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X-ray powder diffraction for illite polytypes analysis

Agnese Stunda 1Ilze Luse 2Liga Berzina-Cimdina 1Valdis Seglins 2

1. Riga Biomaterials Innovation and Development Centre, Pulka Str. 3/3, Riga LV-1007, Latvia
2. University of Latvia, Raina Bulvaris 19, Riga LV1009, Latvia

Abstract

X-ray powder diffraction (XRPD) is one of main methods for clay minerals polymorphism research. For polytypes analyzing it is important to acquire unoriented clay XRPD pattern and in addition to it pattern should be intensive enough to recognize polytypes peaks.

Clay mineral crystallites have a small size and layered structure, therefore XRD pattern has a very small intensity. Polytype characterizing unbasal peaks have considerably lower intensity than basal peaks have. The aim of these studies is to achieve XRPD patterns of unoriented samples with hight resolution of unbasal reflexes. For these studies we used clay samples from Latvia with different genesis and various illite polytypes content. The samples were separated into 2 and 1 micron fractions, using different kind and different concentration of dispersants, [Na(PO3)]6 and NH4OH. Than each sample was tested either heated at 550oC, either saturated with glycol.

Analyzing clays by X-ray diffraction it was tried in several combinations to improve the intensity keeping background smooth.  Sample amount was very small, yet sample was placed in such a way, that irradiated diameter of sample reached 10 mm, thickness approximately 1 mm. We tested time prolongation from 30 till 120 s per step, split 1/4o and 1/2o, mask 5 and 10 mm and several irradiated length combinations.

XRD.GIF

Analyzable clay samples mostly contain illite and kaolinite. Using dispersants either doesn’t influences or makes X-ray pattern worse. Time prolongation and split opening improves reflection intensity, however damage background (see figure: a - 120, b - 60, c - 30 s/step), that obstruct interpretation of X-ray powder diffraction pattern.

 

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Related papers

Presentation: Poster at 11th European Powder Diffraction Conference, Poster session, by Agnese Stunda
See On-line Journal of 11th European Powder Diffraction Conference

Submitted: 2008-04-30 20:33
Revised:   2009-06-07 00:48