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School of Engineering and Science - Jacobs University

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1.50<br />

HF-HClO 4<br />

carbonate (HNO 3<br />

)<br />

1.25<br />

JUB / reference average<br />

1.00<br />

0.75<br />

0.50<br />

0.25<br />

0.00<br />

Sc Ti Co Ni Rb Sr Y Zr Nb Mo Cs Ba La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Hf Ta W Pb Th U<br />

Figure 20. Comparison <strong>of</strong> analytical accuracy relative to average reference values for both HF-HClO 4<br />

<strong>and</strong> carbonate (HNO 3 ) decompositions <strong>of</strong> the JDo-1 dolomite. Based upon similar results for the two<br />

decomposition methods, Sr, Y, the REE, W, Th, <strong>and</strong> U are considered to be quantifiable using the<br />

carbonate decomposition method. Additionally, note the excellent results for Ni determined from the<br />

carbonate decomposition method, which were calculated using the 62 Ni isotope. Elements likely to be<br />

hosted in refractory aluminosilicate phases that resist complete dissolution using the carbonate<br />

decomposition include Ti, Rb, Zr, Nb, Cs, Hf, <strong>and</strong> Ta.<br />

refractory mineral phases. If that is the case, then these refractory minerals may not be<br />

homogenously distributed within the JDo-1 powder, <strong>of</strong>fering a possible explanation<br />

for the wide variation in reported concentrations for incompatible elements.<br />

Compared to the HF-HClO 4 decomposition method the carbonate<br />

decomposition method is not expected to completely dissolve all mineral phases (e.g.,<br />

aluminosilicates), <strong>and</strong> data for JDo-1 obtained using the two different decomposition<br />

methods are presented in Figure 20. Regarding the carbonate decomposition <strong>of</strong> JDo-1,<br />

<strong>and</strong> many other carbonate samples as well, a black residue is commonly filtered out <strong>of</strong><br />

the sample solution, <strong>and</strong> this residue is presumed to be refractory organic carbon. The<br />

black solid retained during the filtering step does not appear to be <strong>of</strong> significance for<br />

the determination <strong>of</strong> Ni, Sr, Y, the REE, W, Th, <strong>and</strong> U, <strong>and</strong> it is concluded that these<br />

elements are hosted primarily by carbonate minerals, <strong>and</strong> therefore are quantifiable<br />

using the carbonate decomposition method. The accurate quantification <strong>of</strong> Ni using<br />

the carbonate method is notable, as this is only possible in an HNO 3 acid matrix <strong>and</strong><br />

by monitoring the 62 Ni isotope. Unlike 60 Ni, which is generally not suitable for Ni<br />

46

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