The production and characterization of NBS K-411 glass microspheres in the 2–40 μm range for certification as NIST Standard Reference Material® 2066 (SRM®) are described. Quantitative analysis and heterogeneity testing of the microspheres were done with an electron probe microanalyzer-X-ray energy dispersive spectrometry (EPMA-EDS) automated particle analysis procedure. Results for the trimmed and normalized data produced mean compositions for the elements Mg, Si, Ca, Fe, and O (calculated from stoichiometry) that are in good agreement with the certified values for the K-411 bulk glass (NBS SRM 470 Glasses for Mineral Analysis), but with uncertainties about twice as large as those for the bulk material. Differences from the bulk are attributable to microsphere geometry as well as mass and size effects.
