbornik - RMZ (Mining and Metallurgy Quarterly) has been published by the Division of Mining and Metallurgy, University of Ljubljana. Later the journal has been regularly published quarterly by the Departments of Geology, Mining and Geotechnology, Materials and Metallurgy, and the Institute for Mining, Geotechnology and Environment. On the meeting of the Advisory and the Editorial Board on May 22nd 1998 Rudarsko-metalurski zbornik has been renamed into "RMZ - Materials and Geoenvironment (RMZ -Materiali in Geookolje)" or shortly RMZ - M&G. RMZ - M&G is managed by an international advisory and editorial board and is exchanged with other world-known periodicals. All the papers are reviewed by the corresponding professionals and experts. RMZ - M&G is the only scientific and professional periodical in Slovenia, which is published in the same form nearly 50 years. It incorporates the scientific and professional topics in geology, mining, and geotechnology, in materials and in metallurgy. The wide range of topics inside the geosciences are wellcome to be published in the RMZ -Materials and Geoenvironment. Research results in geology, hydrogeology, mining, geotechnology, materials, metallurgy, natural and antropogenic pollution of environment, biogeochemistry are proposed fields of work which the journal will handle. RMZ -M&G is co-issued and co-financed by the Faculty of Natural Sciences and Engineering Ljubljana, and the Institute for Mining, Geotechnology and Environment Ljubljana. In addition it is financially supported also by the Ministry of Higher Education, Science and Technology of Republic of Slovenia. Editor in chief Table of Contents - Kazalo Original Scientific Papers - Izvirni znanstveni članki Microstructural stability of gray iron thin section castings for enameling 101 Mikrostrukturna stabilnost sive litine z lamelnim grafitom v tankih stenah za emajliranje Zeljko, S., Glavaš, Z., Terzič, K., Unkič, F. The effect of cooling rates on microstructures and hot workability of BRCMO2 tool steel Vpliv ohlajevalnih hitrosti na mikrostrukturo in vročo preoblikovalnost orodnega jekla BRCMO2 Večko PiRTovŠEK, T., Fazarinc, M., Kugler, G., Mrvar, P., Terčelj, M. Effect of heat treatment and test temperature on fracture type of steel Nitronic 60 Vpliv toplotne obdelave in temperature preizkušanja na vrsto preloma jekla Nitronic 60 GiGOVIČ-GEKIČ, A., Oruč, M., Nagode, A., Avdušinovič, H. Bacterial indicators of faecal pollution and physiochemical assessment of tributaries of Ganges River in Garhwal Himalayas, India Bakterijski indikatorji fekalnega onesnaženja in fiziološko-kemijska ocena pritokov reke Ganges v Garhwalski Himalaji v Indiji Sati, A., Sood, A., Sharma, S., Bisht, S., Kumar, V. Integrated geophysical and geotechnical investigation of the failed portion of a road in basement complex Terrain, Southwest Nigeria Povezane geofizikalne in geotehnične preiskave poškodovanega dela ceste na ozemlju metamorfne podlage v Jugozahodni Nigeriji Osinowo, O. O., Akanji, O. A., Akinmosin A. Sequence stratigraphic framework of K-field in part of Western Niger delta, Nigeria Sekvenčna stratigrafija naftnega polja K v zahodnem delu delte reke Niger, Nigerija Nton, M. E., Ogungbemi, T. S. Environmental impacts of asphalt and cement composites with addition of EAF dust Okoljski vplivi asfaltnih in cementnih kompozitov z dodatkom EOP-prahu Oblak, T., Ščančar, J., Vahčič, M., Zuliani, T., Mladenovič, A., Milačič, R. 113 121 129 143 163 Adsorption capacity of the Velenje lignite: methodology and equipment 193 Adsorptivnost velenjskega lignita: metodologija in oprema Žula, J., Pezdič, J., Zavšek, S., Burič, E. Short Papers - Strokovni članki Strokovni posvet Podnebni ekstremi in varna oskrba s pitno vodo 217 Čenčur Curk, B. In Memoriam In Memoriam Prof. dr. inž. Ciril Pelhan 219 In Memoriam Prof. dr. Bogdan Sicherl 222 Authors Index, Vol. 58, No. 2 225 Instructions to Authors 227 Template 235 Microstructural stability of gray iron thin section castings for enameling Mikrostrukturna stabilnost sive litine z lamelnim grafitom v tankih stenah za emajliranje Snježana Zeljko1, Zoran Glavaš2, *, Katarina Terzic2, Faruk Unkic2 1Plamen International, d. o. o., Njemačka ulica 36, p. p. 209, 34000, Pozega, Croatia ^University of Zagreb, Faculty of Metallurgy, Aleja narodnih heroja 3, 44103 Sisak, Croatia Corresponding author. E-mail: glavaszo@simet.hr Received: March 13, 2011 Accepted: May 17, 2011 Abstract: The influences of chromium on the stabilization of pearlite in the microstructure of gray iron thin section castings and distortion of castings during enameling were analyzed in this paper. Chromium content varied from the mass fractions 0.08 % to 0.37 %. It is found that the distortion of castings with or without the addition of chromium in the as-cast condition was in the acceptable range. The microstructure of castings in as-cast condition was consisted of pearlitic metal matrix and graphite flakes dispersed throughout. The results showed that the distortion of castings containing the mass fractions 0.08 % and 0.17 % of chromium was outside the acceptable range after enameling, due to decomposition of pearlite and transformation to austenite during enameling. After enameling, distortion of castings containing 0.37 % chromium was acceptable. Decomposition of pearlite was considerably lower than in castings containing 0.08 % and 0.17 % chromium. The obtained results confirmed the beneficial effect of chromium on the stabilization of iron carbide and prevention of decomposition of pearlite at elevated temperatures. Izvleček: V delu je narejena analiza vpliva kroma na stabilnost perlita v mikrostrukturi sive litine z lamelnim grafitom v tankih stenah ter deformacije ulitkov med procesom emajliranja. Masni delež kroma se spreminja med 0,08 % in 0,37 %. Ugotovljeno je bilo, da je deformacija ulitkov z dodatka kroma ali brez njega v litem stanju v zadovoljivih mejah. Mikrostruktura ulitkov v litem stanju sestoji iz perlitne matrice in grafitnih lamel v njej. Rezultati analiz kažejo, da je deformacija ulitkov, ki vsebujejo med 0,08 % in 0,17 % kroma, zunaj dovoljenega območja po izvedenem emajliranju. Vzrok za to je razpad perlita in transformacija avstenita med emajliranjem. Po izvedenem emajliranju je za ulitke, ki vsebujejo masni delež Cr 0,37 %, ugotovljeno, da je deformacija v sprejemljivih mejah. Razpad perlita je značilno manjši v tem primeru kot v litinah, ki imajo masni delež Cr 0,08 in 0,17 %. Dobljeni rezultati potrjujejo ugoden učinek kroma na stabilizacijo železovih karbidov in preprečujejo razpad perlita pri delovnih temperaturah. Key words: gray iron, microstructure, enameling Ključne besede: siva litina z lamelnim grafitom, mikrostruktura, emajliranje Introduction Gray iron refers to a broad class of ferrous casting alloys normally characterized by a microstructure of flake graphite in a ferrous metal matrix which is usually a fully pearlitic.[1, 2] They are relatively inexpensive and easy to produce. They have high thermal conductivity and damping capacity, low modulus of elasticity and an ability to withstand thermal shock.[3] This make them suitable for castings subjected to local or repeated thermal stressing, such as components of ovens and stoves.[3] The components of ovens and stoves are in many cases enameled in order to improve corrosion resistance, thermal stability, appearance and many other features.[4] Enamels are inorganic vitreous coatings applied to products or parts made of cast iron to improve ap- pearance and to protect the metal surface. They may be applied to the surface of components by either the wet process or the dry process. After that, they are fused to the casting surface at temperatures 780-800 °C during the firing process.[4] During enameling, distortion of castings may occur due to high firing tem-peratures.[4] Distortion of castings results from low metal strength at the firing temperature, thermal stresses due to non-uniform heating and cooling, decomposition of pearlite and transformation to austenite.[4] Changes in design of the components and firing practice alleviate the first two causes, and properly alloying minimizes decomposition of pearlite and transformation to austenite. Moreover, dimensional stability of gray iron castings at elevated temperatures is affected by factors such as growth, scaling, and creep rate. [5-9] To prevent these processes, alloying elements must be added to stabilize pearlite.[5-10] The objective of this paper was to determine the influence of various additions of chromium on the stabilization of pearlite and distortion of castings during enameling. Materials and methods The gray iron melts were produced in two mains frequency coreless induction furnaces from a charges consisting of pig iron, steel scrap, gray iron returns, ferrophosphorus, silicon carbide and recarburizer. To obtain desired chromium content in the melts, granulated ferrochromium containing the mass fraction 65,0 % of chromium was added. During charging, heating and melting the induction furnaces followed the same power-time program as a means to keep the thermal history of the melts as controlled as possible in the "furnace" phase. Gray iron melts from induction furnaces were tapped and then poured at 14001420 °C into vertically-parted green sand molds produced in vertically parted molding machine. The dimensions of the molds were: 800 mm x 1000 mm x 250 mm. Pouring was performed by automatic pouring system (pressurized pouring furnace). Late (stream) inoculation was performed with 0.1 % of calcium/aluminum/strontium containing ferrosilicon. Poured castings were used as components of stoves. After shakeout and blasting, castings were inspected for defects and distor- Figure 1. Casting after shakeout and blasting. Distortion was measured along the marked lines (1 and 2). Samples for metallographic examinations were cut from areas marked with the letters "A" and "B" tion. Distortion, i.e. concavity of castings was measured along the ribs 1 and 2 according to figure 1. Maximum acceptable distortion was 1.0 mm. Enamel was applied to both sides of the castings by wet process (spraying). Fusing of the enamel coating to the castings surface was done in a continuous furnace. Coated castings were fired at 780 °C. Firing time was 10 min. After enameling, distortion of the enameled castings was measured on the previously described manner. The maximum allowable distortion of the castings after enameling was 1.0 mm. a light metallographic microscope with a digital camera and the image analysis system. Samples were cut from two places as shown in Figure 1: between openings ("A" sample) and from the rib ("B" sample), due to different section thickness (4.0 mm and 6.0 mm). Kinetics of phase transformations in the castings containing 0.08 % and 0.37 % chromium was analyzed by differential scanning calorimetry. The conditions were the same as in the enameling process. Samples were heated at 780 °C and then held at that temperature for 10 min. Heating rate was 40 K/min. The cooling rate after holding at 780 °C was 30 K/min. Hardness of the castings before and after enameling was measured by Brinell Results and discussion tester. Metallographic examinations of the castings in as-cast condition and The chemical compositions of exam- enameled castings were performed by ined gray iron heats are given in table 1. Table 1. Chemical composition of examined gray iron heats in mass fractions, w/% Gray iron Chemical composition, w/% heat C Si Mn P S Cr Cu CE 1 3.55 2.44 0.43 0.370 0.064 0.08 0.09 4.49 2 3.56 2.54 0.44 0.360 0.066 0.17 0.10 4.53 3 3.55 2.47 0.42 0.370 0.071 0.37 0.09 4.50 Table 2. Distortion of castings before and after the enameling Distortion of castings. mm Gray iron heat The number of Along the rib 1 (see figure 1) Along the rib 2 (see figure 1) castings Before enameling After enameling Before enameling After enameling 1 20 0.15-0.25 1.70-1.90 0-0.20 1.85-1.95 2 50 0.20-0.25 1.20-1.30 0.25 1.20-1.30 3 40 0.10-0.20 0.35-0.50 0.35-0.50 0.30-0.50 With a carbon content in the gray iron melts in the range from 3.55 % to 3.56 %, silicon content in the range from 2.44 % to 2.54 % and a phosphorus content in the range from 0.36 % to 0.37 % carbon equivalents in the range from 4,49 to 4,53 were achieved. This corresponds to slightly hypereutectic compositions. Total carbon and silicon contents were in the target range. If both are low, the iron tends to be brittle and to blister during enameling. If both are high, the iron is soft and warps easily when reheated for enameling. Phosphorus was added intentionally to increase the fluidity of the gray iron melts. Within this range (0.36 % to 0.37 %), phosphorus has a negligible effect on the strength of the gray iron castings at enameling firing temperatures. However, these contents of phosphorus may result in the formation of phosphide eutectic (steadite). The sulfur content was balanced with manganese to promote the formation of manganese sulfides. They were distributed through the structure and acted as nuclei for eutectic graphite. Chromium was added intentionally in gray iron melts number 2 and 3 to stabilize pearlite in the microstructure of castings. Copper promotes pearlite formation, but its content was low in all melts. The results of measuring distortion (concavity) of castings before and after enameling are given in table 2. It can be observed from table 2 that in all cases distortion of castings before enameling was in the acceptable range. After enameling distortion of casting containing 0.08 % and 0.17 % chromium was exceeded the maximum allowed value, while the distortion of castings containing 0.37 % chromium was acceptable. The results of metallographic examinations show that the chromium has pronounced effects on microstructural stability of gray iron castings at firing temperatures (Figures 2 to 4). It can be observed from figures 2 to 4 that all castings in as-cast condition were fully pearlitic. Types B, C and D graphite flakes were found in thinner "A" samples. In thicker "B" samples, types B and C graphite flakes were present. A large volume fraction of coarse type C graphite flakes was obtained due to hypereutectic compositions. This type of graphite flakes is desirable in applications requiring a high degree heat transfer and high resistance to thermal shock, such as components of stoves. Types B and D graphite flakes are undercooled forms which form when solidification occurs at a large undercooling. Undercooling was occurred due to inadequate nucleation of graphite for a given high cooling rates. The increase of the undercooling during the solidification results in increasing of volume fraction of type D flake Figure 2. Optical micrographs of the microstructure of gray iron casting containing 0.08 % chromium: a) "A" sample before enameling (as-cast condition), b) "B" sample before enameling (as-cast condition), c) "A" sample after enameling, d) "B" sample after enameling graphite. High phosphorus contents were resulted in the formation of another microstructural constituent, stea-dite. Due to the high cooling rates and chromium addition, a small amount of carbides was also found (especially in the microstructure of castings containing 0.37 % chromium). The results of examinations show that enameling was altered the metal ma- trix, but no effect on size and shape of graphite achieved during solidification (figures 2 to 4). The pearlite content in the metal matrix decreases after enameling. However, decomposition of the pearlite to ferrite and graphite and transformation to austenite in microstructure of castings containing 0.37 % chromium was considerably lower than in castings containing 0.08 % and 0.17 % chromium. Due to Figure 3. Optical micrographs of the microstructure of gray iron casting containing 0.17 % chromium: a) "A" sample before enameling (as-cast condition), b) "B" sample before enameling (as-cast condition), c) "A" sample after enameling, d) "B" sample after enameling that, distortion of castings containing 0.37 % after enameling was acceptable. It is obviously that chromium stabilizes iron carbide and therefore prevents the breakdown of pearlite at the firing temperature. This improves the dimensional stability of gray iron castings during enameling. Although the size and type of the graphite flakes was unaffected by fir- ing process, the size and type had a marked influence on the carbon kinetics during firing process. In castings with a high volume fraction of fine type D graphite flakes, the carbon diffusion paths were shorter, which facilitates the decomposition of pearlite. If pearlite was not stabilized, shorter carbon diffusion paths resulted in higher ferrite volume fraction in the metal matrix after enameling. Figure 4. Optical micrographs of the microstructure of gray iron casting containing 0.37 % chromium: a) "A" sample before enameling (as-cast condition), b) "B" sample before enameling (as-cast condition), c) "A" sample after enameling, d) "B" sample after enameling DSC analysis (figure 5) confirmed the results of metallographic examinations. Heating curve of the sample containing 0.08 % chromium shows that a significant decomposition of pearlite occurred already at =350 °C. Decomposition of pearlite progressed very intensively with a further increase in temperature. The maximum was reached at =620 °C. Decomposition of the pearlite to ferrite and graphite occurred due to instability at elevated temperatures. Growth, residual stresses and dimensional instability of the casting are the results of the breakdown of the pearlite and transformation to austenite, which occurred at =742 °C. Heating curve of the sample containing 0.37 % chromium shows that the decomposition of pearlite to ferrite and graphite and transformation to austen- ite was considerably lower than in sample containing 0.08 % chromium. Very small decomposition of pearlite occurred up to 550 °C. Small increase in pearlite decomposition occurred in the range 550-650 °C. This confirms beneficial effect of chromium on the stabilization of iron carbide and the prevention of breakdown of pearlite during enameling. Because of that growth and residual stresses are reduced and the dimensional stability is increased. The obtained results show that the hardness of all castings decreases after enameling, due to the decomposition of pearlite (table 3). However, castings containing 0.37 % chromium had lower decrease in hardness after enameling than castings containing 0.08 % and 0.17 % chromium, due to much more stable pearlite. The hardness of all castings in as-cast condition and after enameling did not exceed the maximum allowable 230 HB. Figure 5. Simultaneous thermal analysis of gray iron samples containing 0.08 % and 0.37 % chromium by DSC method Table 3. Hardness of castings before and after enameling Gray iron heat Hardness of castings, HB Between openings ("A" sample, see figure 1) On the rib ("B" sample, see figure 1) Before enameling After enameling Before enameling After enameling 1 206 144 214 149 2 216 163 217 166 3 217 183 229 186 Conclusions The obtained results indicated that the chemical composition has a significant effect on the microstructure of gray iron castings after enameling. During enameling, due to high firing temperatures, decomposition of pearlite and transformation to austenite occurs if pearlite is not stabilized. Phase transformations may result in distortion and dimensional changes of castings. To prevent these processes, alloying elements must be added to stabilize pearl-ite. The results of this examinations show that the chromium, when added in proper amount, stabilizes the iron carbide and therefore prevents the breakdown of pearlite during enameling process. Chromium is very effective in stabilization of pearlite, but the use of higher chromium content is limited. It is a strong chill and carbide former, and therefore, high chromium additions can be detrimental to machina-bility. It is obvious that the chromium content in gray iron casting for enamelling is an important process parameter and must be adapted depending on the required metal matrix structure and section thickness of castings. Highly branched Type D graphite flakes reduce carbon diffusion distances, which facilitates the decomposition of pearlite. High cooling rates (thin sections) and low nucleation state of melt favors the formation of Type D graphite flakes and carbides. Due to that, melts must be prepared with suitable charge materials (such as pig iron) and properly inoculated. References [1] Craig, d. b., Hornung, m. j., Mc- cluhan, t. k. (1988): Gray Iron, chapter in the book: Metals Handbook, Vol. 15, Casting. ASM International, Metals Park, Ohio, 1988, pp. 629. [2] Asm International (1999): Metallur- gy and Properties of Gray Irons, chapter in the book: Cast Irons, ASM Specialty Handbook. ASM International, Materials Park, Ohio, pp. 32. [3] Elliott, R. (l988): Cast Iron Technol- ogy, Butterworths & Co., London, pp. 11. [4] Technical Publications Committee Of The Porcelain Enamel Institute (1998): Porcelain Enameling, chapter in the book: ASM Handbook, Vol. 5, Surface Engineering. ASM International, Materials Park, Ohio, pp. 1343. [5] Asm International (1999): Elevated- Temperature Properties, chapter in the book: Cast Irons, ASM Specialty Handbook. ASM International, Materials Park, Ohio, pp. 409. [6] Asm International (1997): Alloy Cast Irons, chapter in the book: Heat-Resistant Materials, ASM Special- ty Handbook. ASM International, Materials Park, Ohio, pp. 179. [7] Asm International (1999): Metallurgy and Properties of High-Alloy Graphitic Irons, chapter in the book: Cast Irons, ASM Specialty Handbook. ASM International, Materials Park, Ohio, pp. 123. [8] Novosel, m. (1988): Procesi zarenja sivog lijeva. I. dio. Livarstvo; Vol. 3, No. 2, pp. 35-44. [9] Novosel, m. (1988): Procesi žarenja sivog lijeva. II. dio. Livarstvo; Vol. 3, No. 3, pp. 67-72. [10] Afs Cast Iron div. (2000): Stabilizing Pearlite in Gray Cast Iron. Modern Casting; Vol. 90, No. 11, pp. 40-43. The effect of cooling rates on microstructures and hot workability of BRCMO2 tool steel Vpliv ohlajevalnih hitrosti na mikrostrukturo in vročo preoblikovalnost orodnega jekla BRCMO2 T. Večko PiRTovšEK1, M. Fazarinc1, G. Kugler1, P. Mrvar1, M. Terčelj1, * faculty for Natural Sciences and Engineering, University of Ljubljana, Aškerčeva 12, 1000 Ljubljana, Slovenia Corresponding author: milan.tercelj@omm.ntf.uni-lj.si Received: May 12, 2011 Accepted: June 27, 2011 Abstract: The influence of solidification and cooling rate on obtained microstructure is especially emphasized in BRCMO2 tool steel. Various cooling rates during solidification process result in considerably different size of grains as well as in different type, size, shape and distribution of carbides. Cast ingot is solidified with different cooling rates across its section leading to different hot workability. Consequently dimensions of ingot are very important since they determine the lowest acceptable cooling rate of the tool steel. Time course of temperature field during the solidification of ingot made from BRCMO2 tool steel has been simulated and obtained microstructures have been analyzed. Finite element analysis was used for estimation of cooling rates and calculation of fractions of solid/liquid at various locations of selected cross-sections of ingot during its cooling. The hot workability of BRCMO2 tool steel was studied using hot compression tests at different deformation conditions on Gleeble 1500D testing equipment. Izvleček: Vpliv hitrosti strjevanja in ohlajanja na mikrostrukturo je posebej poudarjen pri hitroreznem orodnem jeklu BRCMO2. Tako različne hitrosti ohlajanja med procesom strjevanja kritično vplivajo na različno velikost in razporeditev zrn, prav tako pa tudi na tip, velikost, obliko ter razporeditev karbidov. To se pogosto zgodi pri vlitju jekla v ingot, kjer so hitrosti strjevanja in ohlajanja različne v različnih delih ingota. To ima za posledico tudi različno preobliko- valnost v vročem. Tako so dimenzije ingota zelo pomemben parameter, saj določajo najpočasnejšo ohlajevalno hitrost v njem. V tem delu je bil analiziran potek temperature v različnih delih ingota med strjevanjem in ohlajanjem. Z metodo končnih elementov je bila ocenjena ohlajevalna hitrost ter razmerje med talino in trdnim stanjem. Z uporabo naprave Gleeble 1500D je bila preiskana vroča preoblikovalnost na podlagi tlačnih preizkusov. Keywords: BRCMO2 tool steels, hot workability, cast microstructure, carbide distribution, effect of cooling rates Ključne besede: orodno jeklo BRCMO2, vroča preoblikovalnost, lita mikrostruktura, razporeditev karbidov, vpliv ohlajevalnih hitrosti Introduction The dissolution of alloying elements and precipitation of carbides in lede-buritic tool steels result in a high strength and hardness, small deformation during the heat treatment, a very good wear resistance, and poor hot plasticity. Thus, tool steels usually exhibit a decreased but sufficient hot deformability only in a relatively narrow hot-working range, and as such belong to the group of low-de-formable steels.[1-4] During hot working of ledeburitic tool steels a large number of mutually dependent process parameters influence the intrinsic material properties that make an investigation in this area very specific. Solidification rate can essentially influence the obtained microstructure. During solidification, heating, soaking and hot deformation, various processes take place in the tool material: the formation of carbides, their decomposition, dissolution, growth, etc. Consequently the size, distribution, type and fraction of carbides, the thermo-mechanical history, the temperature range, etc., have a major influence on the hot workability of ledeburitic tool steels. As a result, hot workability cannot be considered as a constant, but rather as a variable property.[4-8] BRCMO2 tool steel has excellent hot hardness and wear resistance and is commonly employed to machine hard materials in high speed cutting applications as well as for cold-working dies. But on other hand the tool steel exhibits very poor hot deformability in industrial practice thus improvement in its production is desired. In this contribution time course of temperature in various cross-sections of ingot during solidification of BRCMO2 ledeburitic tool steel have been calculated by FEA. Additionally, microstructures at various cooling rates were determined and their influence on hot workability has been investigated. Materials and methods Materials BRCMO2 is a molybdenum type tool steel. The chemical composition is given in Table 1. The samples for metallographic analysis were cut from various spots on three various cross section of ingot, i.e. ingot head, ingot bottom, ingot half height, and on various distances from ingot surface, i.e. ingot surface, 10 mm, 50 mm, 90 mm from the surface, and in ingot center. Optical microscopy (OM, Carl Zeiss AXIO Imager.A1m) was applied for the observation of the microstructure and measurements of the size of eutec-tic cells where intercept method was applied. The specimens for the optical microscopy were grinded with a sequence of sand papers from 180 to 1200 meshes of granulation, followed by polishing with diamond paste of 1 |im and 0.25 |im granulation and then etched with Nital. Simulation of cooling rates in ingot using ProCast software The measured temperature of the melt in the ladle was 1490 °C. It was considered that this temperature was also temperature of the melt in the filled ingot. The simulation of filling and solidification of ingots was calculated using finite element casting simulation program, ProCast. Fluid flow was calculated according to Navier-Stokes equations and solidification properties were based on heat flow according to Fourier's equation.[9] Whole geometry of molds and other parts needed during ingot solidification were modeled in 3D geometry and meshed in ProCast by tetrahedral elements. Thermodynamic properties of die material, fireclay, exothermic and insulation materials were taken from the ProCast database. Properties of pouring material were calculated using CompuTherm software on the basis of chemical composition. For better results of solidification and cooling the stress module was activated in the software to account for the effect of gap formation on metal/die interface on cooling of ingot.[9] Initial heat transfer coefficient (HTC) h between solidified ingot and mold was considered to Table 1. Chemical composition of applied BRCMO2 in mass fractions, wt/% C Si Mn Cr Mo V W Co 1.09 0.26 0.25 3.81 9.32 1.09 1.40 8.20 be around 2000 W/(K m2). In general HTC is decreasing with gap formation during solidification and contraction. When the metal is liquid, HTC between the metal and die is a function of ferro-static pressure given by the equation: where h0 is initial heat transfer coefficient, P is pressure and A is empirical constant to account for contact pres- sure.[8] Cooling rates were calculated on the basis of the difference between time and temperature from the start of casting to complete solidification. Hot compression tests Hot compression tests were applied for assessment of hot deformability as well as for determination of flow curves. For assessment of hot deformability the procedure described in [1] was used. For determination of flow curves samples were taken so from the surface part as well as form centre of ingot's head. The following testing conditions were selected: temperature range 8501130 °C, strain rates between 0.001 s-1 and 5 s-1 and a true strain of 0.9. The specimens were heated to 1130 °C with a heating rate of 3 °C/s which was followed by holding them for 10 min at this temperature, and cooling with a rate of 2 °C/s to the deformation temperature, holding for 10 min, followed by hot compression and water quenching afterwards. Tantalum foil with a thickness of 0.1 mm was inserted between the cylindrical specimen and the compression anvil, and a Ni-based lubricant was used. For the higher strain rates the obtained flow curves were temperature compensated according to the procedure described in [7]. Results and discussion FEM calculated results on ingot cooling and obtained microstructures The simulated distribution (Figure 1) of solid fraction (left) and of temperature (right) during solidification of ingot at various times after begin of filling; i.e. 570 s (a), 950 s (b), and 1470 s (c) after casting start. It can be noticed that solidification starts on the bottom of ingot already during its filling. The solidification front is then moving from ingot surface towards the center and up to the head of ingot where solidification ends. On Figure 2 calculated time courses of temperature on spots with various distances from ingot surface are presented. It is clearly seen that due to rapid fall of temperature spots closer to ingot surface undergo considerably higher cooling rates. Furthermore, it is also clear that that fall of temperature is considerably higher on ingot bottom in comparison to ingot head. Calculated values of cooling rates in ingot head cross-section are given in Table 2. Calculated cooling rates on ingot surface are higher than 10 °C/s while in the ingot center these values are higher than 0.18 °C/s. Ledeburitic steels solidifie through the eutectic transformation is the last transformation of liquid to solid in the solidification process. Therefore, the nucleation and growth of eutectic (eutectic carbides + austenite) occurs in the remaining liquid area between primary dendrites. As-cast microstructure of ledeburitic tool steel consists of dendrites surrounded by an almost continuous inter-dendritic network of eutectic carbides and the size of eu-tectic cells is directly dependent on solidification rate. Consequently average size of eutectic cells on ingot surface was relative small and amount ca 21 pm while in ingot center these values are around 121 pm. From point of view of deformability obtained values for size of eutectic cells in ingot center indicates on approaching of upper limit of their size. Figure 3 a shows micro- structure obtained in the center of ingot's head which underwent slowest cooling rates. In the soft annealed condition the solidified microstructure of BRCMO2 steel consist colonies of eu-tectic carbides and blocky carbides inserted in the basic microstructure from ferrite and spheroidised carbides. In the vicinity of the ingot surface, where the solidification rate was the highest, eutectic cells are smallest and eutectic carbides are impossible to distinguish from the base microstructure detect using OM (see Figure 3b). With the increasing distance from the ingot surface, the eutectic colonies and eutectic carbides became incomparably coarser and also the size and the number of blocky carbides increase. Thus the size of the eutectic cells increase from few micrometers under the ingot surface up to about 86 pm at the 50 mm distance from the ingot surface (see Figure 3 c) and in ingot center are around 121 pm where also some micro-porosity was observed. Through the whole cross-section of the ingot the eutectic carbides have lamellar morphology typical for M2C type of eutectic. Table 2: Calculated cooling rates and the size of eutectic cells on ingot head cross-section at various distances from ingot surface. Distance /mm Assessed cooling rates The average size of eutectic cells /pm Up to 1.7 >10 °C/s 21 10 >0.8 °C/s 36 50 >0.23 °C/s 86 center >0.18 °C/s 121 Figure 1. Simulated distribution of solid fraction (left) and of temperature (right) during solidification at: 570 s (a), 950 s (b) and 1470 s (c) after begin of filling. Figure 2. Simulated cooling curves on different depths from ingot surface: top of the ingot (ingot head) (a) and 20 cm from bottom (b). Figure 3. Obtained microstructure on ingot head cross-section: in center (a), on surface (b) and 50 mm from ingot surface. Hot workability Different microstructures obtained at different cooling rates result in different hot workability. This was investigated by hot-compression tests at max strain of 0.9, a strain rate of 5 s-1 and various deformation temperatures.[1] The as-cast microstructure (Figure 3b) taken from the region under the ingot surface when cooling at a rate >10 °C/s does not crack during the upsetting at 1130 °C, whereas the cast microstructure from the ingot core, formed at a cooling rate of 0.18 °C/s cracks under these deformation conditions. Eutectic cells are believed to be responsible for this behavior. On the other hand at values of strains around 0.6, that are also typical in practice, the cracks were not observed on compressed samples. These results indicate on upper limit of dimensions of ingot since these determine lowest acceptable cooling rate. In laboratory simulation of solidification at cooling rate of 0.167 °C/s new type of eutectic carbide appeared in microstructure that additionally reduced hot deformability. As mentioned, flow curves for various temperatures and strain rates were obtained. The comparison of the flow curves is presented in Figure 5. The data gathered from the specimens at the surface of the ingot exhibit higher flow stresses and shape of flow curves indicate on dynamic recrystallization. The samples taken from the center of the ingot reach about 100 MPa lower flow stresses. Samples from ingot center exhibited lower hot deform-ability since most of them exhibited surface cracking during hot compression at applied strain of 0.9. Figure 4. Flow curves measured at different temperatures at strain rate of 5 s-1. Ingot surface (a), center of ingot's head (b). Conclusions Calculation of time course of temperatures by FEM on various spots of various cross-sections of ingot during solidification of BRCMO2 tool steel has been carried out. Hot workability of cylindrical samples has been studied by hot compression tests. The following conclusions can be drawn from the presented study: • Maximal calculated cooling rate on surface area of ingot head amounts >10 °C/s while the lowest value in centre of ingot head amounts around 0.18 °C/s. • BRCMO2 tool steel is very sensitive on cooling rate since this influence on solidified microstructure. Higher cooling rate (>10 °C/s) results in considerable lower size of dendrites as well as eutectic cells in comparison to lowest calculated cooling rate in solidified ingot. • From point of view of hot deform-ability microstructure obtained at cooling rate of about 0.18 °C/s presents transition from acceptable to non-acceptable microstructure. • Hot deformability of samples taken from ingot surface does not considerable differ from samples taken from ingot center. • Applied dimensions of ingot for this tool steel present the upper limit since lower cooling rate would be obtained in ingot with larger dimensions. • Obtained values for flow curves of compressed samples from ingot surface are higher in comparison to values of samples taken from ingot center. References [1] Vecko Pirtovsek, t., Kugler, g., Godec, m., Tercelj, m. (2011): Materials Characterization; Vol. 62, No. 2, pp. 189-197. [2] Ghomashchi, m. r., Sellars, c. m. (1993): Metallurgical transactions A, Vol. 24A, pp. 2171-2180. [3] Fajfar, p., Bombac, d., Markoli, b. (2010): RMZ - Materials and Geoenvironment, Vol. 57, No. 2, pp.159-164. [4] Rodenburg, c., Kryzanowski, m., Beynon, j. h., Rainforth, w. m. (2004): Materials Science and Engineering A 386, pp. 420-427. [5] iMBERT, c., rYAN, n. d., McQueen, h. j. (1984): Metallurgical Transactions A 15A, pp. 18551864. [6] Milovic, r., Manojlovic, d., Andjelic, m., Drobnjak, d. (1992): Steel Research 63/2, pp. 78-84. [7] imbert, c. a. c. & McQueen, h. j. (2000): Materials Science and Technology, Vol. 16, pp. 532-538. [8] liu, j., Chang, h., wu, r., hsu, t. y., Ruan, x. (2000): Materials Charact. 45, pp. 175-186. [9] Kermanpur, a., Eskandari, m., Purmohamad, h., Soltani, m. a., Shateri, r. (2010): Materials and Design 31, pp. 1096-1104. Effect of heat treatment and test temperature on fracture type of steel Nitronic 60 Vpliv toplotne obdelave in temperature preizkušanja na vrsto preloma jekla Nitronic 60 Almaida Gigovic - Gekic1 *, Mirsada Oruč2, Aleš Nagode3, Hasan Avdušinovic1 University of Zenica, Faculty of Metallurgy and Materials Science, Zenica, Bosnia and Herzegovina ^Metallurgical Institute "Kemal Kapetanovic", Zenica, Bosnia and Herzegovina 3University of Ljubljana, Faculty of Natural Sciences and Engineering, Ljubljana, Slovenia Corresponding author. E-mail: almaida.gigovic@famm.unze.ba Received: March 17, 2011 Accepted: June 22, 2011 Abstract: Nitronic 60 is a commercial name for austenitic stainless steel. Requirements in terms of chemical composition and mechanical properties of steel Nitronic 60 meet the requirements for steel UNS S21800. This steel has an increased content of manganese and silicon, which contributes to its excellent resistance to abrasion and adhesive wear. In this paper the fracture surface of the specimen after tensile test were examined in order to detect changes in ductile properties and the type of fracture depending on the condition of material and test temperature. Analysis of the fracture surface was performed on the stereo, optical and scanning electron microscope. Izvleček: Nitronic 60 je komercialno ime za avstenitno nerjavno jeklo. Glede na kemijsko sestavo in mehanske lastnosti jeklo Nitronic 60 izpolnjuje zahteve za jeklo UNS S21800. To jeklo ima povečano vsebnost mangana in silicija, ki prispevata k odlični odpornosti proti abraziji in adheziji. V tem delu smo preiskali prelomne površine vzorcev po nateznem preizkusu in spremljali spremembe duktilnih lastnosti ter ugotavljali vrsto preloma v odvisnosti od stanja materiala in temperature preizkušanja. Za analizo prelomnih površin smo uporabili stereo-, optični in elektronski mikroskop. 122 Gigqvic - Gekic, A., Qruc, M., Nagode, A., Avdušinovic, H. Key words: Nitronic 60, brittle fracture, ductile fracture, fracture surface Ključne besede: Nitronic 60, krhek prelom, duktilni prelom, prelomna površina Introduction Because of the unstable and high nickel price on the world market there is a need for replacing expensive nickel with some other cheaper austenite stabilizing elements.11, 2] The solution of this problem is substitution a portion of nickel with manganese and nitrogen. In this way a new steel group was created, which according to the UNS (Unified Numbering System) system, referred to as the series 200. In this group of steel nitrogen content ranges from 0.08-0.6 %, manganese 4-19 % and nickel 0.5-18 %.[3, 4] Nitronic 60 is a commercial name for austenitic stainless steel, which according to their chemical composition belonging to series 200. Steel Nitronic 60 has excellent resistance to abrasion and adhesive wear due to an increased content of manganese and silicon. Compared to steel alloyed with nickel and cobalt, Nitronic 60 has the same or better properties and lower price. Also, it has good impact resistance at low temperatures. Steel Ni-tronic 60 is applied to work at elevated temperatures because of good creep resistance and high temperature corrosion resistance.[5] The ASTM standard for this group of steels prescribes mechanical properties in the annealed condition, hot or cold deformed. This paper presents and discuss the results of the analysis of fracture surface of the specimens after tensile test at room and elevated temperature for three corresponding chemical composition of test material in a rolled and annealed condition. Materials and methods Tests were conducted using three melts produced in a vacuum induction furnace (type- Heraeus) at the Metallurgy Institute „Kemal Kapetanovic" in Zenica. The results of chemical analysis of the experimental melts and comparative values prescribed by ASTM standards are given in Table 1. As seen from the Table 1 the chemical composition of test melts is in good agreement with chemical composition as prescribed in ASTM A276. This standard applies to steel S21800, which is taken as a reference for Nitronic 60. Mechanical and metallographic examinations were conducted on samples in a rolled and solution annealed state. To obtain the austenitic microstructures free of precipitates extracted samples were Table 1. The chemical composition of melts -Nitronic 60[5] in mass fractions, w/% Melt Chemical composition, w/% C Si Mn Cr Ni P S N ASTM A276 <0.10 3.5-4.5 7-9 16-18 8-9 <0.006 <0.03 0.08-0.18 V1694 0.04 3.74 8.6 18.0 8.0 0.007 0.005 0.160 V1696 0.05 3.5 7.9 16.9 8.6 0.005 0.005 0.120 V1697 0.05 3.5 7.2 16.9 8.6 0.005 0.010 0.168 Table 2. Test results of mechanical properties of steel Nitronic 60[5] Melt Test condition Test temperature Mechanical properties Rp0.2 Z(N/ mm2) Rm /(N/mm2) Z/% A/% V1694 rolled Room temperature 860 1026 50 18.1 V1696 681 874 68 35.6 V1697 779 937 61 27.9 V1694 annealed Rom temperature 400 750 75 51.8 V1696 331 681 76 57.2 V1697 366 716 68 55.7 V1694 annealed 750 0C 211 292 49 38.7 V1696 158 245 48 45.5 V1697 182 299 42 29.9 ic 60 is shown in Figure 1 with polygonal austenite grains with the characteristic twins. The basic parameters of the mechanical properties of tested samples are presented in table 2. Mechanical tests were conducted on a universal hydraulic machine for static testing (200 kN) at the Metallurgical Institute »Kemal Kapetanovic« in Zenica. The process of testing and preparing of test specimens for testing performed in accordance with the standards BAS EN 10002-1/02 and BAS EN 10002-5/01. Tensile testing of mechanical properties at room and elevated temperature (750 °C) was carried out on specimens obtained from the 0 15 mm rod. Figure 1. Microstructure of austenitic stainless steel Nitronic 60. (aqua regia, x 100)[5] annealed at a temperature of 1020 °C for 1 h and quenched in water. Microstructure of austenitic stainless steel Nitron- Test results from Table 2 for annealed samples tested at room temperature are in agreement with the standard ASTM A276. while the test results for annealed samples tested at elevated temperature are in accordance with the manufacturer demand. Examination of the fracture surface appearance was performed in three steps. • Analysis of fracture surfaces on specimens at the stereo microscope Leica with a maximum magnification of 60-times • 3D simulation of the fracture surface of specimen using Olympus optical microscope with appropriate software. Development of the simulation was based on a series of photographs taken on the optical microscope with magnification of 50-times • Analysis of the fracture surface using SEM Jeol JSM 5610 at different magnifications. Results and discussion Analysis of the tensile test results Analysis of the results of mechanical tests showed that the material in the rolled condition has the maximum value of tensile properties, while the increase in temperature leads to decreasing of the strength. Specimens tested in annealed condition at room temperature have the best ductile properties. These results are a consequence of the microstructure obtained for different tasted states. Annealing at temperatures above 1000 °C leads to dissolution of precipitates, mainly M23C6 type of carbides, which have a negative effect on the ductility properties.[6] However, heating austenite steel in the temperature range from 400-900 °C leads to their re-precipitation. Otherwise, the final rolling temperature was an average of 850 °C, which affected the amount of extracted precipitates, and thus the ductility and tensile properties of tested material. Fracture surfaces analysis Stereo microscope analysis Figures 2, 3 and 4 give the appearance of the fracture surfaces of tested specimens made from melts V1696, V1694 and V1697. From Figure 2 and 3 can be seen that the fracture surface of specimens tested at room temperature made of melts V1696 and V1694 have typical Cup-Cone ductile fracture with pronounced plastic deformation while this type of fracture is not present at the specimen made from melt V1697 tested at of 750 ° C v *■ ■ - ■ ■:« 1 ■ . •< , . m a) magnification 20-times b) magnification 12.5-times Figure 2. Fracture surface (melt V1696, rolled condition, room temperature) a) magnification 16-times b) magnification 16-times Figure 3. Fracture surface (melt V1694, annealed condition, room temperature) a) magnification 16-times b) magnification 12-times Figure 4. Fracture surface (melt V1697, annealed condition, tested at 750 °C) Optical microscope analysis Samples presented in the previous chapter were used for 3D analysis of fracture surface. The appearance of the obtained fracture surface is shown in Figures 5, 6 and 7. Analysis of 3D images of the fracture surface confirmed the assumption after observing the samples at a stereo microscope. At the figures 5 and 6 can be observed ductile type of fracture, while in Figure 7 the brittle fracture characteristics can be seen. Figure 5. 3D view of fractured surface (melt V1696, rolled condition, room temperature) Figure 6. 3D view of fractured surface (melt V1694. annealed condition, room temperature) Figure 7. 3D view of fractured surface (melt V1697, annealed condition, test temperature 750 °C) SEM analysis of the fracture surfaces SEM (scanning electron microscope) analysis was carried out for a detailed analysis of the type of fracture. SEM micrographs were used for confirmation the assumptions made after stereo and optical microscope analysis. The analysis was performed at the University of Ljubljana (Faculty of Natural Sciences and Engineering) at the scanning electron microscope JEOL at different magnifications. Analysis of fracture surfaces showed that the ductile fracture occurs during testing at room temperature in both cases, i.e. in rolled and annealed conditions of samples. Fracture surfaces of samples tested at 750 °C showed the presence of intergranular brittle fracture with small portion of ductile fracture. Appearance of fracture surfaces of specimens is shown in Figures 8, 9,10 and 11 which is consistent with the 3D fracture analysis. Figure 8. Fracture surface - SEM (melt V1696, rolled condition, room temperature) Figure 10. Fracture surface - SEM (melt V1697, annealed condition, tested at 750 °C) Figure 9. Fracture surface - SEM (melt V1694, annealed condition, room temperature) 20 k U XI T see Í S»m NTF Figure 11. Microstructure of the sample - SEM (melt V1697, annealed condition, tested at 750 °C) Conclusions On the basis of the research and analysis of the results it can be concluded that the tensile test specimens tested at room temperature in a rolled and annealed condition have ductile fracture, while during testing at 750 °C appears brittle intergranular fracture. Samples that were solution annealed have austenitic microstructure without extracted precipitates inside the grains and at grain boundaries what has a significant influence on the ductile properties and the type of fracture. Temperature rising during testing at 750 °C leads to excretion of the first precipitates at grain boundaries and then inside the grains, which leads to a decrease in ductile properties and the occurrence of brittle fracture, Figures 10 and 11.[5] Acknowledgments Parts of the research described in this paper were conducted at the Faculty of Natural Sciences and Engineering University of Ljubljana in accordance to the bilateral agreement between the Republic of Slovenia and Bosnia and Herzegovina within the project SLO-BA/10-11/011"Application of new materials in the automotive industry". References [1] http://ar.outokumpu.com/2009/this-is- outokumpu/market-review; Market review. (4. 5. 2010) [2] Oshima, t., Habara, y., Kuroda, k. (2007): Efforts to save Nickel in Austenitic Stainless Steels. ISIJ International, Vol. 4, No. 3, pp. 359-364. [3] Beganqvic, o., Pihura, d., Stergulc, i., Kratina, e.. Fakic, b. (2007): Osvajanje prototipova proizvoda od materijala Nitronic 60 i Nimonic 80A (Osvajanje žice za izradu prototipa pin od čelika Nitronic 60), Metalurški institut „Kemal Kapetanovic", Izvještaj br. E-1529, Zenica. [4] Lula, r. a. (1986): Stainless Steel, American Society for Metals, Ohio. [5] Gigqvic-Gekic. a. (2010): Kvantifikaci- ja uticaja alfa-gama obrazujucih elemenata na mehaničke os-obine i pojavu delta ferita kod nehrdajuceg austenitnog čelika Nitronic 60. Univerzitet u Zenici. doktorska disertacija, Univerzitet u Zenici, Fakultet za metalurgiju i materijale. [6] Gigqvic-Gekic, a., Qruč, m., Vitez, I. (2011): The effect of solution annealing on properties of steel Nitronic 60, Metalurgija, Vol. 50, No. 1, pp. 21-24. Bacterial indicators of faecal pollution and physiochemical assessment of tributaries of Ganges River in Garhwal Himalayas, India Bakterijski indikatorji fekalnega onesnaženja in fiziološko-kemijska ocena pritokov reke Ganges v Garhwalski Himalaji v Indiji Archna Sati1, Anchal Sood1, Shivesh Sharma2, *, Sandeep Bisht1, Vivek Kumar3 1Department of Microbiology, SBS Post Graduate Institute of Bio-Medical Sciences and Research Balawala, Dehradun, Uttarakhand, India 2Department of Applied Mechanics (Biotechnology), Motilal Nehru National Institute of Technology, Allahabad, Uttar Pradesh, India 3Microbiology Section, Department of Soil and Water Research, Public Authority of Agricultural Affairs & Fish Resources, PO Box 21422, Safat-13075, Kuwait Corresponding author. E-mail: dr.shiveshsharma@gmail.com Received: February 22, 2011 Accepted: March 27, 2011 Abstract: A study was undertaken to investigate the water quality of Alaknanda and Bhagirathi rivers (tributaries of River Ganges) in Garhwal Himalayan region during the periods of monsoon, summer and winter seasons. Both the rivers are sacred and are important source of water for drinking and irrigation. Water samples were analyzed for various bacteriological parameters including total viable count (TVC), total coliform (TC), faecal coliform (FC) and faecal streptococci (FS). Also, physicochemical attributes viz. dissolved oxygen (DO), biological oxygen demand (BOD) and chemical oxygen demand (COD) was assessed. Total viable count exceeded the maximum permissible limits in all the samples irrespective to different seasons. The high most probable number (MPN) values and presence of faecal coliforms and streptococci in the water samples suggests the potential presence of pathogenic microorganisms which might cause water borne diseases. A direct effect of season and human activities on the pollution status was observed at all the water sampling sites. The over all objective of this work was to investigate the incidence of these indicator organisms, coliform, faecal coliform, faecal streptococci and physi-ochemical parameters during different seasons in two main tributaries of Ganges River. Izvleček: Namen študije je bil raziskati kakovost vode rek Alaknanda in Bhagirathi (pritokov Gangesa) na območju Garhwalske Himalaje v monsunskem, poletnem in zimskem obdobju. Obe reki veljata za sveti in sta hkrati pomemben vir pitne in namakalne vode. V vzorcih vode so določali različne bakteriološke parametre, kot tudi celotno število za življenje sposobnih organizmov (TVC), celotne koliformne organizme (TC), fekalne koliformne organizme (FC) in fekalne streptokoke (FS). Določali so tudi fiziološko-kemijske lastnosti, kot so raztopljeni kisik (DO), biološka potreba po kisiku (BOD) in kemijska potreba po kisiku (COD). Celotno število za življenje sposobnih organizmov presega najvišje dopustne meje v vseh vzorcih, ne glede na čas vzorčenja. Visoke vrednosti najverjetnejšega števila (MPN) in navzočnost fekalnih koliformov ter streptokokov v vzorcih nakazuje možno navzočnost patogenih mikroorganizmov, ki utegnejo povzročati obolenja, ki se širijo z vodo. Na vseh vzorčnih mestih je mogoče opazovati vpliv letnega odobja in človekovih dejavnosti na stanje onesnaženosti. Poglavitni namen dela je bil raziskati pogostnost indikatorskih organizmov, koliformov, fekalnih koliformov, fekalnih streptokokov in fiziološko-kemijskih parametrov v različnih obdobjih leta v dveh glavnih pritokih reke Ganges. Key words:, coliforms, bacteriological, physicochemical, Ganges, river Ključne besede: koliformi, bakteriološki, fiziološko-kemijski, reka Ganges Introduction The Ganges or Ganga rises in the Northern Himalayas on the Indian side of the Tibet border. Its five headstreams i.e. the Bhagirathi, Alaknanda, Manda-kini, Dhauliganga and Pindar rise in Uttarakhand region. Of these, the two main headstreams are the Alaknanda (Latitude: 30°7'60'' N, Longitude: 78°35'60'' E) about 4 402 meter above sea level (the longer of the two), which rises about 30 miles north of the Himalayan Peak of Nanda Devi and the Bhagirathi (Latitude: 30°7'60'' N, Longitude: 78°34'60'' E) about 3 050 meters above sea level in an ice cave at the foot of the Himalayan glacier known as Gangotri, merges at Dev Prayag to form river Ganges, flows through the northern Indian planes, providing drainage and water for around 400 million people. In the recent past, expanding human population, industrialization, intensive agricultural practices and discharges of massive amount of wastewater into the river have resulted in deterioration of water quality. The impact of these anthropogenic activities has been so extensive that the water bodies have lost their self-purification capacity to a large extent. Therefore, there is a grown recognition and need that aquatic water bodies or ecosystem like Ganga must be sustained so that they may support human life. This has resulted in scarcity of potable water supply and loss of biodiversity in aquatic system. The health and well being of the human race is closely tied up with the quality of water used (Sharma et al., 2005). Most of the people in the Himalayan region use surface water for drinking which is most vulnerable to pollution due to the surface run off. Almost all major rivers have been tapped at source for drinking water supplies, but there is no monitoring of water quantity or quality on regular bases. During bathing the river water is also used for drinking (Aachman), irrespective of its water quality. But, it is evident from a course of studies carried out by different (Srivastava et al., 1996; Kulshres-tha & Sharma, 2006) that Ganges water is highly contaminated with coli-forms. Microorganisms are widely distributed in nature, and their abundance and diversity may be used as an indicator for the suitability of water (Okpokwasili & Akujobi, 1996). The use of bacteria as water quality indicators can be viewed in two ways, first, the presence of such bacteria can be taken as an indication of faecal contamination of the water and thus as a signal to determine why such contamination is present, how serious it is and what steps can be taken to eliminate it; second, their presence can be taken as an indication of the potential danger of health risks that faecal contamination posses. The higher the level of indicator bacteria, the higher the level of faecal contamination and the greater the risk of waterborne diseases (Pipes, 1981). A wide range of pathogenic microorganisms can be transmitted to humans via water contaminated with faecal material. These include enteropathogenic agents such as salmonellas, shigellas, entero-viruses, and multicellular parasites as well as opportunistic pathogens like Pseudomonas aeroginosa, Klebsiella, Vibrio parahaemolyticus and Aero-monas hydrophila (Hodegkiss, 1988). It is not practicable to test water for all these organisms, because the isolation and identification of many of these is seldom quantitative and extremely complicated (Cairneross et al., 1980; World Health Organization (WHO), 1983). An indirect approach is based on assumption that the estimation of groups of normal enteric organisms will indicate the level of faecal contamination of the water supply (WHO, 1983). The most widely used indicators are the coliform bacteria, which may be the total coliform that got narrowed down to the faecal coliforms and the faecal streptococci (Harwood et al., 2001; Pathak & Gopal, 2001; Kistemann et al., 2002). Concurrently, contamination of water by enteric pathogens has increased worldwide (Craun, 1986; Islam et al., 2001). However, to the best of our knowledge, no report is available on the bacterial as well as physiochemical parameters analysis of two main tributaries of Ganges River in Garhwal Himalayan region. The overall objective of this work was to investigate the incidence of these indicator organisms, coliforms, faecal coliforms and faecal streptococci in relation with physiochemical parameters of Alaknanda and Bhagirathi rivers in different seasons in Garhwal Himalayas, India. Materials and methods Collection of water samples Intensive survey of the study area was done to select different sites from Gangetic river system of Garhwal region. The Ganges River in Garhwal Figure 1. Map of the study area of Bhagirathi and Alaknanda river system of Garhwal Himalayas. Table 1. Sample collection sites of Alaknanda and Bhagirathi rivers. Alaknada Bhagirathi A1 Vasundhara B1 Bhojwasa A2 Mana B2 Chirwasa A3 Badrinath (Gandhi ghat) B3 Gangotri A4 Badrinath (Rishi ghat) B4 Harsil A5 Gobind ghat B5 Jhala A6 Hanuman Chatti B6 Bhaironghati B7 Gaumukh Himalayas comprises of two tributaries Bhagirathi and Alaknanda, so sampling was done from both the rivers (Figure 1). The total stretch covered in this study was about 250 km, out of which Alaknanda comprised a stretch of 135 km and Bhagirathi about 115 km. Samples were collected during the monsoon, summer and winter seasons. The samples were carefully collected in triplicate from 13 different places (Table 1) in sterile containers, and were transported in ice boxes at 3° C and brought to the laboratory for analysis (Sharma et al 2010). The results presented in the table are average of triplicate samples of a particular site. Bacterial analysis The bacterial population (total viable count, TVC) in different samples was estimated by inoculating nutrient agar plates with 0.1 mL of suitable dilutions. The results were expressed as colony forming units (cfu) per unit volume, enumerated after 48 h of incubation. The water quality was determined by the standard most probable number (MPN) method. Coliforms were de- tected by inoculation of samples into tubes of MacConkey broth and incubation at 37 ± 1 °C for 48 h. The positive tubes were sub cultured into brilliant green bile broth (BGBB) and were incubated at 44.5 ± 1 °C. Gas production in BGBB at 44.5 ± 1 °C was used for the detection of faecal coliform after 48 h incubation. Faecal streptococci were detected by inoculation of water samples into Azide Dextrose broth and incubation at 37.5 ± 1 °C for 24-48 h (APHA et al, 1999). All the culture media were obtained from Hi-Media Pvt. Ltd., Mumbai, India. Physiochemical analysis Physicochemical parameters including total dissolved solids (TDS), conductivity and pH were analyzed on site at the time of sample collection by water analysis kit (Model LT-61, Labtron-ics, Guelph, Ontario, Canada) as per manufacturer instruction. Other parameters i.e. dissolved oxygen (DO), biological oxygen demand (BOD) and chemical oxygen demand (COD) were performed in laboratory by standard ti-trimetric method (APHA et al, 1999). The data were analyzed statistically by using analysis of variance (ANOVA) to find out significance at 5 % levels. In figures, error bars indicate standard error of the mean, where error bars are not visible; they are smaller than the marker. Results The TVC value showed a regular trend (Figure 2). The values increased in monsoon season, thus generally highest counts were observed, intermediate in summer season and least in winter season for each sampling site. The highest TVC was noted in Badrinath ghat of Alaknanda river and Gangotri of Bhagirathi river, where the values were as high as 22.2 x 103 and 19.8 x 103, respectively. The lowest value 10.2 x 103 were recorded in Gobind ghat of Alaknanda and 10.2 x 103 in Bhairong-hati of Bhagirathi river, respectively. The total coliform count was high in all water samples (Figure 3), values ranged from 24/100 mL to 310/100 mL. The highest MPN (310/100 mL) was recorded during monsoon at Vasundha-ra of Alaknanda, the least count MPN (24/100 mL) was obtained in summer and winter season from Bharionghati of Bhagirathi. Even the water samples during less human activities in winter season were not found suitable for drinking as per the Bureau of Indian Standards (BIS), (1991). Results for FC and FS counts have also shown a similar trend to TVC and TC, i.e. higher in monsoon season, intermediate in summer season and least during winter season (Figure 4 and 5). Highest FC count was observed in Alaknanda at Badrinath (160.4, 122.3, 101.2)/100 mL and lowest count was at Mana (15.3, 10.2, 9.8)/100 mL during monsoon, summer and winter season, respectively. In Bhagirathi the Chirwasa and Gangotri sites showed almost similar trend of highest count (45.7, 35.4, 29.8) and 45.3, 36.9, 32.1)/100 mL during monsoon, summer and winter seasons, while the least was observed in Bhaironghati (5.9, 4.5, 3.9)/100 mL during monsoon, summer and winter seasons. Similar trend was also observed in FS, the higher count in Alaknanda was at Badrinath (25, 20, 18)/100 mL, lowest at Mana (8, 7, 7)/100 mL, while in Bhagirathi, highest at Harsil (12, 11, 10)/100 mL and least at Chirwasa (6, 3, 3)/100L. The DO value in Alaknanda ranged from 14.2-18.9 mg/L in monsoon samples and 16.9-23.1 mg/L in winter samples. In Bhagirathi DO values ranged from 10.2-15.4 mg/L in monsoon and 13.2-19.8 mg/L in winter season (Figure 6). Badrinath and Chir-wasa showed a remarkable increase in DO in winter season. Though, in general the DO content of all the river water samples show a uniform trend with varying seasons i.e. least during 25 20 15 x 1 " 10 A6 B1 B2 B3 B4 Sampling sites □ Monsoon [U Summer El Winter B6 B7 Figure 2. Total viable count (TVC) from Alaknanda and Bhagirathi rivers 'il A2 A3 A4 A5 A6 0 Monsoon Q] Summer El Winter B1 B2 B3 B4 B5 B6 B7 Sampling sites Figure 3. Total coliforms Alaknanda and Bhagirathi rivers El Monsoon [Q Summer 11 Winter Al A2 A3 A4 A5 A6 B1 B2 B3 B4 B5 B6 B7 Sampling sites Figure 4. Feacal coliforms count in Alaknanda and Bhagirathi rivers 30 25 20 6 o o 15 10 E3 Monsoon [D Summer El Winter Al A2 A3 A4 A5 A6 B1 B2 B3 B4 B5 B6 B7 Sampling sites Figure 5. Feacal streptococci from Alaknanda and Bhagirathi rivers monsoon, highest during winter and intermediate in summer season. However, all the samples were found to be saturated with oxygen and were fit for bathing, wild life and irrigation with respect to the amount of dissolved oxygen. The BOD values for most of the water samples were above the permissible limit (Figure 7), samples in monsoon season have high BOD value, and thus the water was not fit for drinking. Considerably higher COD values were recorded in the monsoon season in all the sites of study area, the COD ranged from 4.5 mg/L to 31 mg/L in all water samples (Figure 8). The effect of season was observed in the pH of water samples throughout this study. The pH was slightly alkaline in winter, but al- most neutral in summer and monsoon seasons. Conductivity and TDS in all the sites were found to be well within the minimum prescribed limits (APHA et al, 1999) (data not given). Discussion In present study, all sites were found to have high TVC. In fact, the water of Ganga is used for drinking (Aachman) as part of rituals in this region. Although the higher TVC values suggest that this practice should be avoided. Earlier Baghel et al, (2005) and Sood et al., (2008) have also observed high TVC values in the entire stretch of river Ganga in Uttarakhand region. Baghel AI A2 A3 A4 A5 A6 0 Monsoon CD Summer H Winter B1 B2 B3 B4 B5 B6 B7 Sampling sites Figure 6. Dissolved oxygen in Alaknanda and Bhagirathi rivers 25 20 15 I 10 Al A2 A3 A4 A5 A6 Sampling sites E3 Monsoon □ Summer El Winter B1 B2 B3 B4 B5 B6 B7 Figure 7. Biological oxygen demand in Alaknanda and Bhagirathi rivers 35 30 25 20 15 10 5 0 i Al A2 A3 A4 A5 A6 Sampling sites 0 Monsoon □ Summer 0 Winter B1 B2 B3 B4 B5 B6 B7 Figure 8. Chemical oxygen demand in Alaknanda and Bhagirathi rivers et al, (2005) concluded that large number of animals used by natives and pilgrims in upper stretch of Gangetic river system increase FS load. As a matter of fact, the banks of Alaknanda are more densely populated and face heavy anthropological activity as compared to Bhagirathi. Earlier, Fokmare & Musaddiq (2001) have correlated high content of MPN in surface and ground water of Akola, Maharashtra (India) with the population density. Also the fact that the number of sub-tributaries falling in Alaknanda is more than Bhagirathi may be responsible for the higher col-iform count. The less number of FC and FS in most of the sites of study area may be attributed to the fever anthropological activities. All the sites included in this study were found suitable for bathing purpose with respect to the maximum permissible limits of FC and FS counts as per the standards laid by National River Conservation Directorate (NRCD), India. Earlier, Sood et al, (2008) have also studied water quality of Ganga in Utt-arakhand Himalayas, India and have reported a high level of BOD due to introduction of organic matter into the system as a result of anthropogenic activities. Also these values showed a proportional relation with human activities i.e. the fewer the human activities (in winter), the better the water with respect to physicochemi-cal parameters. Higher BOD values in most of the water samples suggest that either these rivers are rich in organic matter or organic matter is being introduced in the rivers by anthropogenic activities (Tijani et al, 2005), since, BOD provides a direct measurement of state of pollution. Relationship between BOD, COD and microbial count was found inversely proportional, implying that at high organic loading rates, the ecosystem retards the growth of aerobic microorganisms and favors the growth of anaerobes; our findings draws support from Mtui & Nakamurs (2006). The use of coliform bacteria as a measure of the faecal contamination of streams and lakes has been in practice for many years. Our study gives an indication of the extent of relation of microbial pollution and physiochemi-cal parameters; any further addition of wastes may deteriorate the existing hygienic quality in the area. These results suggest that increase of population of coliforms in a river environment are directly proportional to the degree of sewage and human waste pollution, which is reflected by BOD and COD levels. Sah et al. (2000) have stressed on the point that the pollution in rivers and water bodies from industries may adversely affect aquatic life of water bodies' as well human health in the vicinity of rivers/lakes. In a broad view, the river site with higher catchments area, soil cover and land use are more polluted, owing to more anthropogenic activities. McLellan et al, (2001) stated that faecal pollution indicator organisms can be used to a number of conditions related to the health of aquatic ecosystems and to the potential for health effects among individuals using aquatic environments. The presence of such indicator organisms may provide indication of water-borne problems and is a direct threat to human and animal health. Our studies on microbial ecology and physiochemical analysis in the upper Gangetic tributaries in relation to pollution have clearly revealed that there is significant presence of bacterial indicators of faecal pollution; the situation is serious and alarming. Presence of bacterial indicators of faecal contamination in river water at origin clearly revealed the bacteriological status of the water at that site. For this reason, monitoring of microbial contamination in river should be an essential component of the protection strategy in that area. The base line data generated on bacteriological water quality of rivers may serve as biomonitoring standard and comparisons for other rivers and may be useful for all scientists, decision makers and resource managers working with environmental planning and management of such areas. Conclusions The rationale of this study was to evaluate the impact of season and human activities on the pollution status of main upper Gangetic tributaries. This study revealed that tributaries at origin are threatened by high influx of pollutants and enteric pathogenic contamination and it can be concluded that In Alaknanda River, Badrinath is most polluted and Mana is the least, while in Bhagirathi River Gangotri is most polluted and Gaumukh is least. The constant surveillance of these water bodies with respect to the bacterial indicators and physicochemi-cal parameters provides us with the opportunity of true microbiological monitoring of the area as well as proper management actions could be applied in order to improve the quality of these holy rivers and consequently reduce public health risk. Acknowledgments Authors are grateful to the Management of SBS Post Graduate Institute of Bio-Medical Sciences and Research Balawala, Dehradun, (UK), India for providing research facilities required to carry out this work. References APHA, AWWA, WEF (1998): Standards for Examination of Water and Wastewater, 20th ed. American Public Health Association, Washington DC USA. Baghel, V. S., Gopal, K., Diwedi, S. & Tripathi, R. D. (2005): Bacterial indicators of faecal contamination of the Gangetic river system right at its source. Ecol. Indicators, Vol. 5, pp 49-56. BIS (1991): Indian standard specification for drinking water. IS: 10500, Indian Standard Institute. Cairneross, S., Carruthers, I., Curtis, D., Feachem, R., Bradley, D. & Baldwin, G. (1980): Evaluation for Village Water Supply Planning. Wiley, Chichester, p. 277. Craun, G. F. (1986): Water Borne Disease in the United States. CRC Press, Boca Raton, FL. Fokmare, A. K. & Musaddiq, M. (2001): Comparative studies of physico chemical & bacteriological quality of surface & groundwater at Akola (Maharastra). Pollution Res., Vol. 20, No. 4, pp 651-655. Harwood, V. J., Brownell, M., Perusek, W. & Whitelock, J. E (2001): Vancomycin-resistant enterococ-cus sp. Isolated from waste water and chicken feces in the United States. Appl. & Environ. Microbiol. Vol. 67, pp. 4930-4933. Hodegkiss, I. J. (1988): Bacteriological monitoring of Hong Kong marine water quality. Environ. Int. Vol. 14, pp. 495-499. Islam, M. S., Siddika, A., Khan, M. N. H., Goldar, M. M., Sadique, M. A., Kabir, A. N. M. H., Huq, A. & Colwell, R. R. (2001): Microbiological analysis of tube-well water in a rural area of Bangladesh. Appl. & Environ. Microbiol. Vol. 67, pp. 3328-3330. Kistemann, T., Claben, T., Koch, C., Dangendorf, F., Fischeder, R., Gebel, J., Vacata,V. & Exner, M. (2002): Microbial load of drinking water reservoir Tributaries during extreme rainfall and runoff. Appl. & Environ. Microbiol. Vol. 68, pp. 2188-2197. Kulshrestha, H. & Sharma, S. (2006): Impact of mass bathing during Ar-dhkumbh on water quality status of river Ganga. J. Environ. Biol. Vol. 27, No. 2, 437-440. McLellan, S. L., Daniels, A. D. & Sal-more, A. K. (2001): Clonal populations of thermotolerant en-terobacteriaceaes in recreational water and their potential interference with foecal Escherichia coli counts. Appl. & Environ. Microbiol. Vol. 67, pp. 4934-4938. Mtui, G. V. S. & Nakamurs, Y. (2006): Physiochemical and microbiological water quality of lake Sagara in Malagarasi wetlands. J. Eng. & Appl. Sci. Vol. 1, No. 2, pp. 174180. okpokwasili, G. C. & Akujobi, T. C. (1996): Bacteriological indicators of tropical water quality. Environ. Toxicol. & Water Quality. Vol.11, pp 77-81. Pathak, S. P. & Gopal, K. (2001): Rapid detection of Escherichia coli as an Sharma, S. (2008): Assessment of indicator of faecal pollution in wa- bacterial indicators and physico- ter. Indian J. Microbiol.Vol. 41, pp chemical parameters to investigate 139-151. pollution status of Gangetic river Pipes,W. O. (1981): Bacterial indicators of system of Uttarakhand (India). pollution. CRC Press Inc., Boca Ecol. Indicators. Vol. 8, 709-717. Raton, FL, p. 242. Srivastava, R. K., Sinha, A. K., Pandey, Sah, J. P., Sah, S. K., Acharya P., Pant D. D. P., Singh, K. P. & Chandra, H. & Lance V. A. (2000): Assessment (1996): Water quality of the river of water pollution in the Narayani Ganga at Phaphamau (Allahabad): River, Nepal. Int. J. of Ecol. & En- Effect of mass bathing during Ma- viron. Sci. Vol. 26, pp 235-252. hakumbh. Environ. Toxic. Water Sharma, P., Sood, A., Sharma, S., Bisht, Quality. Vol. 11, No. 1, pp 1-5. S., Kumar, V., Pandey, P., Gusain, Tijani, M. N., Balogun, S. A. & Adel- M. P. & Gusain, O. P. (2010): Bac- eye, M. A. (2005): Chemical and terial indicators of faecal pollution microbiological assessment of and physiochemical assessment water and bottom-sediments con- of important North Indian lakes. taminations in Awba lake (U.I), RMZ-Mate. & Geoenviron. Vol. Ibadan, SW-Nigeria. RMZ-Mate. 57, pp 25-40. & Geoenviron. Vol. 52, pp. 123- Sharma, S., Bajracharya, R. M., Sitaula, 126. B. K. & Merz, J. (2005): Water World Health organization (1983): quality in the central Himalaya. Guidelines for Drinking Water Curr. Sci. Vol. 81, pp 774-786. Quality, Vol. 3. World Health Or- Sood, A., Singh, K. D., Pandey, P. & ganization, Geneva. Integrated geophysical and geotechnical investigation of the failed portion of a road in basement complex Terrain, Southwest Nigeria Povezane geofizikalne in geotehnične preiskave poškodovanega dela ceste na ozemlju metamorfne podlage v Jugozahodni Nigeriji Osinowo, O. Olawale1, *, Akanji, A. Olusoji1, Akinmosin Adewale2 University of Ibadan, Department of Geology, Ibadan, Nigeria 2University of Lagos, Department of Earth Sciences, Lagos, Nigeria *Corresponding author. E-mail: wale.osinowo@mail.ui.edu.ng Received: March 23, 2011 Accepted: May 3, 2011 Abstract: Several efforts by the local authority to fix the bad portions of Ijebu-Ode-Erunwon road, southwest Nigeria have yielded no meaningful result, as the road often get deteriorated shortly after repairs. Geophysical investigation integrated with geo-technical studies were undertaken to determine causes of the consistent failure of the highway. Very Low Frequency Electromagnetic (VLF-EM) and Electrical Resistivity (ER) methods were employed to map sections of the road with anomalous electrical responses and interpreted in-terms of structures, li-thology and water saturation. VLF-EM plots identified positive peaks of filtered real amplitudes greater than 30 % which correspond to major and minor linear fractures within the basement rocks. High current density >30 and low resistivity <10 Q m delineated rock units underlying the failed pavement to be water saturated. Liquid limit, linear shrinkage and plastic limit index results; 24.0-48.5 %, 2.1-12.9 %, 7.5-27.4 % respectively, indicate excellent to good engineering index properties. However, soaked and unsoaked CBR results; 70.3-83.9 %, and 12.9-31.6 % respectively, indicate percentage reduction in strength with wetness up to 80 %. This study implies that integrated geophysical and geotechni-cal investigation offers very useful approach for characterizing near surface earth which could be helpful in site preparation prior to construction. Izvleček: Vrsta poizkusov krajevnih oblasti, da bi popravili slabe odseke ceste Ijebu-Ode-Erunwon v jugozahodni Nigeriji ni bila uspešna, ker se je navadno stanje ceste poslabšalo kmalu nato, ko so jo popravili. Da bi ugotovili vzroke za ponavljajoče se propadanje ceste, so opravili geofizikalne raziskave v povezavi z geotehničnimi študijami. Z zelo nizkofrekvenčno elektromagnetno metodo (VLF-EM) in metodo specifične električne upornosti (ER) so preiskali odseke ceste z anomalnimi električnimi lastnostmi in jih interpretirali z ozirom na zgradbo, litolo-gijo in nasičenost z vodo. Na diagramih VLF - EM so ugotovili pozitivne vrhove filtri-ranih realnih amplitud večjih od 30 %, ki ustrezajo večjim in manjšim linearnim razpokam v kamninah podlage. Visoka gostota toka >30 in nizka specifična upornost <10 Q m sta značilni za zemljine, nasičene z vodo, ki leže pod poškodovanim cestnim površjem. Vrednosti meje tečenja 24.0-48.5 %, meje krčenja 2.1-12.9 % in indeksa meje plastičnosti 7.5-27.4 % nakazujejo od odlične do dobre inženirske indeksne lastnosti. Toda rezultati preskusa CBR v nasičenem in nenasičenem stanju, 70.3-83.9 % in 12.9-31.6 %, kažejo, da se zmanjša nosilnost pri vlagi do 80 %. Raziskava priča o tem, kako uporabno je povezati geofizikalne in geotehnične preiskave za karakteri-zacijo pripovršinskih tal, kar utegne biti smotrno pri preiskavi terena pred samo gradnjo. Keywords: electromagnetic, resistivity, geotechnical, basement complex, Ijebu-Ode Ključne besede: elektromagnetna metoda, specifična upornost, geotehnične metode, kamnine podlage, cesta Ijebu-Ode, Nigerija Introduction Flexible highway aids easy and smooth vehicular movement, and has been very useful for transportation of people, goods and services from one point to another, especially in developing countries where other means of transportation such as rail, underground tube, air and water transport system have remained largely undeveloped. However, bad portions of road, many of which result from poor construction or being founded on incompetent sub-grade and sub-base materials had been found to do more harm than good. They have been responsible for many fatal accidents, wearing down of vehicles and waste of valuable time during traffic jams. The various types of road failure identified in the study area include failure of the black top surfacing, especially along wheel cracks, pitting or minor dent, shear or massive failure (pot-holes) extending through the pavement occasionally to the subgrade. (Plate 1) The integrity of near surface geophysical investigation methods to complement geotechnical studies in some foundation engineering problems cannot be overemphasized. This research therefore integrates Electromagnetic, Electrical Resistivity and geotechnical techniques to study the causes of consistent failure of Luba-Erunwon axis of Ijebu-Ode-Erunwon road. It involves lateral and vertical probe of the failed, fairly stable, fairly failed and stable portion of the road in order to characterize the near surface geologic materials that constitute the sub-grade, sub-base and the foundation upon which the pavement was founded. The study area is situated within the southwestern part of Nigeria, it lies between longitudes 6049' N and 6°52' N, latitude 3056' E and 3058' E and the studied portion of the pavement is about 2 Plate 1. Failed section of Luba-Erunwon axis of Ijebu-Ode-Erunwon road km in length. The road was initially constructed in 1983 and have since suffered major failures, especially in the northeastern end, towards Erunwon axis of the road. The road has been repaired severally, the repairs usually include minor repair of the road element and resurfacing. However the northeastern part of the road always starts to deteriorate barely six months after reconstruction. Geological setting Ijebu-Ode and environ lies within the transitional zone between the Precam- brian Basement Complex rocks of the southwestern Nigeria and the Cretaceous sediments of Abeokuta Group in eastern part of Dahomey Basin. The basement rocks occur predominantly in the north, northwest and northeastern parts of the field and it is predominantly a Migmatite Gneiss Complex of biotite granite gneiss, biotite-horn-blende gneiss with varying degrees of fracturing (Olayinka and Osinowo, 2009). The southern part of the field is overlain by Ise Member of Abeokuta group that unconformably overlies the basement rocks. Litho-stratigraph-ically, Abeokuta Group comprise of Figure 1. Geological map of Ijebu-Ode and its environ with geological map of Nigeria inserted grits, arkosic sandstones, siltstones and clay with occasional conglomerate of predominantly arenaceous materials (Omatsola and Adegoke, 1981). Figure 1 shows the geology of Ijebu-Ode and its environ. Materials and methods Electromagnetic method is one of the geophysical methods commonly used in foundation investigation and environmental studies (Olorunfemi & Mesida, 1987; Sharma, 1997). The principle is based on induction of a secondary magnetic field Hs in the subsurface conductor of conductivity o due to effect of an artificially generated primary field HP Electromagnetic measurements are usually presented as the mutual impedance ratio Z/Z0 or relative charge in the impedance over a conductor which has ability to provide clear information about the subsurface conductivity and structure. Z/Z0 - 1 = HHrn. o. h. s) HpZ (s) " ABEM WADI was used for VLF-EM measurements, it uses military transmitters as the source of primary electromagnetic waves HP which is located several kilometers away at the high powered military communication transmission stations. The transmitter's antenna transmits signals continuously at low radio frequency range of 15-30 kHz. The signals generated can travel long distance and able to penetrate the subsurface to induce eddy current in buried conductors. The technique measures the components of Very Low Frequency EM field which are related to the geoelectric structure of the subsurface. (Chouteau et al, 1996). Five VLF-EM profile stations were occupied with the profile length ranging from 250 m to 850 m. Readings were taking at station interval of 3 m and 6 m. Measurements such as raw real, raw imaginary, station's latitude and longitude and the signal strength were recorded against station interval. Electrical resistivity investigation of the subsurface involved determination of the distribution of ground resistivity based on its response to the flow of electric current injected during surface measurement. True ground resistivity of the subsurface can be estimated and can further be employed to interpret the subsurface qualitatively and quantitatively ((Loke, 2001). Georesistiv-ity survey involved measurement of potential difference generated by the current electrodes adapted to Wenner and Schlumberger electrode configurations. p = AV/I • K 'a K is the geometric factor. Two measurement methods were adopted; 1-D Vertical Electrical Sound- ing (VES) and 2-D resistivity measurement using Electrical Resistivity Traversing (ERT) technique. The 1D VES measurements aimed at determining the variation in the geoelectric parameters with depth at the probed stations while 2D method mapped resistivity continuity useful to delineate structurally weak zones that could be responsible for continuous failure of the road. Ge-opulse Tigre resistivity meter was used to measure ground resistance. Current electrodes for 1D measurement were spread from AB/2 of 1 m to 133 m for VES measurement. Two dimensional measurements was made by increasing the electrode spacing along the levels. Ten levels along profiles were covered with electrode spacing range from 3 m to 30 m at incremental step of 3 across 100 m long profile. Geotechnical studies to determine some engineering index properties of sub-grade and sub-base materials employed to corroborate the geophysical measurements involved collection of twelve disturbed bulk samples from four pits each drilled to depth of 1 m and at sampling depths of 0-0.3 m, 0.3-0.6 m and 0.6-1.0 m from each pit. Sample recovering pits were constructed at the failed, fairly stable, fairly failed and stable parts of the road at 80 m, 247 m, 300 m and 470 m on the road. Mechanical sieving helped determined particle size distribution of gravel and sand proportions of dried coarse frac- tion. Consistency Limit Tests generally known as the Atterberg limits gave the plasticity characteristics of the cohesive fraction of the sieved samples. The consistency limit test includes; liquid limit, plastic limit and linear shrinkage test. The difference between the liquid and plastic limits gave the plasticity index, which is the range of moisture contents over which the soil remains plastic. California Bearing Ratio (CBR) test, widely used to characterize and select sub-grade materials for use in road construction was carried out. The test was devised by the California Highway Association and it is simply the ratio of the load that cause a penetration of 2.5 mm or 5.0 mm material to a standard load that causes similar penetration on a standard California sample, notably 13.24 kN and 19.96 kN respectively. C B R = Load that caused a penetration of 2.5/5.0 mm x 100 % 13.24/19.96 (kN) Both soaked and unsoaked CBR tests were carried out and swelling of samples was carefully monitored during the 96 h of soaking period to assess the likely effect of water ingress on the swelling of base material. The samples were compacted at the modified AASHTO level as described under procedure for compaction test in a standard CBR mold. Data processing The obtained raw real (in-phase) and raw imaginary (quadrature) components contain valuable diagnostic information of the subsurface but in a complex pattern that cannot directly and easily be related to the causative body. They contain noise, the raw real/ imaginary data are also often wrongly located on the source along the profile. To correct the above effects and obtain profiles or pseudo-section/images that are easy to interpret, two different data processing techniques were applied. Fraser (1969) and Karous & Hjelt (1977, 1983) filtering operators. Fraser filter is a linear high-frequency bandpass filter that yields semi-quantitative interpretation of data. It transforms the in-phase components into contourable data with noise reduced to the best possible minimum. VLFPROS MATLAB code for processing VLF-EM data developed by Sundararajan et al. (2006) was employed to carry out both the Fraser and the Karous and Hjelt filtering operations. Electrical resistivity data processing involved cleaning the data to remove spurious readings. Resultant VES data were plotted on bi-log paper and partial curve matched using standard two layer curves and auxiliary curves; Cagniard graph (Koefoed, 1979), to obtain some geoelectrical parameters such as layer depth/thickness and layer resistivity values (Orellana & Mooney, 1966). The obtained geoelectrical parameters from partial curve matching were used as initial model parameters to interpret the geoelectrical sounding curves using inversion model software RESIST (Vander Velpen, 1988) and WinG-Link. The inversion algorithm involves the calculation of curves for observed data by convolving the resistivity transform with appropriate filter coefficient, (Ghosh, 1971 and O'Neill, 1975). The inversion algorithm filters spurious data, enhance signal as well as correct depth matched for obtained geoelectric layers. Data Quality Check (QC) was carried out on the obtained ERT data for spurious data. The resultant data were inverted using the DIPRO inversion software based on the inversion principle presented by Yi & Kim, (1988). The software is a 2 2 dimensional inversion subroutine designed based on the Least Square inversion algorithm and uses two different modeling and smoothening approaches. The FDM Inversion performs smoothness constrained least square inversions based on the finite difference modeling assuming flat topography, while the FEM performs smoothness constrained least square inversion based on finite element modeling. The software automatically determines a two dimensional resistivity model of the subsurface for the obtained data. A forward modeling 150 osinqwq, o. o., Akanji, o. A., Akinmqsin A. subroutine is applied to calculate theoretical apparent resistivity values and a non-linear least squares optimisation techniques was used for the inversion subroutine, (DeGrqqt-Hedlin & Constable, 1990 and Sasaki, 1989). Results Palacky et al. (1981), De Rqqy et al. (1986), Hazell et al. (1988) and other authors have shown the relevance of EM method to be in overburden thickness estimation and basement fracture delineation. Figures 2 (a-f) present the VLF-EM plot of raw real and filtered real components against the profile distance in meters. Two basic anomaly types were identified using characteristic feature curves of coincident inflections on real component anomaly curves as well as the amplitude of the filtered real anomaly. The sign 'F' indicates point with positive peak filtered real anomaly with amplitude ranging between 30-60 %. It characterizes regions or points along the profile with major linear displacement at depth <5 m which may represent a fractured or sheared zone. The sign 'f' indicates positive filtered real anomaly of amplitude <30 % and characterizes zones or points with loose materials at depth <5 m. Five major linear features F1-F5 were delineated at 87 m, 178 m, 298 m, 657 m and 810 m of the profile. Features F1, F2 and F5 were identified at the failed portion while features F4 and F3 were found at the fairly failed part of the road respectively. This shows that 60 %o of the identified major features underlie the intensely failed portion while 40 % underlies fairly failed portion. Also, features f1—f8 were detected around locations 203 m, 3330 m, 410 m, 482 m, 553 m, 578 m, 848 m, 1040 m of the profile length. Figure 3 is the current density plot along profile 1 which traversed the failed, fairly stable and stable portions of the road from NE-SW. The profile indicates relatively high conductive zone as evident by high current density (up to 30) close to the surface in the north-eastern end and central part of the profile. These zones coincide with the failed portion of the road, it also coincides with the highly fractured part. The high conductivity is likely due to high water filled fractures in the basement rock. Similarly, low resistivity section at the north-eastern end of the road (high conductivity) was identified on the 2-D inverted section obtained from the ERT profile (Figure 4) and resistivity section (Figure 5) constructed from VES data around the study area. The stable portion has a relatively thick and dry sandy unit upon which the pavement rests directly. Vertical Electrical Soundings (VES) identified three to four layered earth interpreted as top soil, loose saturated clayey sand unit and highly saturated fractured basement at the failed section of the road. Figure 6 (a and b) present the representative around the stable and failed portion of curves and interpreted log of VES data the road. 1.76 296.56 (P4) 87.05 -2.04 85.01 + 10.70 19.48 m 8 (PK) 9S.71 Drop of pressure to 1 bar and desorption of gas (mainly CO;+N:) lasting for 15 hours 6.89 12.55 Decrease then tacmwe of pressure nt ntlsorplion of COj + Ni r. tPT Jl - ft i : m* M P(«iiar# 4SD- p. r— Pi nt nl hid *t M i-nD i^f iiat Timr (fc> 1UP 1MQ lita ^7\¡f> "1 Prt-nUfflt«1) H>P-> Figure 6. Graphic presentation of the used starting pressures (Pp P2, P3, P4) with adsorption in particulate phase and especial event (Px) with decrease and then increase of pressure during the adsorption process of CO2 - - N2 mixture. Figure 7. Pressure behaviour as measured in autoclave after 1st and 2nd dosing by CO2, and after dosing by N2 (in a linear and the logarithmic scale). Note that dosing by CO2 causes adsorption of gas into coal substance (detected as two slight decreases of pressure in the first two 45 min lasting steps), and that N2 dosing causes - after an instant time of adsorption - a release of gas from coal (detected as slight increase and then stabilizing of pressure in the time interval between 1.75 h and 8 h). Note also considerably higher pressure of N2 dosing in comparison to CO2. 1 ? i i Da s sorption Sample 2 71m« (Hour] - lin.sc« 6 7 a -1 lie 9 10 11 --- - ressire (tarHlofl. time scale} Tessure iknaiXfcn line st^cj 2 13 N S ! S * ...... 55 - fi j ï , S t a 2.5 2 1 î g o.c M>1 0 il Tit e(H QU ri- to 9 3C 1 ate 0 1 DO Figure 8. Desorption of gas from sample 2-1. Measurements expressed by A pressure values are shown in a normal linear scale and the logarithmic scale, respectively. detected by Pezdic at el. (1999b) and was explained by different possible processes, which would need additional investigations. One explanation is enhanced release of gases from coal, and some other explanations are thoroughly given in Pezdic et al. (1999b), Pezdic et al. (2007) . • Comparing results for sample 2-1 and 2-2, adsorption due to CO2 dosing is slightly more effective for the first sample, whereas gas release due to N2 dosing is somewhat higher in the second sample. • Desorption is 6.67 bar or 12.09 g/ kg in the first measurement case (21), and 6.89 bar or 12.55 g/kg in the second case (2-2), respectively. Sample 1-1 and Sample 4-1: Samples 1-1 (X 100 %) and 4-1 (X 80 %, dXxD 10 %, fD 10 %) are very similar in lithotype composition, but demonstrate quite diverse sorption characteristics (Figure 10). In the first and the second CO2 loading stage together, sample 4-1 adsorbed 3.26 g/kg or 43.10 % less of CO2 than sample 1-1 with 5.73 g/kg. Additional N2 pressure caused initially a slight decrease of the total pressure in both samples, but then the pressure started to rise (as principally visible from Figure 7), and reached after six hours the value of 90.25 bar for sample 1-1 and the value of 92.57 bar for sam- ple 4-1. Sample 1-1 released 5.87 bar of gas or 10.44 g/kg, whereas sample 4-1 released 11.09 bar of gas or 19.01 g/kg i.e. for almost 80 % more than sample 1-1. Proportion of released gas depends on the proportion of adsorption in the first two steps, on CO2 compression at the time of addition of N2 overpressure, and on velocity of gas mixture release, as we decreased the pressure to 1 bar. For the same reason desorption varies too. The desorption for sample 1-1 equals to 5.30 g/kg or to 32.78 % of the wholly adsorbed gas (5.73 + 10.44 g/ kg), and for 4-1 to 3.74 g/kg or 16.80 %. Already our findings so far categorized the samples of such entirely xylite, and xylite-very-rich lignite lithotypes as the most resistant for sorption. In this sense, our present measurements published in this paper confirm this finding once again. Sample 3-1 and Sample 6-1: Samples 3-1 (dXxD 20 %, fD 80 %) and sample 6-1 (dXxD 7 %, fD 93 %) differ significantly in content of xy-lite-detrite (dXxD) component. Even though this difference (20-7 %) is numerically not very big it seems to be decisive to give the two samples quite distinctive gas adsorption characteristics. As visible from Figure 10, total CO2 adsorption in the sample 3-1 amounts to 6.06 g/kg, and in sample 6-1 to 7.62 g/kg. In the second stage, less than a half of gas than in the first stage was adsorbed. Additional N2 pressure caused initially a slight decrease of the total pressure for both samples, but afterwards the pressure started to rise and reached the value of 95.25 bar for sample 3-1, and 93.93 bar for sample 6-1. Sample 3-1 released 16.06 g/kg of gas and sample 6-1 16.69 g/kg of gas. Desorption of the sample 3-1 equals 8.09 g/kg or 36.57 %, and of the sample 6-1 7.09 g/ kg or 29.90 %. Sample 2-1 and Sample 5-1: Samples 2-1 (fD90%, G10%) and sam- ple 5-1 (X 15 %, fD 65 %, G 20 %) have the same lithotype code (9.5), although their composition is different. The sample 2-1 comes from a fault zone and the sample 5-1 from a borehole. What is common to both samples is remarkable degree of gelification which was most probably enhanced due to alkalinity evidenced by e.g. carbonate coatings of vegetal remnants (see Table 1). Their gas adsorption and desorption values are much higher than for all previous samples, and this feature is connected to our opinion to geli-fication. Total adsorption of sample 2-1 is 8.98 g/kg, and of sample 5-1 9.80 g/ kg (Figure 10). Compared to the sample 4-1 with the lowest adsorption, this is around 60 % more. Figure 9. Amount of adsorbed CO2 gas depends on lithotype code cs «.00 7,00 6.00 5.00 $ J.OD 1 3.00 1 | 2.00 1,00 Amount of adsorbed C02 gas in the first two stages 3 2D 9 10 fD9i n uoa 030 n K BD 1 ■ 1 - 1 1 n 1 0.00 SaH^1 □ Adsorption I stage ■ Adsorption 2 stage Satni)lei sa^t^^ sa^P1®* semi*®5 sa^6 Lignile samples Figure 10. Amounts of adsorbed CO2 as achieved by 1st and 2nd step of dosing by CO2 at pressures of between 55 bar and 59 bar. Time of adsorption was 45 min for each step. (JS us. hi C! Ctunpirluili (if ¡H c\hui r ill jdiarpliOH fc „ ^^^^ I ni r G (n n»