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Behaviour of Indian Natural Baryte Mineral

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Behaviour of Indian Natural Baryte Mineral International Journal of ChemTech Research CODEN( USA): IJCRGG ISSN : 0974-4290 Vol.5, No.1, pp 220-231, Jan-Mar 2013 Behaviour of Indian natural Baryte mineral B. Prameena3, G. Anbalagan1*, V. Sangeetha2, S. Gunasekaran3 and G.R. Ramkumaar3 1PG and Research Department of Physics, presidency college, TN, Chennai-600005, India 2Department of Physics, DG VaishnavCollege, T N, Chennai – 600106, India 3PG and Research Department of Physics, pachaiyappa’s college, TN, Chennai-600030, India *Corres. Author: [email protected] Abstract: The mineral Baryte has been investigated by X-ray diffraction, infrared, optical absorption and Thermo gravimetric analysis (TGA) studies. In X-ray diffraction, structure has been determined as orthorhombic. In FTIR the fundamental stretching and bending vibrations observed in the infrared region for Ba and SO4.The optical absorption shows the presence of Fe in the mineral. EPR results in the presence of iron and presence of manganese in the mineral. The thermal decomposition behaviour was determined by means of thermogravimetric analysis (TGA) at different heating rates in nitrogen. The activation energies of the thermal degradation were calculated by four different methods: Coats-Redfern, Flynn-Wall, Kissinger, and Kim-Park. The Flynn-Wall and Kim-Park methods were the most suitable methods to calculate the activation energy. Keywords : X-ray powder diffraction; FTIR, thermogravimetric analysis (TGA); Baryte. 1. Introduction has been studied in the range 1µ to25µ using ten different specimen, belonging to 001 and 110 Baryte, or baryte, (BaSO4) is a mineral sections. The extension of the range of study beyond consisting of barium sulfate(1). The baryte group 16 has revealed the presence of fundamentals at consists of baryte, celestine, anglesite and anhydrite. 21.3µ (470 cm-1) and 22.8µ (439 cm-1) besides other Baryte itself is generally white or colourless, and is absorption maxima. Also the laser induced, time- the main source of barium. Baryte and celestine resolved luminescence technique is a suitable tool form a solid solution (Ba,Sr)SO4(2). Baryte is a for the identification of rare-earths in baryte and the sulfate of barium with chemical formula, BaSO4 discrimination of their oxidation states. Along with (BaO 65.7% and SO3 34.3%). Barytes contains little the common Eu2+ luminescence, the emission of or no soluble salts and is insoluble in water and acid. Eu3+was detected for the first time in baryte. There Pure barytes is white opaque to transparent but are at least two structural positions for Eu3+ in baryte impurities cause a wide variation in colour. It is crystal lattice. FTIR spectroscopy, can be used for chemically inert and has a high density. It the identification of constituent materials of Cultural crystallizes in normal class orthorhombic barytes Heritage as far as they provide information about type with rhombic dipyramidal symmetry. Its characteristic vibrational levels(3-9). Nevertheless, mainly used in oil industries, electronics, TV screen, not all transitions between vibrational molecular glass, ceramics and medical applications. Its also levels are allowed. Some transitions can appear only used in car fillers and paint industry. Previously its in the infrared spectrum. The IR-or Raman-allowed been found that, the infrared absorption of barytes or forbidden transitions are determined by the G. Anbalagan et al /Int.J.ChemTech Res.2013,5(1) 221 selection rules. Molecules with low symmetry, most secondary optics, 45 kV voltage and 20 mZ current. of the vibrational modes appear in both the IR and The powdered sample was mounted on a quartz Raman spectra, but, normally, with very different support to minimize background. A Perikin-Elmer intensities, because the polarizability change for a Spectrum one FT-IR spectrometer was used, and the vibration (which is a required selection rule for samples were analyzed in KBr pellets. Spectra were Raman scattering) differs from the dipolar moment traced in the range 4000 – 400 cm-1, and the band change (a required selection rule for IR absorption) intensities were expressed in transmittance(%). for the vibration (10,11). Thus, the vibrational The optical absorption spectrum of the information obtained by IR spectroscopy (12). sample was recorded using Varian Cary 5E UV- Crystals commonly have tabular habit and some Visible-NIR spectrophotometer in the range 200 – have prismatic, columnar, and sometimes globular, 2500 nm by employing mull technique. massive, rosette, fibrous, and crystal forms. The EPR spectrumwas recorded on a Bruker details of baryte mineral are as shown in the Table 1. EMX Plus spectrometer with a Modulation Frequency of 100 kHz and 20 mW microwave 2. Experimental power. Thermal analysis were performed in a The Baryte mineral were ground with an simultaneous TG-DTA (Netzsch STA 409) agate mortar and pestle. The powdered sample was procedure. The temperature was increased from 30°- sieved, and the particles with diameter smaller than 1000° C, at heating rates of 5°, 10°, and 20° C/min. 50 micrometer were submitted to XRD, FTIR, UV Measurements were made in nitrogen atmosphere. and TGA studies. XRD analysis were Barytewas takenin the pellet state and the sample performed with a SEIFERT X-ray diffractometer weight was about 13mg. with Cu Kα radiation (λ=1.54 A), Cu filter on Table 1. The morphology of the baryte mineral Space Mineral Formula Cell constants Volume group a(Å) b(Å) c(Å) (Å)3 Baryte BaSO4 Pbnm Z = 4 8.886 ±0.026 5.479±0.025 7.203±0.049 350.74 Fig. 1X-ray Diffraction of baryte G. Anbalagan et al /Int.J.ChemTech Res.2013,5(1) 222 3. Results and discussion 3430 and 1650cm-1 (14). All the spectra of the studied bartyes sample are dominated by an intense 3.1 X-ray diffraction analysis ν1 band (symmetric stretching of SO4tetrahedra) at The room temperature powder X-ray 982 cm-1 for bartye. ADLEER & KERR (1965) (15) diffraction pattern of the baryte is given in Fig. 1 found spectral shifts of the stretching modes (ν3 and which shows quite sharp peaks with little ν4) to lower frequencies with increasing cation mass, background absorption. The presence of principal such as the case of substitution Ba for Sr. The FTIR reflections at the d-spacings4.4320, 3.9079, 3.4476, studies support the suggestion that the baryte contain 3.3285, 3.1126, 2.7399, 2.4992, 2.2231, 2.0697 Å -1 traces of calcite ν1(1083 cm ), which coincides with indicates the presence of barytes and these readings -1 ν3 of the SO4 group and ν4(634cm ) bands. The free are compared with JCPDS file No. 72-1390. It has SO4 molecule belongs to the Td symmetry. an orthorhombic structure (pbnm), where S situated Corresponding to each of the vibration of the free in tetrahedral coordination with O and Ba is SO4 molecule, one expects to find the number of surrounded by 12 oxygen’s of 7 SO4 tetrahedra(13). vibrations in the crystalline state. The number and The BaO12 polyhedral and the SO4tetrahedral are their respective symmetry properties can be found edge-bound. The BaO12polyhedral are irregular; six out according to the procedure outlined by Couture of the Ba-O distances are 2.77-281 Å, and the other and Mathieu (16). The effect of the crystalline state 6 – 2.91 – 3.32 Å, which suggests a “sheet” structure on the free SO oscillation is two-fold. The parallel to {001}. 4 symmetry of a single SO4 molecule is changed from the tetrahedral group Td to the monoclinic local 3.2 FTIR spectral analysis symmetry Cs, lifting the degeneracies of the doubly The FTIR spectrum of baryte are shown in and triply degenerate oscillations in this manner the Fig. 2. The sulfate group has 4 fundamental four fundamentals of the free SO4 molecule give vibrational modes: one non-degenerate mode (ν1), nine fundamentals. Table 2 is band component one doubly degenerate mode (ν2), two triply analysis of the IR of baryte. The infrared (IR) degenerate mode(ν3and ν4). The IR spectrum of spectra of baryte from different occurrences are baryte exhibits several significance bands.Two characterized by relatively weak but strongly strong bands corresponding to asymmetric stretching pleochroic absorption bands at 3435 and 2923 cm−1. and bending(ν3 and ν4) and two weak ones These bands are assigned to anti-symmetric and corresponding to symmetric stretching and symmetric OH stretching vibrations of two types of bending(ν1 and ν2). Only one reference reports the H O molecules localized on vacant Ba sites. presence of water in the IR spectrum of baryte at 2 Fig.2 FTIR spectrum of baryte G. Anbalagan et al /Int.J.ChemTech Res.2013,5(1) 223 Table 2. FTIR Assignments of baryte Sl.No. IR Assignment 1 3435 ν3OH 2 2923 ν3OH 3 1623 ν3 SO4 4 1179 ν3 SO4 5 1083 ν1 SO4 6 982 ν1 SO4 7 634 ν4 SO4 8 610 ν4 SO4 one nondegenerate mode (ν1) one doubly degenerate mode (ν2) two triply degenerate mode(ν3and ν4) Fig. 3 Optical absorption of baryte 3.3 Optical absorption spectrum (1954)(23) diagram of d5 configuration. From the 6 4 4 6 4 4 The optical absorption spectrum (Fig. 3) A1→ T1( G), A1→ T2( G) transition energies and exhibits features similar to those of Fe2+ and Fe3+ the Tanabe-Sugano equations (17), the ligand field impurities in different iron bearing minerals (17-20). theory parameters Dq, B and C are calculated. There are six bands observed in the spectrum and all 3.3.2 Fe2+ ion are attributed to different transitions arising from Crystal field theory predicts that a d6 ion in isolated Fe2+ and Fe3+ as well as by pairs of iron an octahedral site will produce a single absorption ions.
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