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Supplementary Methods
Samples PAR-1, DSM23, and DSM05A were supplied by Marcel Regelous, Open University
from the Open University collection. The samples were crushed to 1-2 mm, washed in
absolute ethanol and air-dried. Five to six total rock grains from each sample were loaded
into 21-pit Al irradiation disks, together with Fish Canyon neutron fluence monitors ((28.201
± 0.046 Ma) (Kuiper et al., 2008)), following the geometry in Vasconcelos et al. (2002). The
disk was wrapped in aluminum foil, vacuum sealed in a quartz vial, and irradiated for 14
hours at Oregon State University (USA) Radiation Center B-1 CLICIT TRIGA reactor
facility. After a decay period, three distinct grains from each sample were separately dated
by the laser incremental heating 40Ar/39Ar method at the University of Queensland Argon
Geochronology in Earth Sciences (UQ-AGES) laboratory. J-factors for each Al-disk were
determined by the laser total fusion analyses of 15 individual aliquots of neutron fluence
monitor, each consisting of one to three grains of Fish Canyon sanidine. Before analysis, the
rock grains and fluence monitors were baked-out under vacuum at ~200 °C for ca. 12 hours.
The rock grains were heated incrementally with a continuous-wave Ar-ion laser with a
defocused beam. Active gases released during laser heating were removed by a -133 ºC cold
trap and two C-50 SAES Zr-V-Fe getters. Argon isotopes in the cleaned gas fractions were
analyzed in a MAP 215-50 noble gas mass spectrometer. Full system blanks and air pipettes
were determined before and after each sample. The data were corrected for atmospheric
A 40Ar/36Ar value of 298.56 ± 0.31 for atmospheric argon (Lee et al., 2006) was used for the
calculation of the mass spectrometer discrimination. All ages are reported using the currently
accepted decay constants (Steiger and Jäger, 1977). All errors are quoted at the 2σ confidence
level (95%), and include the errors in the irradiation correction factors and the error in J. The
reported errors do not include the uncertainty in the age of the flux monitor or the uncertainty
post-irradiation decay of 39Ar and 37Ar. Errors in this table are 1σ. The heating time for all
analyses was ~45 seconds, not including the laser ramp-up time. Abbreviations used are: %
Rad., % radiogenic argon; Discr., discrimination. The J factor for all analysis is 0.003603 ±
0.000007. The error in the J factor is not included in the tabulated error in the age in Table
S1, but is included in all plateau, age probability, and isochron ages throughout the text. The
mass spectrometer gain was calculated based on the analysis of an air pipette (1.72 x 10-13
moles 40Ar) on the Faraday detector (~4 mV) equipped with a 1 x 1011 Ohms resistor,
Balzers 217 Electron Multiplier with a 1 x 109 Ohms resistor produced a signal of ~3.4 nA
40
Ar. The operating gain of the electron multiplier-Keithley electrometer combination relative
to the Faraday detector was ~8.5 x 104. The historical irradiation correction factors for the
CLICIT facility, TRIGA reactor, Oregon State University, USA are: (2.64 ± 0.02) x 10-4 for
(36Ar/37Ar)Ca, (7.04 ±0.06) x 10-4 for (39Ar/37Ar)Ca, and (8 ± 3) x 10-4 for (40Ar/39Ar)K