Zircon concentrate was separated from 2-4 kg sample

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Appendix S1, auxiliary material
U/Th–Pb LA-ICPMS geochronology at the Senckenberg Naturhistorische Sammlungen,
Dresden
Zircons were analyzed for U, Th, and Pb isotopes by LA-ICPMS techniques using a ThermoScientific Element 2 XR sector field ICP-MS coupled to a New Wave UP-193 Excimer Laser
System. A teardrop-shaped, low volume laser cell constructed by Ben Jähne (Dresden) and
Axel Gerdes (Frankfurt/M.) was used to enable sequential sampling of heterogeneous grains
(e.g., growth zones) during time resolved data acquisition. Each analysis consisted of
approximately 15 s background acquisition followed by 30 s data acquisition, using a laser
spot-size of 25 and 35 µm, respectively. A common-Pb correction based on the interferenceand background-corrected
204
Pb signal and a model Pb composition [Stacey and Kramers,
1975] was carried out if necessary. The necessity of the correction is judged on whether the
corrected
207
Pb/206Pb lies outside of the internal errors of the measured ratios. Discordant
analyses were generally interpreted with care. Raw data were corrected for background signal,
common Pb, laser induced elemental fractionation, instrumental mass discrimination, and
time-dependant elemental fractionation of Pb/Th and Pb/U using an Excel® spreadsheet
program developed by Axel Gerdes (Institute of Geosciences, Johann Wolfgang GoetheUniversity Frankfurt, Frankfurt am Main, Germany). Reported uncertainties were propagated
by quadratic addition of the external reproducibility obtained from the standard zircon GJ-1
(~0.6% and 0.5-1% for the
207
Pb/206Pb and
206
Pb/238U, respectively) during individual
analytical sessions and the within-run precision of each analysis. Further details of the
instruments settings are available in Table S1. For further details on analytical protocol and
data processing see Gerdes and Zeh [2006].
The uncertainty in the degree of concordance of Precambrian–Palaeozoic grains dated by
the LA-ICPMS method is relatively large and results obtained from just a single analysis have
to be interpreted with care. A typical uncertainty of 2–3% (2σ) in
207
Pb/206Pb for a Late
Neoproterozoic grain (e.g., 560 Ma) relates to an absolute error on the
207
Pb/206Pb age of 45–
65 Myr. Such a result gives space for interpretation of concordance or slight discordance. The
latter one could be caused by episodic lead loss, fractionation, or infiltration Pb isotopes by a
fluid or on micro-cracks. Thus, zircons showing a degree of concordance in the range of 90–
110 % in this paper are classified as concordant because of the overlap of the error ellipse
with the concordia [e.g., Linnemann et al., 2011].
Th/U ratios are obtained from the LA-ICP-MS measurements of investigated zircon grains. U
and Pb content and Th/U ratio were calculated relative to the GJ-1 zircon standard and are
accurate to approximately 10%.
Gerdes, A., and A. Zeh (2006), Combined U-Pb and Hf isotope LA-(MC-)ICP-MS analysis of detrital zircons:
Comparison with SHRIMP and new constraints for the provenance and age of an Armorican metasediment
in Central Germany, Earth and Planetary Science Letters, 249, 47–61.
Linnemann, U., K. Ouzegane A. Drareni, M. Hofmann, S. Becker, A. Gärtner, and A. Sagawe (2011), Sands of
West Gondwana: An archive of secular magmatism and plate interactions – A case study from the
Cambro―Ordovician section of the Tassili Ouan Ahaggar (Algerian Sahara) using U-Pb LA-ICPMS detrital
zircon ages, Lithos 123, 188–203.
Stacey, J.S. and J.D. Kramers (1975), Approximation of terrestrial lead isotope evolution by a two-stage model,
Earth Planet. Science Letters 26, 207–221.
Table S1. Settings for the instruments used in the Geochronological Laboratory
(GeoPlasmaLab Dresden) of the Senckenberg Naturhistorische Sammlungen Dresden
(Excimer Laser, New Wave, UP 193) and (ICP-MS, Thermo-Fisher, Element 2 XR).
ICP-MS
Finnigan Element 2 XR
Forward Power
Gas flow rate
1390 W
15.0 l min-1 (plasma)
1.07 l min-1 (aux)
E-scan
202, 204, 206, 207,
208, 232, 235, 238
300
18 ns
< 1%
4 ms
≤ 1 ms/amu
1500
15 s
30 s
1.4 s (=25 scans)
Scan mode
Scanned masses
Mass resolution
Dead time
Oxide UO+/U+
Dwell time
Settling time
Number of scans
Background
Ablation time
Integration time
Laser system
Nominal spot diameter
Carrier gas
Laser settings
Drill speed (DS) /
Raster scan speed (RSS)
Cell volume
Sensitivity
UP193 New Wave
193 nm, excimer
25-35 µm (unknowns)
35 µm (standard)
0.25 l min-1 He
1.1 l min-1 Ar
10 Hz, 55% LP
~ 0.5 µm/s (DS)
c. 3 cm3
6 x 10 counts/pg U
6
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