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School of Engineering and Science - Jacobs University

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1.50 SGR-1b (n=3)<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 17. Accuracy estimation for ICPMS analysis <strong>of</strong> shale SGR-1b, 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 measured concentrations for Ni, Y, Tb, <strong>and</strong> Tm are not necessarily considered<br />

anomalous, <strong>and</strong> likely represent small interferences (Ni) <strong>and</strong> relatively large uncertainties in the<br />

reference data (Y, Tb, Tm; see text <strong>and</strong> App. 1).<br />

not likely to adversely affect Nb determinations, assuming Nb is present in the sample<br />

at concentrations <strong>of</strong> several mg/kg or higher.<br />

SGR-1b<br />

The SGR-1b (Green River) shale is a petroleum <strong>and</strong> carbonate rich CRM<br />

issued by the USGS. The SGR-1b shale is identical to the original SGR-1 shale (S.A.<br />

Wilson, USGS, personal communication) <strong>and</strong> contains 6.5% Al 2 O 3 , 4.4% MgO, 8.4%<br />

CaO, 3.0% Fe 2 O 3 , <strong>and</strong> minor amounts <strong>of</strong> Mn (267 mg/kg). While the Al content <strong>of</strong><br />

SGR-1b is low compared to the SCo-1 shale, it is still high enough to produce<br />

significant Al-chloride interferences on 62 Ni. As a result Ni concentration data<br />

reported for SGR-1b are determined solely from analyses <strong>of</strong> the 60 Ni isotope. For the<br />

remaining major elements, significantly higher MgO <strong>and</strong> CaO in SGR-1b compared<br />

to SCo-1 would be expected to erroneously increase measured signal intensities for<br />

60 Ni, due to MgCl <strong>and</strong> CaO(H) inteferences. The combined magnitude <strong>of</strong> these Mg<br />

<strong>and</strong> Ca interferences on 60 Ni is estimated to be ~2 mg/kg (App. 2), <strong>and</strong> this is<br />

41

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