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Mineralogical Characterization of Riebeckite from Alinci, Republic of Macedonia

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Mineralogical Characterization of Riebeckite from Alinci, Republic of Macedonia 337 Geologica Macedonica, Vol. 32, No. 1, pp. 75–87 (2018) GEOME 2 In print: ISSN 0352 – 1206 Manuscript received: February 1, 2018 On line: ISSN 1857 – 8586 Accepted: May 7, 2018 UDC: 552.4:[548.734.3:549.643.32 Original scientific paper MINERALOGICAL CHARACTERIZATION OF RIEBECKITE FROM ALINCI, REPUBLIC OF MACEDONIA Tena Šijakova-Ivanova1, Lidija Robeva-Čukovska2, Filip Jovanovski1, Stevan Kareski1 1Faculty of Natural and Technical Sciences, “Goce Delčev” University in Štip, Blvd. Goce Delčev 89, 2000 Štip, Republic of Macedonia 2National Conservation Centre – Skopje, Republic of Macedonia [email protected] A b s t r a c t: In this paper are presented the preliminary mineralogical characterization of riebeckite from Alinci, Republic of Macedonia. Several crystals of riebeckite were collected for research. The following three methods were used for the examination: scanning electron microscopy (SEM), coupled with energy dispersive X-ray spectrometer (EDS), X-ray powder difraction (XRD) and Fourier Transform Infrared Spectroscopy using Diffuse Reflectance method (FTIR/DRS). With these methods was established that the investigated mineral is riebeckite. Riebeckite from Alinci appears in needle crystals with dark green-black colour, vitreous luster and greenish brown streak. The concen- tration of elements in riebeckite crystals is: Na (2.97–4.94%), Mg (4.89–6.96%), Fe (10.83–27.21%), Si (21.90– 26.42%), Ca (0.89–4.38%). The Fe/Mg ratio is from 1.8 to 3.8. Riebeckite (with Fe/Mg >> 1) is common mineral in alkaline granites and syenites. In alkaline granites and syenites, a continuous series exists between arfvedsonite and the riebeckite. Оuter surface of riebeckite is covered with the crust various thickness and width. In this crust concentration of elements is: P (0.60–15.22), Mg (0.58–5.14%), Fe(4.98–13.13%), Si (3.50–25.39%), Ca (0.59–1.63%), Al (0.73– 17.33%), Ti (0.12–0.40%). There is proportional dependence between phosphorus and silicon in riebeckite crystals and crust. In the crust content of phosphorus increases, while the content of silicon decreases. Fine-grained phosphates are formed by superficial alteration processes. The nucleation and crystallization of Al and Fe phosphate phases are directly from aqueous solutions. Al and Fe phosphate phases readily precipitate from supersaturated solutions. This crust is likely a result of surface chemical reaction through altered surface layers and riebeckites dissolution at Earth surface temperatures. The most intense registered maxima in the studied powder pattern [d values (in Å), I, (hkl)] are: 8.44 (100), 3.12 (51), 2.80 (17), 3.14 (10), 3.27 (10), 2.71 (5), 4.20 (4), 1.65 (4), 3.25 (3). Key words: riebeckite; X-ray powder diffraction; scanning electron microscopy; Fourier transform infrared spectroscopy INTRODUCTION The Alinci locality is situated 11 km south- Texture is massive. They are composed of feldspar, west of Prilep. It covers an area of 4 km2 and is built quartz, amphibole, pyroxene, sphene and apatite. up of gneisses, syenites, marbles and schists (Figure So far, investigations on this locality are 1). The first data on geological research at the mostly related to the geology of the locality and is locality Alinci are given by Kossmat (1924) and given a description of only certain minerals among Protić (1959). Bermanec (1992) examines the which is not the mineral riеbeckite. Chukanov mineral monazite and sennait from this locality. (2013) give infrared spectra of magnesioriebeckite Syenite is present as a magmatic body length 3 from Alinci and Nežilovo. With our investigation in km and width 2 km. Syenite body has a fine-grained these syenites we found small lens bodies with structure and a massive texture. Fine grained sye- pegmatite structure and coarse grains of microcline nites are grayish white. They are composed of mic- and quartz in which are present crystals of mineral rocline, albite, quartz, arfvedsonite, augite, aegirine, that looked like such as riebeckite. biotite, sphene, apatite and zircon. Also are found For this purpose we took out several repre- coarse grains of syenite. Coarsely grain syenites are sentative samples from this mineral for examina- also compact, hard with green-white colour. tion. 76 T. Šijakova-Ivanova, L. Robeva-Čukovska, F. Jovanovski, S. Kareski 1. 2. 3. 4. 5. 6. 7. 8. 9. Legend: 1. proluvium; 2. diluvium; 3, syenite; 4. granodiorite; 5. marble; 6. metamorphosed diabases; 7. graphite schist; 8. albite gneiss; 9. gneiss Fig. 1. Geological map of locality Alinci 1:100 000 (M. Karajanović, T. Ivanovski, 1964–1972) ANALYTICAL METHODS For our research were used the following three IRPrestige 21 spectrophotometer (Shimadzu, methods: Fourier Transform Infrared Spectroscopy Japan), capable of Diffuse Reflectance Spectros- using Diffuse Reflectance method (FTIR/DRS), copy (DRS), was employed in this study. The DRS scanning electron microscopy (SEM), coupled with analyses were performed by using a DRS-8000 at- energy dispersive X-ray spectrometer (EDS) and X- tachment (Shimadzu). About 1 mg of the pow- der- ray diffraction (XRD). ed samples were diluted to about 5 % by weight in The use of these three methods showed that dry KBr and then placed into a sample cup (2 mm they are very useful methods for rapid mineral ana- diameter; 1 mm depth) which is a component of the lysis contributing important analytical information. DRS equipment. The spectra was recorded in the Geologica Macedonica, 32, 1, 75–87 (2018) Mineralogical characterization of riebeckite from Alinci, Republic of Macedonia 77 spectral range 400–4000 cm–1 at a resolution of possesses adequate accuracy to obtain stoichio- 4 cm–1 with 62 scans. For spectra manipulation was metric mineral from atomic ratios of constituent el- used IR Solution 1.5 software (Shimadzu Corpora- ements and identify analyzed mineral phases. tion). X-ray powder diffraction (XRD) is a rapid SEM is model VEGA3LMU, increasing 2× analytical technique primarily used for phase iden- 1000 000, W-wire, voltage up 200 V to 20 kV, in- tification of a crystalline material. The analyzed ma- frared camera, maximum sample size 81 mm height, terial is finely ground, homogenized, and average 30 mm width. The standards used are as follows: O: bulk composition is determined. X-ray researches SiO2; Na: albite; Mg: MgO; Al: Al2O3; Si: SiO2; P: were performed using an XRD-6100 Diffractometer GaP; Ca: wollastonite; Ti: Ti; Fe: Fe; Br: KBr. (Shimadzu) with X-ray Cu (1.54060 Ǻ) radiation Results of SEM/EDS analyses of mineral pha- operating at 40 kV and 30 mA. The powdered samp- ses demonstrated usefulness of this method for iden- les were scanned over the 5–80° range with step size tification and characterization of mineral phases of 0.02° and scanning speed of 1.2°/min. The most whose size is often below the resolution of an opti- intense registered maxima in the studied powder cal microscope. diagrams were compared with the corresponding diagrams from PDF-2 software. According to semi-quantitative results of SEM /EDS analyses, it can be concluded that SEM/EDS RESULTS AND DISCUSSION The name “riebeckite” was first used by Sauer x-ray data is given by Borg (1967) for eleven analy- 2+ 3+ (1888) when describing a blackish amphibole col- zed alkali amphiboles [Na2(Mg, Fe )3(Al, Fe )2 lected in Socotra (Yemen) by Dr. E. Riebeck. Si8O22(OH)2]. Riebeckite is mineral of the amphibole (alkali) gro- Complete physical, chemical and crystallo- 2 up. The ideal formula of riebeckite is [Na2] [Fe3 ] graphic data on a single sample are missing in the Si8O22(OH)2 (Palache, 1951; Burke and Lake, 2004; literature. Hawthorne, 2012). The first refinements of the crys- Riebeckite from Alinci usually appears in very tal structures of magnesio-riebeckite and riebeckite elongated prismatic fibrous or radial fibrous aggre- were done by Whittaker (1949) and Colville and gates (Figures 2 and 3). Riebeckite is with dark Gibbs (1964), respectively. Oberti et al. (2017) green-black colour, vitreous luster and greenish reported some unique peculiarities in riebeckite at brown streek. high temperature. A complete set of new optical and Fig. 2. Crystals of riebeckite from Alinci locality, Fig. 3. Crystals of riebeckite from Alinci locality, Republic of Macedonia Republic of Macedonia Geologica Macedonica, 32, 1, 75–87 (2018) 78 T. Šijakova-Ivanova, L. Robeva-Čukovska, F. Jovanovski, S. Kareski The infrared spectrum of the analyzed sample scopy (Figure 4b). The second derivative profile of is given in Figure 4. In order to achieve resolution the original spectrum reveals a series of resolved enhancement of the original absorption spectrum bands which could not be assigned in a straight-for- (Figure 4a) we used the second derivative spectro- ward manner. Fig. 4. (a) Infrared spectrum of the analyzed sample. (b) Second derivative profile (inverted curve) The spectra inspection led to following assess- Тhe chemical properties of the riebeckite are ments: given by Murgoci (1906), Miayshiro (1957) and – The hydroxyl stretching region exhibits a Deer et al. (1963). Oberti et al. (2018) give crystal- series of four bands at 3664, 3651, 3635 and 3616 chemical characterization of magnesio-riebeckite. cm–1 assigned to MOH vibrations. The strong ab- Riebeckite is found in a wide variety of para- sorptions observed at 3030–3400 cm–1 is due to OH genesess. It is a common constituent of alkalic stretching vibrations of water, while the band at granites and syenites (Borley, 1963; Lyons, 1972, around 1650 cm–1 corresponds to the bending mode. 1976). Distinct compositional differences occur – The IR spectrum shows complexity in the between riebeckites from different parageneses. region at about 1100 to 900 cm–1, with several over Тhe results for the chemical composition of the lapping bands. This region is attributable to the anti- riebeckite from the Alinci obtained by SEM-EDS symmetric stretching modes of Si–O–Si (Makreski, for sample 1 are given in the Figures 5–8 and Table 2006; Jovanovski, 2009; Apopei, 2011), but also it 2.
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