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School of Engineering and Science - Jacobs University

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1.50 SCo-1 (n=4)<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 16. Accuracy estimation for ICPMS analysis <strong>of</strong> shale SCo-1, where n equals the number <strong>of</strong><br />

separate HF-HClO 4 sample decompositions <strong>and</strong> ICPMS analyses in 0.5 M HCl. Grey bars represent<br />

variability in the calculated ratio that is due solely to uncertainty in the reference average. Vertical lines<br />

represent the variability in the calculated ratio due to the uncertainty <strong>of</strong> the JUB data, <strong>and</strong> all data are<br />

presented in App. 1. The triangles for Sc, Ti, Co, <strong>and</strong> Ni represent average JUB data that excludes a<br />

single analysis that determined anomalously high values for these four elements, <strong>and</strong> when the<br />

‘anomalous’ data are not considered the JUB averages more closely match the reference values for Sc,<br />

Ti, Co, <strong>and</strong> Ni.<br />

to a single JUB analysis <strong>of</strong> SCo-1 that determined much higher concentrations for<br />

these elements, <strong>and</strong> when these ‘anomalous’ data are not considered (see Fig. 16), the<br />

measured concentrations for 30 <strong>of</strong> 32 analyzed elements are between 90–110% <strong>of</strong> the<br />

reference value.<br />

Potential major element interferences on trace metal determinations in SCo-1<br />

would include 27 Al 35 Cl on 62 Ni, <strong>and</strong> FeCl on 93 Nb (Table 4). The impact <strong>of</strong> Alchloride<br />

interferences on 62 Ni is significant enough that it is recommended that 62 Ni<br />

not be used for Ni determinations in shales (or sediments) that contain more that a<br />

few percent Al 2 O 3 <strong>and</strong> that are diluted in HCl (see App. 2). Note that the Ni data<br />

presented in App. 1 <strong>and</strong> Fig. 16 reflect concentrations for SCo-1 that were determined<br />

solely by monitoring <strong>of</strong> 60 Ni. As for Nb, the presence <strong>of</strong> ~5% Fe 2 O 3 in SCo-1 would<br />

be predicted to increase Nb concentrations by roughly 0.1 mg/kg, which is<br />

insignificant when compared to the SCo-1 reference Nb value <strong>of</strong> 11.9 mg/kg. It is<br />

therefore concluded that Fe 2 O 3 concentrations in shales (or sediments) <strong>of</strong> 3-7% are<br />

40

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