Rt. Watkins et al., DETERMINATION OF RARE-EARTH ELEMENTS IN COAL USING MICROWAVE DIGESTION AND GRADIENT ION CHROMATOGRAPHY, Chemical geology, 121(1-4), 1995, pp. 273-283
The combined application of microwave digestion, high-performance ion
chromatography (HPIC) and on-line sample solution concentration provid
es a technique for the routine determination of rare-earth elements (R
EE) in coals. Acid dissolution of whole powdered coal samples using mi
crowave pressure digestion removes the necessity of dry ashing to elim
inate organic carbon, providing considerable time savings and signific
antly reducing the risk of sample loss and cross-contamination when sa
mples are prepared in batches. HPIC analysis using chelation chemistry
and gradient elution enables the separation and determination of 12 o
f the 14 naturally occurring REE in coals. The use of on-line sample s
olution concentration provides detection limits for individual element
s of between 10 and 50 ng g(-1) in the original coal. These are satisf
actory for the analysis of low-ash, low-REE, coals, despite the small
sample size (0.2 g) employed in this study, which was dictated by the
use of medium-pressure digestion vessels. Reproducibility of the techn
ique has been determined as generally better than +/- 5% CoV in the an
alysis of low-ash coals. REE data produced for coal standard reference
materials NBS-1632a, SARM-18, SARM-19 and SARM-20 are generally in go
od agreement with published values. Data are also provided for the new
low-ash coal standard CLB-1.