High-precision microcline 40Ar/39Ar dating by combined techniques

K-feldspar is one of the most common minerals applied for 40Ar/39Ar dating because of its high K content and ubiquitous presence. Excess 40Ar in K-feldspar resulting in unreliable ages has long been reported, however, its occurrence and trapping time are still inconclusive. Combined argon extraction techniques, including laser step heating, and step crushing, as well as succedent furnace incremental heating, have been applied to six microcline samples from two hydrothermal ore deposits in South China, to address these issues. Two microcline samples (09SZ37 & 39) measured by all the above three gas extraction techniques yield flat age spectra and concordant inverse isochron ages respectively. However, one sample (09NL10) produces a flat spectrum but with abnormally low radiogenic 40Ar, and the other three samples obtain uneven age spectra, by laser heating. All six samples measured by step crushing yield quite similar age spectra characterized with declining staircases for the first several steps, and followed with very flat plateaus of high-precision plateau ages for the subsequent later crushing steps. The declining sections with abnormally old ages indicate that excess 40Ar (and obvious atmospheric argon) was trapped in the microcracks and the secondary fluid inclusions. The data points corresponding to age plateaus well define inverse isochron ages which are in consistence with their plateau ages respectively. Furthermore, the crushed powders of all six samples by further furnace step heating also yield very flat age spectra, whose plateau ages are well concordant with those obtained by the foregoing step crushing experiments. The trapped excess 40Ar caused the total fusion ages of laser heating 0.7–17.8% older than their true ages. Mineral grains of ca. 0.10 mm may effectively remove excess 40Ar in microcracks and secondary fluid inclusions, proposed for direct 40Ar/39Ar step heating. Stepwise crushing, combined with furnace heating, is not only very useful to date fluid inclusions, but also robust to remove excess 40Ar and obtain more precise true ages for K-bearing minerals, e.g., K-feldspar, amphibole, tourmaline, and so on.