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A procedure was developed that allows precise determination of Fe isotopic composition. Purification of Fe was achieved by ion chromatography on AG1-X8 strongly basic anion-exchange resin. No isotopic fractionation is associated with column chemistry within 0.02 [per thousand]/amu at 2[sigma]. The isotopic composition was measured with a Micromass IsoProbe multicollection inductively coupled plasma hexapole mass spectrometer. The Fe isotopic composition of the Orgueil CI1 carbonaceous chondrite, which best approximates the solar composition, is indistinguishible from that of IRMM-014 (-0.005 [+ or -] 0.017 [per thousand]/amu). The IRMM-014 reference material is therefore used for normalization of the isotopic ratios. The protocol for analyzing mass-dependent variations is validated by measuring geostandards (IF-G, DTS-2, BCR-2, AGV-2) and heavily fractionated Fe left after vacuum evaporation of molten wustite (FeO) and solar (MgO-[Al.sub.2][O.sub.3]-Si[O.sub.2]-CaO-FeO in chondritic proportions) compositions. It is shown that the isotopic composition of ICe during evaporation of FeO follows a Rayleigh distillation with a fractionation factor [alpha] equal to [([m.sub.1]/[m.sub.2]).sup.1/2], where [m.sub.1] and [m.sub.2] are the masses of the considered isotopes. This agrees with earlier measurements and theoretical expectations. The isotopic composition of Fe left after vacuum evaporation of solar composition also follows a Rayleigh distillation but with a fractionation factor (1.013 22 [+ or -] 0.000 67 for the [sup.56]Fe/[sup.54]Fe ratio) that is lower than the square root of the masses (1.018 35). The protocol for analyzing mass-independent variations is validated by measuring terrestrial rocks that are not expected to show departure from mass-dependent fractionation. After internal normalization of the [sup.57]Fe/[sup.54]Fe ratio, the isotopic composition of Fe can be measured accurately with precisions of 0.2[epsilon] and 0.5[epsilon] at 2[sigma] for [sup.56]Fe/[sup.54]Fe and [sup.58]Fe/[sup.54]Fe ratios, respectively ([epsilon] refers to relative variations in parts per 10 000). For [sup.58]Fe, this precision is an order of magnitude better than what had been achieved before. The method is applied to rocks that could potentially exhibit mass-independent effects, meteorites and Archaean terrestrial samples. The isotopic composition of a 3.8-Ga-old banded iron formation from Isua (IF-G, Greenland), and quartz--pyroxene rocks from Akilia and Innersuartuut (GR91-26 and SM/GR/171770, Greenland) are normal within uncertainties. Similarly, the Orgueil (CI1), Allende (CV3.2), Eagle Station (ESPAL), Brenham (MGPAL), and Old Woman (IIAB) meteorites do not show any mass-independent effect.

Abstract: High precision SIMS 26Al–26Mg isotope analyses were performed for a pristine Type B1 CAI Leoville 3535-1 on multiple mineral phases that include aluminum-rich zoned melilite mantle (Åk20–Åk60), magnesium-rich melilite (Åk70), fassaite, spinel and anorthite in the core. The data yield a well-defined internal isochron with an inferred initial 26Al/27Al ratio of (5.002±0.065)×10−5, which is lower than those of bulk CAIs and pristine fine-grained CAIs. Assuming homogeneous distribution of 26Al in the early solar system, Leoville 3535-1 formed ∼50ka after the time corresponding to the bulk CAI isochron. One anorthite analysis near the grain boundary adjacent to melilite shows sub-μm-scale heterogeneous magnesium distribution, though the 26Al–26Mg data plot on the isochron regression. Thus, the internal 26Al–26Mg system of the CAI remained closed since the last melting event that crystallized anorthite. High precision magnesium isotope analyses of magnesium-rich minerals (fassaite, magnesium-rich melilite, and spinel) show a small amount of scatter from the regression line (∼0.1‰) beyond analytical uncertainties. Most spinel and some fassaite data are systematically displaced below and above the regression line, respectively. It is likely that spinel remained unmelted at the time of the last melting event, while fassaite and anorthite crystallized from a partial melt. The regression line made by fassaite and anorthite data shows an initial 26Al/27Al ratio indistinguishable from that using all data. Mass dependent fractionation of magnesium isotopes in spinel is the same as those in melilite and fassaite (δ25Mg∼5‰), indicating that magnesium isotope fractionation, presumably from evaporative magnesium loss, predated the last melting event. Thus a majority of the CAI appears to have escaped magnesium isotope exchange with nebular gas during the last melting event, except for the outer rim of the melilite mantle that shows slightly lower δ25Mg values. The 26Al–26Mg systematics of this Leoville Type B CAI suggest it experienced a final melting event at ∼50ka after the initial Al–Mg fractionation event. This may correspond to melting during the active protostar stage (known as “Class I”), during which sporadic high temperature heating events repeatedly affected refractory solids in the solar nebula. [Copyright &y& Elsevier]