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X-ray diffraction, infrared and TGA/DTG analysis of hydrated nacrite

Published online by Cambridge University Press:  09 July 2018

A. Ben Haj Amara*
Affiliation:
L.P.M., Faculté des Sciences de Bizerte, 7021 Zarzouna, Bizerte, Tunisia

Abstract

An homogenous 8.4 Å hydrate was obtained after washing intercalated KAc- nacrite. X-ray diffraction analysis based on comparison of the experimental and calculated profiles enabled the amount of water (one molecule per Si2Al2O5(OH)4) and the z coordinate along c* (6.5 Å) to be determined. The hydration state was accompanied by a decrease in the coherent domain along c* in the order nacrite > KAc-nacrite > H2O-nacrite. The IR spectrum of the hydrated nacrite showed an evolution of the structure with a shift of ν(OH) from 3702, 3649 and 3630 cm−1 to 3690, 3641 and 3620 cm−1, respectively for the nacrite hydroxyls. The ν(OH) stretching bands of the interlayer water appeared at 3602 and 3545 cm−1 and their bending band at 1655 cm−1. The TGA/DTG analysis of the air-dry hydrated nacrite showed a loss of water at 245°C the weight loss (1 molecule per Si2Al2O5(OH)4) corresponding to the interlamellar water, in agreement with that determined by XRD.

Type
Research Article
Copyright
Copyright © The Mineralogical Society of Great Britain and Ireland 1997

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References

Bellamy, L.J. & Owen, A. (1969) A simple relationship between the infrared stretching frequencies and the hydrogen bond distances in crystals. Spectrochim. Acta, 25, 329333.Google Scholar
Ben Brahim, J., Armagan, N., Besson, G. & Tchoubar, C. (1983) X-ray diffraction studies on the arrangement of water molecules in a smectite. I- Homogeneous two-water-layer Na beidellite. J. Appl. Cryst. 16, 264269.Google Scholar
Ben Haj Amara, A., Ben Brahim, J., Ben Ayed, N. & Ben Rhaiem, H. (1995) Présence de la nacrite dans des anciens gisements de Pb-Zn. Clay Miner. 31, 113117.Google Scholar
Costanzo, P.M. & Giese, R.F. (1990) Ordered and disordered organic intercalates of 8.4-Å synthetically hydrated kaolinite. Clays Clay Miner. 38, 160170.Google Scholar
Costanzo, P.M., Clemency C+V. & Giese, R.F. (1980) Low-temperature synthesis of a 10-Å hydrate of kaolinite using dimethylsulfoxide and ammonium fluoride. Clays Clay Miner. 28, 155156.Google Scholar
Costanzo, P.M., Giese, R.F. & Clemency, C.V. (1984a) Synthesis of a 10-Å hydrated kaolinite. Clays Clay Miner. 32, 2935.Google Scholar
Costanzo, P.M., Giese, R.F. & Lipsicas, M. (1984b) Static and dynamic structure water in hydrated kaolinite. IThe static structure. Clays Clay Miner. 32, 419428.Google Scholar
Costanzo, P.M., Giese, R.F., Lipsicas, M. & Straley, C. (1982) Synthesis of a quasi-stable kaolinite and heat capacity of interlayer water. Nature 296, 549–551.Google Scholar
Deeds, C.T., van Olphen, H. & Bradley, W.F. (1966) Intersalation and interlayer hydration of minerals of the kaolinite group. Proc. Int. Clay Conf. Jerusalem, 2, 183199.Google Scholar
Drits, V.A. & Tchoubar, C. (1990) The modelization method in the determination of the structural characteristics of some layer silicates: internal structure of the layers, nature and distribution of stacking faults. Pp. 233–303 in: X-ray Diffraction by Disordered Lamellar Structures, Springer-Verlag, Berlin.Google Scholar
Farmer, V.C. (1974) The layer silicates. Pp. 331-363 in: The Infrared Spectra ∼f Minerals (Farmer, V.C., editor). Mineralogical Society, London.Google Scholar
Hall, P.L., Harisson, R., Hayes, M.H.B. & Tuck, J.J. (1983) Particle orientation distributions and stacking arrangements in size-fractionated montmorillonite measured by neutron and X-ray diffraction. J. Chem. Soc. Faraday Trans. 79, 16871700.Google Scholar
Lippman, F. (1970) Functions describing preferred orientation in flat aggregates of flake-like clay minerals and in other axially symmetric fabrics. Contrib. Mineral. Pet. 25, 7794.Google Scholar
Lipsicas, M., Straley, C., Costanzo, P.M. & Giese, R.F. (1985) Static and dynamic structure of water in hydrated kaolinite - Part. II. Dynamic structure. J. Colloid Interf Sci. 107, 221230.Google Scholar
Raythatha, R. & Lipsicas, M. (1985) Mechanism of synthesis of 10-Å hydrated kaolinite. Clays Clay Miner. 33, 333339.Google Scholar
Reynolds, R.C. (1968) The effect of particle size on apparent lattice spacings. Acta Cryst. 24, 319–320.Google Scholar
Reynolds, R.C. (1986) The Lorentz-polarization factor and preferred orientation in oriented clay aggregates. Clays Clay Miner. 34, 359367.Google Scholar
Ross, M. (1968) X-ray diffraction effects by non ideal crystals of biotite, muscovite, montmorillonite. Z. Kristallogr. Kristallogem. 126, 8097.Google Scholar
Tarasevich, Y.I. & Gribina, I.A. (1972) Infrared spectroscopic study of the state of water in halloysite. Kolloidnyi Zh. 34, 405411 (in Russian).Google Scholar
Taylor, R.M. & Norrish, K. (1966) The measurement of orientation distribution and its application to quantitative X-ray diffraction analysis. Clay Miner. 6, 127141.CrossRefGoogle Scholar
Tettenhorst, R. & Robertson, H.F. (1973) X-ray diffraction aspects of montmorillonite. Am. Miner. 58, 7380.Google Scholar
Tunney, J. & Detellier, C. (1994) Preparation and characterization of an 8.4 A hydrate of kaolinite. Clays Clay Miner. 42, 473476.Google Scholar
Wada, K. (1965) Intercalation of water in kaolin minerals. Am. Miner. 50, 924–941.Google Scholar
Wiewiora, A. & Brindley, G.W. (1969) Potassium acetate intercalation in kaolinite and its removal: effect of material characteristics. Proc. Int. Clay Conf Tokyo, 1, 723733.Google Scholar
Zheng, H. & Bailey, S.W. (1994) Refinement of the nacrite structure. Clays Clay Miner. 42, 46–52.Google Scholar