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Gravimetric Determination of Monolayer Glycerol Complexes of Clay Minerals

Published online by Cambridge University Press:  01 January 2024

Earl B. Kinter  and
Sidney Diamond
Earl B. Kinter
Affiliation:
Bureau of Public Roads, Physical Research Division, Washington, D.C, USA
Sidney Diamond
Affiliation:
Bureau of Public Roads, Physical Research Division, Washington, D.C, USA
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Abstract

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Glycerol-treated montmorillonite gradually loses one layer of the normal two-layer glycerol complex upon moderate heating at 110°C, forming a monolayer complex with a sharp x-ray diffraction peak at about 14A. In the presence of free glycerol vapor, this complex is quantitatively stable on further heating. A simple gravimetric procedure has been devised to determine the weight of glycerol retained. The procedure involves addition of a dilute glycerol solution to a dried and weighed sample of clay in an aluminum foil dish, and subsequent oven drying over a glycerol surface until constant weight is attained. The portion of the glycerol retained on external surfaces is assessed by measuring the retention of a replicate sample previously collapsed irreversibly by heating at 600°C or higher.

The retention of monolayer glycerol complexes of vermiculite and endellite can be similarly determined. Ethylene glycol forms an analogous series of complexes, and its retention against heating can be measured in exactly the same way. Differential thermal analysis of glycerol- and glycol-treated montmorillonite suggests that both complexes decompose with endothermic reactions at about 300°C.

Glycerol retention values were shown to be independent of sample size and to be almost independent of equilibration temperature between 70°C and 150°C. As expected, they are inversely proportional to particle size. Cation saturation affects the values of both internal and external retention for montmorillonites. It is shown that retention is a function of montmorillonite content in a series of artificial mixtures. Glycerol retention values of a number of clay materials are presented.

Type
Article
Information
Clays and Clay Minerals (National Conference on Clays and Clay Minerals) , Volume 5 , February 1956 , pp. 318 - 333
Copyright
Copyright © Clay Minerals Society 1956

References

Bower, C. A., and Gschwend, F. B., 1952, Ethylene glycol retention by soils as a measure of surface area and interlayer swelling: Soil Sci. Soc. Amer. Proc., v. 16, p. 342–345.CrossRefGoogle Scholar
Broadhurst, S. D., and Teague, K. H., 1954, Halloysite in Chattooga Co., Georgia: Ga. Mineral Newsletter, v. 7, no. 2, p. 56–61.Google Scholar
Diamond, S., and Kinter, E. B., 1958, Surface areas of clay minerals as derived from measurements of glycerol retention: in Clays and Clay Minerals, Nat. Acad. Sci.—Nat. Res. Council pub. 566, p. 334–347.Google Scholar
Dyal, R. S., and Hendricks, S. B., 1950, Total surface of clays in polar liquids as a characteristic index: Soil Sci., v. 69, no. 6, p. 421–432.CrossRefGoogle Scholar
Dyal, R. S., and Hendricks, S. B., 1952, Formation of mixed-layer minerals by potassium fixation in montmorillonite: Soil Sci. Soc. Amer. Proc., v. 16, no. 1, p. 45–51.CrossRefGoogle Scholar
Kinter, E. B., and Diamond, S., 1956, A new method for preparation and treatment of oriented-aggregates of soil clays for x-ray diffraction analysis: Soil Sci., v. 82, no. 2, p. 111–120.CrossRefGoogle Scholar
Kunze, G. W., 1955, Anomalies in the ethylene glycol solvation technique used in x-ray diffraction: in Clays and Clay Minerals, Nat. Acad. Sci.—Nat. Res. Council, pub. 395, p. 88–93.Google Scholar
MacEwan, D. M. C., 1946, The identification and estimation of the montmorillonite group of clay minerals with special reference to soil clays: J. Soc. Chem. Ind. (London), v. 65, p. 298–304.CrossRefGoogle Scholar
Martin, R. T., 1955, Ethylene glycol retention by clays: Soil Sci. Soc. Amer. Proc., v. 19, no. 2, p. 160–164.CrossRefGoogle Scholar