QUALITATIVE DISCOVERY OF QUARTZ IN MOUAU SOILS USING AN X-RAY DIFFRACTION METHOD I.E.OTUOKERE*, V.E. OKO AND O.K. AMADI Department of Chemistry, Michael Okpara University of Agriculture, Umudike Email: tosmanbaba@yahoo.com ABSTRACT Qualitative determination of the mineralogical composition of Michael Okpara Universiry of Agriculture Umudike (MOUAU) soils were performed by means of the Hanawalt method using Xray powder-diffraction. Result obtained was analyzed using Bragg-Wolf equation and International centre for diffraction data software. Bragg’s equation was used to find the d-value corresponding to Bragg’s angles. The d-spacing’s and relative intensities of the X-ray diffraction patterns for the various colleges in MOUAU compare well the d-spacing in the reference stick pattern for quartz (SiO2) 3.342 Å (100.00%), 4.257 Å (22.00%), 1.8178 Å(14.00%). Other dspacings values of the diffractogram compare well with the reference stick pattern. X-ray diffraction pattern of MOUAU soil suggested the presence of quartz mineral. Keywords: Qualitative; quartz; minerals; x-ray diffraction; soil; Umudike INTRODUCTION Quartz, or α-quartz, is the mineral form of SiO2 stable at low temperatures and pressures. The English word derives from the Saxon word querkluftertz (cross-vein ore)1. It occurs in igneous, sedimentary, metamorphic, and hydrothermal mineral environments, particularly in continental regions. It is, however, rare in oceanic rocks. As the structure is acentric, it 1 occurs in both left and right-handed varieties and is both piezoelectric and pyroelectric. It is usually nearly pure and accepts only very limited amounts of other elements in substitution. Polymorphs include β-quartz, tridymite, cristobalite, coesite, stishovite, and keatite. The structure of quartz consists of corner-sharing SiO4 tetrahedra so that each Si is bonded to four oxygens, and each oxygen is bonded to two silicon atoms. The resulting structure forms an open three-dimensional framework, so that quartz is classified as a tektosilicate or framework silicate. Quartz is the stable form of SiO2 at atmospheric temperature and pressure. It is denser than tridymite and cristobalite, the high temperature forms, but less dense than the high pressure forms, coesite and stishovite 2. At 573 ºC, trigonal low quartz transforms reversibly to hexagonal high quartz 2. Many methods of quartz determination have been proposed, in particular chemical methods diffraction(XRD) methods 5,6 3,4 and X-ray which are less accurate but more rapid. The technical evolution and automation of XRD equipment has made the XRD determination of quartz easier and more accurate and such a method has been developed and tested on different particle sizes7. Michael Okpara University of Agriculture, Umudike is located within 7km east of the capital city of Abia State ‘Umuahia’ in present day Ikwuano Local Government Area of Abia state. The presence of these institutions has undoubtedly added to a great increase in the population of the area. Rapidly increasing population, rising standards of living and exponential growth in industrialization and urbanization tends to add pressure on natural resources8. In view of this; we have decided to determine mineralogical composition of soils in Michael Okpara University of Agriculture, Umudike (MOUAU) using an X-ray diffraction method. 2 MATERIALS AND METHODS Description of the Study Area: Michael Okpara University of Agriculture, Umudike is located in Ikwuano Local Government Area, Abia State. Ikwuano Local Government Area is geologically situated in the Eastern Niger Delta and lies within latitudes 5 20 and 5 32' N, and longitudes 7 32 and 7 40 E (Fig 1).8 0 ' 0 0 ' 0 ' Figure 1: Map of Ikwuano L.G.A showing, Michael Okpara University of Agriculture, Umudike 3 Sample Collection: Soil samples were collected from various colleges in Michael Okpara University of Agriculture, Umudike (MOUAU) at a depth of 15-30 cm. The samples were packed in a small plastic bag and labeled. The collected sample were strained to remove the fibrous and undesired materials with the help of 2mm sieve and dried by heating to remove humidity because humidity affects the results very badly and then grounded to make them homogeneous before XRPD analysis. Particle size determination was made by the Bouyoucos hydrometer method 9. Colour was compared with standards. pH was determine using Ciba Corning pH meter. Qualitative phase analysis: X-ray diffraction patterns were made with a monochromatic x-ray Diffractometer system XPERT-PRO with beta filter CuKα radiation wavelength of 1.5406Aº and automated silt. A set of 2θ angle ranging from 10º- 90º was used; this was done at Sheda Science and Technology Complex (SHESTCO), Abuja Nigeria. Qualitative phase analysis was used for the study of crystal structure and unknown phases of soil. RESULTS AND DISCUSSIONS The textural characterization of Michael Okpara University of Agriculture, Umudike soil is presented in Table 1. The selected d-spacings and relative intensities of the diffractogram are presented in Table 2. The x-ray diffractogram of soil samples from MOUAU is presented in Figures 2-8. The reference pattern from International Centre for Diffraction Data using POWD-12++ have been presented in Figure 9. 4 Table 1: pH and soil texture of MOUAU Soil College CAERSE CAFST CASAP CASE CMBB CNREM COLPAS Sand (%) 95.21 97.21 99.21 95.21 94.21 92.21 96.21 Silt (%) 4.20 2.20 0.30 4.20 5.00 7.20 3.00 Clay (%) 0.59 0.59 0.49 0.59 0.79 0.59 0.79 pH 4.31 7.47 8.51 5.22 4.30 5.43 7.00 Table 2: Selected d-spacing (Å) and relative intensity (%) of the X-ray diffractogram for the Colleges in MOUAU are presented in Table 2. d1 Å(%) 3.33517 (100.00%) 3.33960 (100.00%) 3.33223(100.00%) 3.33898 (100.00%) 3.33536 (100.00%) 3.33734 (100.00%) 3.32038 (100.00) 5 d2 Å(%) 4.23748 (68.70%) 4.24678(54.40%) 4.24132(19.05%) 4.24962(10.16 %) 4.24252 (20.87) 4.24724 (29.09%) 4.21452(21.62%) d3 Å(%) 1.81512 (15.24%) 1.81538(26.78%) 1.81497(8.05%) 1.81657(7.42%) 1.81559 (10.90) 1.81640 (11.22%) 1.81129(17.83%) College CAERSE CAFST CASAP CASE CMBB CNREM COLPAS Figure 2: X-ray diffractogram of soil from CAERSE, MOUAU Figure 3: X-ray diffractogram of soil from CAFST, MOUAU 6 F igure 4: X-ray diffractogram of soil from CASAP, MOUAU Figure 5: X-ray diffractogram of soil from CASE, MOUAU 7 Figure 6: X-ray diffractogram of soil from CMBB, MOUAU Figure 7: X-ray diffractogram of soil from CNREM, MOUAU 8 Figure 8: X-ray diffractogram of soil from COLPAS, MOUAU Figure 9: The reference stick pattern from ICDDusing POWD-12++ 9 The pH analysis (Table 1) of the soil showed that CAERSE, CASE, CMBB and CNREM soils are acidic; CAFST and COLPAS are neutral while CASAP is mildly alkaline. Acidic loving crops would flourish in the acidic soils. Some of the acidic loving crops are sweet potatoes, peppers, potatoes, beans, cabbage, carrots, cucumbers, onions, sweet corn, tomatoes and grapes11. The soil texture (Table 1) showed that MOUAU soil is a sandy soil. The d-spacings and relative intensities of the X-ray diffraction pattern (Table 2) for the various colleges compare well the d-spacing in the reference stick pattern for quartz SiO2 3.342 Å (100.00%), 4.257 Å (22.00%), 1.8178 Å(14.00%). Other d-spacing values of the diffractogram compare well with the reference stick pattern. The identification of quartz with hexagonal Crystal system, space group P3221, a (Å): 4.9141, b (Å): 4.9141, c (Å): 5.4060, alpha(°):90.0000, beta (°): 90.0000 ,gamma (°):120.0000, volume of cell (10^6 pm^3):113.10 , Z: 3.00 and RIR: 3.06 10 have been suggested. The occurrences of quartz have been reviewed recently1. Quartz is an abundant mineral in igneous, metamorphic, hydrothermal, and sedimentary environments. In plutonic igneous rocks, it is abundant in silicic rocks ranging in composition from quartz diorite to granite but absent in more mafic compositions. In volcanic rocks, it is common in quartz latites to rhyolites, but uncommon in vitric silicic tuffs. It is common to abundant in welded silicic tuffs. In metamorphic rocks, it is abundant in schists and gneisses of pelitic to granitic compositions. In hydrothermal rocks, it is an abundant as the principal gangue mineral; in low to high temperature vein deposits. Because of its resistance to chemical weathering, it is the principal mineral phase in sandstones and abundant in other non-marine sedimentary rocks. It is also abundant as cryptocrystalline chert in marine limestones and dolomites. 10 Numerous varieties have been described, and defined mainly on color. Quartz is most commonly colorless and transparent. Rose quartz is pink and contains minor Mn impurities, recently identified as dumortrierite 2. Citrine is yellow, and amethyst is purple. CONCLUSION The pH of soils in MOUAU is acidic. This will favor acid loving crops. The soil texture is sandy. X-ray diffraction pattern of MOUAU soil sediments showed that it contains quartz mineral. The discovery of quartz in MOUAU is of enormous economic importance. Extraction of Quartz in MOUAU is hereby recommended. REFERENCES 1. Gaines RV, Skinner HCW, Foord EE, Mason B, Rosenzweig A, King VT, Dowty E Dana's New Mineralogy, Eighth Edition, New York, John Wiley & Sons, 1997; 1819. 2. Smyth JR, Quartz, Adopt-a-Mineral Project Example Paper, 2000; 2 3. Trostel LJ, Wynne DJ, Determination of quartz (free silica) in refractory clays, J. Am. Ceram. Soc. 1940; 23. 4. Kiely PV, Jackson ML,. (1965) Quartz, feldspar and mica determination for soils by sodium pyrosulfate fusion. Soil Sci. Soc Proc.,1965; 29: 159 – 163. 5. Legrand C, Nicolas, J, Contribution a l’etude du dodage du quartz dans les argiles a laide des rayons, X Bull. Soc. Fr. Ceram.,1958; 38: 29 – 41. 6. Till R, Spears DA, The determination of quartz in sedimentary rocks using an X-ray diffraction method. Clay and Clay Miner. 1969; 17: 323 – 327. 7. Hardy M, Eimberck M, Do Dihn T, Jamagne M, Clay mineralogy of grey degraded soils from the red River basin(Vietnam) and its influence on their properties. Proc. 14th Int. Conf. Soil Sci., Kyoto VII,1990; 28 – 33. 11 8. Amos-Uhegbu C, An investigation to determine the suitability of the Groundwater of Aba Metropolis for Agricultural purposes. Archives of Applied Science Research,2012;,4(5):2027-2033 9. Bouyoucos GJ, Hydrometer method improved for making particle size analysis of soils. Agron. J., 1962; 54: 464 - 465. 10. URL:http://www.webmineral.com/data/Quartz.shtml-17th October 2009 11. URL:http//www.gardeningknowhow.com/22nd -July 2014 12