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Contamination in the Rare-Earth Element Orthophosphate Reference Samples.

John J Donovan1, John M Hanchar2, Phillip M Picolli3

  • 1Department of Geological Sciences, The University of Oregon, Eugene, OR 97403-1272.

Journal of Research of the National Institute of Standards and Technology
|July 23, 2016
PubMed
Summary
This summary is machine-generated.

Rare-earth element orthophosphate standards are contaminated with lead due to a lead pyrophosphate flux used in their synthesis. This impurity affects the accuracy of electron probe micro-analysis (EPMA) data derived from these materials.

Keywords:
EPMAREEmicroanalysisorthophosphatesquantitative analysisrare earth elementsrare earth phosphatesstandards

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Area of Science:

  • Geochemistry
  • Materials Science
  • Analytical Chemistry

Background:

  • Rare-earth element (REE) orthophosphate standards are crucial for electron probe micro-analysis (EPMA).
  • Standards produced in the 1980s at Oak Ridge National Laboratory and distributed by the Smithsonian Institution are widely used.
  • Previous studies have not fully addressed the extent of lead (Pb) contamination in these valuable materials.

Purpose of the Study:

  • To investigate and explain the significant lead (Pb) contamination observed in rare-earth element (REE) orthophosphate standards.
  • To rationalize the varying degrees of Pb incorporation between different crystal structures (monazite vs. xenotime).

Main Methods:

  • Analysis of fourteen REE orthophosphate standards grown at Oak Ridge National Laboratory.
  • Identification of lead pyrophosphate (Pb2P2O7) flux as the source of Pb contamination.
  • Comparison of Pb incorporation in monoclinic monazite and tetragonal xenotime structures.

Main Results:

  • Several REE orthophosphate standards are significantly contaminated with lead (Pb).
  • The Pb impurity originates from the Pb2P2O7 flux, synthesized from PbHPO4.
  • Monazite-structure orthophosphates exhibit higher Pb incorporation than xenotime-structure orthophosphates.

Conclusions:

  • The Pb contamination in REE orthophosphate standards, while an issue for EPMA, can be understood through the synthesis process.
  • Understanding the Pb source and its structural preferences is key to interpreting analytical data.
  • These otherwise stable and homogeneous standards remain valuable, but their Pb content must be considered.