Hostname: page-component-848d4c4894-p2v8j Total loading time: 0.001 Render date: 2024-06-01T22:37:23.524Z Has data issue: false hasContentIssue false
  • English
  • Français

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

Published online by Cambridge University Press:  28 February 2024

M. Janek  and
L’. Smrčok
M. Janek
Affiliation:
Institute of Organic Chemistry, Slovak Academy of Science, SK-842 36 Bratislava, Slovak Republic
L’. Smrčok
Affiliation:
Institute of Organic Chemistry, Slovak Academy of Science, SK-842 36 Bratislava, Slovak Republic
Get access Rights & Permissions [Opens in a new window]

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.

Keywords

Alkylammonium MethodInterlayer Cation Exchange CapacityLayer-Charge DeterminationMontmorilloniteSilver BehenateXRD
Type
Research Article
Information
Clays and Clay Minerals , Volume 47 , Issue 2 , April 1999 , pp. 113 - 118
Copyright
Copyright © 1999, The Clay Minerals Society

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Beneke, K. and Lagaly, G., 1982 The brittle mica-like KniAsO4 and its organic derivates Clay Minerals 17 175–183 10.1180/claymin.1982.017.2.02.CrossRefGoogle 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 10.1017/S0885715600014421.CrossRefGoogle Scholar
Číčel, B. Komadel, P., Amoneet, J.E. and Zelazny, L.W., 1994 Structural formulae of layer silicates Soil Science Society of America Miscellaneous Publication, Quanitative Methods in Soil Mineralogy 114–136.CrossRefGoogle 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 10.1107/S0021889877012849.CrossRefGoogle 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 10.1180/claymin.1997.032.4.12.CrossRefGoogle Scholar
Kelley, W.P., 1955 Interpretation of chemical analyses of clays Clays and Clay Minerals 1 92–94 10.1346/CCMN.1952.0010111.CrossRefGoogle Scholar
Lagaly, G., 1981 Characterization of clays by organic compounds Clay Minerals 16 1–21 10.1180/claymin.1981.016.1.01.CrossRefGoogle Scholar
Lagaly, G. and Mermut, A.R., 1994 Layer charge determination by alkylammonium ions Clay Minerals Society Workshop Lectures 6, Layer Charge Characteristics of 2:1 Silicate Clay Minerals .CrossRefGoogle 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 10.1007/BF00652529.CrossRefGoogle 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 10.1002/jpln.19711300103.CrossRefGoogle Scholar
Lagaly, G. and Weiss, A., 1975 The layer charge of smectitic layer silicates Proceedings of the International Clay Conference, Mexico. Wilmette, Illinois Applied Publishing Ltd 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 10.1180/claymin.1976.011.3.01.CrossRefGoogle Scholar
Laird, D.A. and Mermut, A.R., 1994 Evaluation of structural formulae and alkylammonium method of determining layer charge Clay Minerals Society Workshop Lectures 6, Layer Charge Characteristics of 2: 1 Silicate Clay Minerals 79–104.CrossRefGoogle 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 10.2136/sssaj1987.03615995005100060046x.CrossRefGoogle 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 10.1346/CCMN.1989.0370105.CrossRefGoogle Scholar
MacEwan, D.M.C. Ruiz Amil, A. Brown, G. and Brown, G., 1961 Interstratified clay minerals The X-ray Identification and Crystal Structures of Clay Minerals London Mineralogical Society 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 10.1346/CCMN.1979.0270510.CrossRefGoogle 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 10.2136/sssaj1987.03615995005100050048x.CrossRefGoogle Scholar
Mermut, A.R. and Mermut, A.R., 1994 Problems associated with layer charge characterization of 2:1 phyllosilicates Clay Minerals Society Workshop Lectures 6, Layer Charge Characteristics of 2:1 Silicate Clay Minerals Colorado Boulder 105–127.Google Scholar
Reynolds, R.C., Brindley, G.W. and Brown, G., 1980 Interstratified clay minerals Crystal Structures of Clay Minerals and Their X-ray Identification London Mineralogical Society 249–303.CrossRefGoogle 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 10.1180/claymin.1981.016.3.08.CrossRefGoogle 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 10.1180/claymin.1992.027.1.02.CrossRefGoogle 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 10.1021/cm00043a025.CrossRefGoogle Scholar