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A high spatial resolution Ar–Ar dating study of compositionally zoned micas using UV laser extraction has been used to investigate the effect of composition and compositional boundaries upon argon diffusion in mica. The crystals are characterised by muscovite cores and Li–F–Rb–Cs-rich lepidolite rims produced by the interaction of a residual melt-vapour phase with the original muscovite during the late stages of pegmatite crystallisation. Single crystals exhibit dramatic intra-grain age variations, with a maximum range of 2,880–2,117 Ma. Backscattered electron images combined with UV-laser analyses reveal that apparent ages younger than 2,600 Ma are directly associated with the compositionally distinct rims, suggesting that Ar diffusion was faster in the lepidolite than in muscovite. Although it is not possible to be fully quantitative using the present data, it seems that argon diffusion rates in lepidolite are similar to those in biotite. Major rearrangements of the crystal structure needed to accommodate high concentrations of lithium, fluorine and large interlayer cations (Rb+, Cs+) in muscovite account for lower argon retentivity of the crystal rims. In most cases the age profiles show no disturbance at the compositional boundary, despite the transition from a di-octahedral to tri-octahedral mica, indicating that in general the boundaries do not act as fast diffusion pathways. However, in some cases there is a clear drop in ages at the compositional boundary, which acts as an effective sub-grain boundary. The difference between the two types may be related to the internal structure of the compositional boundaries or their degree of contact with the grain boundary network of the rock.

U-Pb isotopic analyses using TIMS and Laser Ablation-Multi Collector-ICP-MS were carried out on columbite-tantalite minerals from three suites of rare-element (Li, Cs, Ta) pegmatites in the Superior Province of Canada. Conventional TIMS analyses of these columbite-tantalite crystals produce scattered data and reverse discordance even after HF leaching of the grains prior to dissolution, possibly reflecting the incomplete removal of the open-system metamict segments during sample preparation. LA-MC-ICP-MS analyses of unleached, primary columbite free from inclusions and alteration give consistent and precise (