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Accurate sex assignment of ancient human remains usually relies on the availability of coxal bones or well‐preserved DNA. Iron (Fe) and copper (Cu) stable isotope compositions (56Fe/54Fe and 65Cu/63Cu, respectively) were recently measured in modern human blood, and an unexpected result was the discovery of a 56Fe‐depletion and a 65Cu‐enrichment in men's blood compared to women's blood. Bones, being pervasively irrigated by blood, are expected to retain the 56Fe/54Fe and 65Cu/63Cu signature of blood, which in turn is useful for determining the sex of ancient bones. Here, we report the 56Fe/54Fe, 65Cu/63Cu, and 66Zn/64Zn ratios from a suite of well‐preserved phalanxes (n = 43) belonging to individuals buried in the 17th and 18th centuries at the necropolis of Saint‐Laurent de Grenoble, France, and for which the sex was independently estimated from pelvic bone morphology. The metals were purified from the bone matrix by liquid chromatography on ion exchange resin and the isotope compositions were measured by multiple‐collector inductively coupled plasma mass spectrometry. The results show that, as expected from literature data on blood, male bone iron is depleted in 56Fe and enriched in 65Cu relative to female. No sex difference is found in the 66Zn/64Zn ratios of bone. The concentration and isotopic data show no evidence of soil contamination. Four samples of five (77%) can be assigned their correct sex, a result comparable to sex assignment using Fe and Cu isotopes in blood (81%). Isotopic analysis of metals may therefore represent a valid method of sex assignment applicable to incomplete human remains. Am J Phys Anthropol 148:334–340, 2012. © 2012 Wiley Periodicals, Inc.

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