Hostname: page-component-cd9895bd7-p9bg8 Total loading time: 0 Render date: 2024-12-27T11:08:16.266Z Has data issue: false hasContentIssue false
  • English
  • Français

Quantification of Crystalline and Noncrystalline Material in Ground Kaolinite by X-Ray Powder Diffraction, Infrared, Solid-State Nuclear Magnetic Resonance, and Chemical-Dissolution Analyses

Published online by Cambridge University Press:  02 April 2024

Hideomi Kodama ,
Luba S. Kotlyar  and
John A. Ripmeester
Hideomi Kodama
Affiliation:
Land Resource Research Centre, Research Branch, Agriculture Canada, Ottawa, Ontario K1A 0C6, Canada
Luba S. Kotlyar
Affiliation:
National Research Council of Canada, Division of Chemistry, M-12 Montreal Road, Ottawa, Ontario K1A 0R9, Canada
John A. Ripmeester
Affiliation:
National Research Council of Canada, Division of Chemistry, M-12 Montreal Road, Ottawa, Ontario K1A 0R9, Canada
Rights & Permissions [Opens in a new window]

Abstract

Core share and HTML view are not available for this content. However, as you have access to this content, a full PDF is available via the ‘Save PDF’ action button.

The capabilities of X-ray powder diffraction (XRD), infrared absorption (IR), solid-state magicangle-spinning nuclear magnetic resonance (MAS-NMR), and chemical dissolution methods were assessed for estimating the amount of noncrystalline material in a ground kaolinite. The Georgia kaolinite was ground in a mechanical mortar for various lengths of time to produce a set of ground samples containing different amounts of the resulting noncrystalline material. In the XRD method, the intensities of characteristic reflections at 7.2 and 4.47 Å did not respond proportionally to the amount of crystalline kaolinite. Although a transmission-type X-ray diffraction method using the hk reflection gave a slightly better estimate than the reflection-type X-ray diffraction method using the basal reflection, both methods gave overestimated values for the amount of noncrystalline material. This overestimation may have been caused by a masking effect due to coaggregation. Using the characteristic IR absorption band at 3700 cm-1 underestimated the amount of the noncrystalline material, if the proportion of this material <50%.

Extraction with NaOH gave estimations 15 to 20% greater than extraction with alkaline Tiron, except for the sample ground for 24 hr, for which both extractions indicated the presence of about 50% noncrystalline material. X-ray powder diffraction data of the residues after these extractions indicated that they consisted of crystalline kaolinite. 29Si NMR spectra of samples ground for ≥ 30 hr suggested that SiO4 tetrahedra were considerably distorted.27 Al NMR spectra showed a signal for tetrahedral A1 for the sample ground for 10 hr, which increased with an increase in grinding time. Plots of the Al(IV)/[Al(IV) + Al(VI)] ratios vs. time were similar to those of chemical extraction curves. Inasmuch as extraction with hot 0.5 M NaOH is a rather harsh treatment, the composition of the noncrystalline material must have been similar to that of the crystalline kaolinite. The chemical dissolution using alkaline Tiron appeared to be superior to other methods, such as XRD, IR, and NaOH extraction, for estimating the amount of noncrystalline material in kaolinite.

Keywords

Chemical dissolutionDry grindingInfrared spectroscopyKaoliniteNoncrystallineNuclear magnetic resonanceX-ray powder diffraction
Type
Research Article
Information
Clays and Clay Minerals , Volume 37 , Issue 4 , August 1989 , pp. 364 - 370
Copyright
Copyright © 1989, The Clay Minerals Society

Footnotes

1

Land Resource Research Centre Contribution LRRC89-11, a joint contribution with National Research Council of Canada.

References

Biermans, V. and Baert, L., 1977 Selective exraction of the amorphous Al, Fe and Si oxides using an alkaline Tiron solution Clay Miner. 12 127 – 135.CrossRefGoogle Scholar
Brindley, G. W. and Nakahira, M., 1959 The kaolinitemullite reaction series: II. Metakaolin J. Amer. Ceram. Soc. 42 314 – 318.CrossRefGoogle Scholar
Freund, F. and Serratosa, J. M., 1973 The defect structure of metakaolinite Proc. Int. Clay Conf., Madrid, 1972 Madrid Division de Ciencias, C.S.I.C. 13 – 25.Google Scholar
Hashimoto, I., Jackson, M. L. and Swineford, A., 1960 Rapid dissolution of allophane and kaolinite-halloysite after dehydration Clays and Clay Minerals, Proc. 7th Natl. Conf., Washington, D.C., 1958 New York Pergamon Press 102 – 113.Google Scholar
Kinsey, R. A., Kirkpatrick, R. J., Hower, J., Smith, K. A. and Oldfield, E., 1985 High resolution aluminum-27 and silicon-29 nuclear magnetic resonance spectroscopic study of layer silicates, including clay minerals Amer. Mineral. 70 537 – 548.Google Scholar
Kodama, H., Jaakkimainen, M., van Olphen, H. and Veniale, F., 1982 A comparative study of selective chemical dissolution methods for separating noncrystalline components produced by grinding of silicates Proc. Int. Clay Conf., Bologna, Pavia, 1981 Amsterdam Elsevier 399 – 410.Google Scholar
Kodama, H., Oinuma, K. and Bradley, W. F., 1963 Identification of kaolin minerals in the presence of chlorite by X-ray diffraction and infrared absorption spectra Clays and Clay Minerals, Proc. 11th Natl. Conf., Ottawa, Ontario, 1962 New York Pergamon Press 236 – 249.Google Scholar
Komameni, S., Fyfe, C. A. and Kennedy, G. J., 1985 Order-disorder in 1:1 type clay minerals by solid-state 27A1 and 29Si magic-angle spinning NMR spectroscopy Clay Miner. 20 327 – 334.CrossRefGoogle Scholar
Lippmaa, E., Magi, M., Samoson, A., Engelhardt, G. and Grimmer, A.-R., 1980 Structural studies of silicates by solid-state high-resolution 29Si NMR J. Amer. Chem. Soc. 102 4889 – 4893.CrossRefGoogle Scholar
Lippmaa, E., Magi, M., Sampson, A., Tarmak, M. and Engelhardt, G., 1981 Investigation of the structure of zeolites by solid-state high-resolution 29Si NMR spectroscopy J. Amer. Chem. Soc. 103 4992 – 4996.CrossRefGoogle Scholar
MacKenzie, K. J. D. Brown, I. W. N. Meinhold, R. H. and Bowden, M. E., 1985 Outstanding problems in the kaolin-mullite reaction sequence investigated by 29Si and27Al solid-state nuclear magnetic resonance: I. Metakaolinite J. Amer. Ceram. Soc. 68 293 – 297.CrossRefGoogle Scholar
Takahashi, H. and Swineford, A., 1959 Effect of dry grinding on kaolin minerals Clays and Clay Minerals, Proc. 6th Natl. Conf, Berkeley, California, 1957 New York Pergamon Press 279 – 291.Google Scholar
Wada, K., Dixon, J. B. and Weed, S. B., 1977 Allophane and imogolite Minerals in Soil Environments Wisconsin Soil Science Society of America, Madison 603 – 638.Google Scholar
Watanabe, T., Shimizu, H., Nagasawa, K., Masuda, A. and Saito, H., 1987 29Si-and 27Al-MAS/NMR study of the thermal transformations of kaolinite Clay Milter. 22 37 – 48.CrossRefGoogle Scholar