An alternative method for the certification of the sulfur mass fraction in coal Standard Reference Materials.
The S mass fractions of coal SRMs 2682b, 2684b, and 2685b are certified by direct comparison with coal SRMs 2682a, 2684a, and 2685a, respectively, using high-temperature combustion analysis with infrared (IR) absorption detection. The S mass fractions of the "a" materials used for calibration were previously determined by means of isotope-dilution thermal-ionization mass spectrometry (ID-TIMS). Therefore, the comparisons performed with the combustion-IR absorption method establish direct traceability links to accurate and precise ID-TIMS measurements. The expanded uncertainties associated with the certified S mass fractions are of approximately the same magnitude as would be expected for the ID-TIMS methodology. An important aspect of these certifications is that each "b" material is essentially identical with the corresponding "a" material, because both were produced from the same bulk, homogenized coal. As a test of the efficacy of the new certification approach when calibrant and unknown are not identical, the S mass fraction of coal SRM 2683b has been determined by direct comparison to coal SRM 2683a. These two coals, which have both previously been analyzed with ID-TIMS, are different in terms of S content and other properties. Whereas the S mass fraction for SRM 2683b determined with the new methodology agrees statistically with the ID-TIMS value, there is reason for caution in such cases. In addition to the usefulness of the alternative approach for certification activities within NIST, this approach might also be an excellent way of establishing NIST traceability during the value assignment process for reference materials not issued by NIST. Further research is needed, however, to understand better the scope of applicability.
Winchester
M R
MR
Analytical Chemistry Division, National Institute of Standards and Technology, Gaithersburg, MD 20899, USA. mwinchester@nist.gov
Kelly
W R
WR
Mann
J L
JL
Guthrie
W F
WF
MacDonald
B S
BS
Turk
G C
GC