Hostname: page-component-586b7cd67f-dsjbd Total loading time: 0 Render date: 2024-11-23T02:10:55.690Z Has data issue: false hasContentIssue false
  • English
  • Français

X-ray powder diffraction study of synthetic Palmierite, K2Pb(SO4)2

Published online by Cambridge University Press:  05 March 2012

Ralph G. Tissot ,
Mark A. Rodriguez ,
Diana L. Sipola  and
James A. Voigt
Ralph G. Tissot*
Affiliation:
Materials Characterization Department 1822, Sandia National Laboratories, Albuquerque, New Mexico 87185
Mark A. Rodriguez
Affiliation:
Materials Characterization Department 1822, Sandia National Laboratories, Albuquerque, New Mexico 87185
Diana L. Sipola
Affiliation:
Ceramic Materials Department 1843, Sandia National Laboratories, Albuquerque, New Mexico 87185
James A. Voigt
Affiliation:
Ceramic Materials Department 1843, Sandia National Laboratories, Albuquerque, New Mexico 87185
*
a)Electronic mail: [email protected]
Get access Rights & Permissions [Opens in a new window]

Abstract

Palmierite (K2Pb(SO4)2) has been prepared via a chemical synthesis method. Intensity differences were observed when X-ray powder data from the newly synthesized compound were compared to the published powder diffraction card (PDF) 29-1015 for Palmierite. Investigation of these differences indicated the possibility of preferred orientation and/or chemical inhomogeneity affecting intensities, particularly those of the basal (00l) reflections. Annealing of the Palmierite was found to reduce the effects of preferred orientation. Electron microprobe analysis confirmed K:Pb:S as 2:1:2 for the for the annealed Palmierite powder. Subsequent least-squares refinement and Rietveld analysis of the annealed powder showed peak intensities very close to that of a calculated Palmierite pattern (based on single crystal data), yet substantially higher than many of the PDF 29-1015 published intensities. Further investigation of peak intensity variation via calculated patterns suggested that the intensity discrepancies between the annealed sample and those found in PDF 29-1015 were potentially due to chemical variation in the K2Pb(SO4)2 composition. X-ray powder diffraction and crystal data for Palmierite are reported for the annealed sample. Palmierite is trigonal/hexagonal with unit cell parameters a=5.497(1) Å, c=20.864(2) Å, space group R-3m(166), and Z=3.

Keywords

PalmieriteX-ray powder diffractionRietveld refinementpreferred orientationsynthesis
Type
New Diffraction Data
Information
Powder Diffraction , Volume 16 , Issue 2 , June 2001 , pp. 92 - 97
Copyright
Copyright © Cambridge University Press 2001

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

Dollase, W. A. (1986). “Correction of intensities for preferred orientation in powder diffractometry: Application of the March model,” J. Appl. Crystallogr. JACGAR 19, 267–272. acr, JACGAR CrossRefGoogle Scholar
International Tables for X-ray Crystallography (1974). (Kluwer Academic, Boston), Vol. IV, 71 pp.Google Scholar
Jenkins, R., and Snyder, R. L. (1996). Introduction to X-Ray Powder Diffractometry (Wiley, New York), pp. 149–150.Google Scholar
March, A. (1932). “Mathematische theorie der regelung nach der Korngestalt bei affiner deformation,” Z. Kristallogr. ZEKRDZ 81, 285–297. zek, ZEKRDZ CrossRefGoogle Scholar
Smith, G. S., and Snyder, R. L. (1979). “F(N): A criterion for rating powder diffraction patterns and evaluating the reliability of powder pattern indexing,” J. Appl. Crystallogr. JACGAR 12, 60–65. acr, JACGAR CrossRefGoogle Scholar
Von Saalfeld, H. (1973). “Crystallographic investigations of Glaserite from Mount Vesuvius (Italy),” Neues Jahrb. Mineral., Monatsh. NJMMAW 2, 75–78. nja, NJMMAW CrossRefGoogle Scholar
Von Schwarz, H. (1966). “I. Sulfate,” Z. Anorg. Allg. Chem. ZAACAB 344, 41–55. zaa, ZAACAB Google Scholar