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Application of an Internal Standard Technique by Transmission X-Ray Diffraction to Assess Layer Charge of a Montmorillonite by Using the Alkylammonium Method

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Clays and Clay Minerals

Abstract

Transmission X-ray diffraction (XRD) of C6–16 alkylammonium ion-exchanged montmorillonite SAz-1 with Ag-behenate as an internal standard provided accurate estimates of d(001) values of the alkylammonium ion-exchanged montmorillonite. Inspection of d(001) values were made to assess the possible formation of gauche conformers (alternate arrangements of the molecules) in the interlayer and to determine the critical carbon chain length, nC. Using conventional constraints for nC(I′) and nC(II) equal to 1.36 and 1.77 nm, respectively, provided ambiguous nC(I′) and nC(II) values. The dependence of full-width at half-maximum values on nC allowed better estimates of nC(I′) and nC(II) because “integral” and “non-integral” peak characteristics relating to interstratification could be included in the assessment.

The effect of inaccurate estimates of nC(I′) and nC(II) values on calculated interlayer cation exchange capacity (Ci) using two conventional concepts of calculation were compared. It was found that a procedure based on the summation of fractions of the layer charge gave relative errors of Ci <2%, even where the number of carbon atoms corresponding to both nC(I′) and nC(II) differed by ± 1 nC from the correct values. This method of calculation of Ci is recommended when reliable values of Ci are needed.

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References

  • Beneke, K. and Lagaly, G. (1982) The brittle mica-like KniAsO4 and its organic derivates. Clay Minerals, 17, 175–183.

    Article  Google Scholar 

  • Blanton, T.N., Huang, T.C., Toraya, H., Hubbard, C.R., Robie, S.B., Louër, D., Göbel, H.E., Will, G., Giles, R., and Raftery, T. (1995) JCPDS-International Centre for Diffraction Data round robin study of silver behenate. A possible low-angle X-ray diffraction calibration standard. Powder Diffraction, 10, 91–95.

    Article  Google Scholar 

  • Číčel, B. and Komadel, P. (1994) Structural formulae of layer silicates. In Soil Science Society of America Miscellaneous Publication, Quanitative Methods in Soil Mineralogy, J.E. Amoneet and L.W. Zelazny, eds., Madison, Wisconsin, 114–136.

    Google Scholar 

  • Hall, M.M., Veeraraghavan, V.G., Rubin, H., and Winchell, P.G. (1977) The approximation of symmetric X-ray peaks by Pearson type VII distributions. Journal of Applied Crystallography, 10, 66–68.

    Article  Google Scholar 

  • Janek, M., Komadel, P., and Lagaly, G. (1997) Effect of autotransformation on the layer charge of smectites determined by alkylammonium method. Clay Minerals, 32, 623–632.

    Article  Google Scholar 

  • Kelley, W.P. (1955) Interpretation of chemical analyses of clays. Clays and Clay Minerals, 1, 92–94.

    Article  Google Scholar 

  • Lagaly, G. (1981) Characterization of clays by organic compounds. Clay Minerals, 16, 1–21.

    Article  Google Scholar 

  • Lagaly, G. (1994) Layer charge determination by alkylammonium ions. In Clay Minerals Society Workshop Lectures 6, Layer Charge Characteristics of 2:1 Silicate Clay Minerals, A.R. Mermut, ed., Boulder, Colorado, 1–46.

    Google Scholar 

  • Lagaly, G. and Beneke, K. (1991) Intercalation and exchange reactions of clay minerals and non-clay layer compounds. Colloid Polymer Science, 269, 1198–1211.

    Article  Google Scholar 

  • Lagaly, G. and Weiss, A. (1969) Determination of the layer charge in mica-type layer silicates. Proceedings of the International Clay Conference, Tokyo, 1969, I, 61–80.

    Google Scholar 

  • Lagaly, G. and Weiss, A. (1971) Neue Methoden zur Char-akterisierung und Idenifizierung quellungsfàhiger Dreis-chichttonminerale. Zeitshcrift Pflanzenern Bodenkunde, 130, 9–24.

    Article  Google Scholar 

  • Lagaly, G. and Weiss, A. (1975) The layer charge of smectitic layer silicates. Proceedings of the International Clay Conference, Mexico. Applied Publishing Ltd, Wilmette, Illinois, 157–172.

    Google Scholar 

  • Lagaly, G., Fernandez Gonzales, M., and Weiss, A. (1976) Problems in layer-charge determination of montmorillon-ites. Clay Minerals, 11, 173–187.

    Article  Google Scholar 

  • Laird, D.A. (1994) Evaluation of structural formulae and alkylammonium method of determining layer charge. In Clay Minerals Society Workshop Lectures 6, Layer Charge Characteristics of 2: 1 Silicate Clay Minerals, A.R. Mermut, ed., Boulder, Colorado, 79–104.

    Google Scholar 

  • Laird, D.A., Scott, A.D., and Fenton, T.E. (1987) Interpretation of alkylammonium characterization of soil clays. Soil Science Society of America Journal, 51, 1659–1663.

    Article  Google Scholar 

  • Laird, D.A., Scott, A.D., and Fenton, T.E. (1989) Evaluation of the alkylammonium method of determining layer charge. Clays and Clay Minerals, 37, 41–46.

    Article  Google Scholar 

  • MacEwan, D.M.C., Ruiz Amil, A., and Brown, G. (1961) Interstratified clay minerals. In The X-ray Identification and Crystal Structures of Clay Minerals, G. Brown, ed., Mineralogical Society, London, 393–445.

    Google Scholar 

  • Maes, A., Stul, M.S., and Cremers, A. (1979) Layer charge—cation-exchange capacity relationships in montmorillonite. Clays and Clay Minerals, 27, 387–392.

    Article  Google Scholar 

  • Malla, P.B. and Lowell, A.D. (1987) Layer charge properties of smectites and vermiculites: Tetrahdral vs octahedral. Soil Science Society of America Journal, 51, 1362–1366.

    Article  Google Scholar 

  • Mermut, A.R. (1994) Problems associated with layer charge characterization of 2:1 phyllosilicates. In Clay Minerals Society Workshop Lectures 6, Layer Charge Characteristics of 2:1 Silicate Clay Minerals, A.R. Mermut, ed., Boulder, Colorado, 105–127.

    Google Scholar 

  • Reynolds, R.C. (1980) Interstratified clay minerals. In Crystal Structures of Clay Minerals and Their X-ray Identification, G.W. Brindley and G. Brown, eds., Mineralogical Society, London, 249–303.

    Google Scholar 

  • Ruehlicke, G. and Kohier, E.E. (1981) A simplified procedure for determining layer charge by the n-alkylammonium method. Clay Minerals, 16, 305–307.

    Article  Google Scholar 

  • Stanjek, H., Niederbudde, E.A., and Häusler, W. (1992) Improved evaluation of layer charge of n-alkylammonium-treated fine soil clays by Lorenz- and polarization-correction and curve-fitting. Clay Minerals, 27, 3–19.

    Article  Google Scholar 

  • Vaia, R.A., Teukolsky, R.K., and Giannelis, E.P. (1994) Interlayer structure and molecular environment of alkylam-monium layered silicates. Chemical Materials, 6, 1017–1022.

    Article  Google Scholar 

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Janek, M., Smrčok, L. Application of an Internal Standard Technique by Transmission X-Ray Diffraction to Assess Layer Charge of a Montmorillonite by Using the Alkylammonium Method. Clays Clay Miner. 47, 113–118 (1999). https://doi.org/10.1346/CCMN.1999.0470201

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  • DOI: https://doi.org/10.1346/CCMN.1999.0470201

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