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A simplified silver phosphate extraction method for oxygen isotope analysis of bioapatite

Shabaga, Brandi M. (University of Manitoba, Department of Geological Sciences, 125 Dysart Road, 240 Wallace Building, Winnipeg, R3T 2N2, Canada ) ; Gough, Hilary (University of Manitoba, Department of Anthropology, 432 Fletcher Argue Building, 15 Chancellor Circle, Winnipeg, R3T 2N2, Canada ) ; Fayek, Mostafa (University of Manitoba, Department of Geological Sciences, 125 Dysart Road, 240 Wallace Building, Winnipeg, R3T 2N2, Canada ) ; Hoppa, Robert D. (University of Manitoba, Department of Anthropology, 432 Fletcher Argue Building, 15 Chancellor Circle, Winnipeg, R3T 2N2, Canada ) ;
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    Rationale Although phosphatic materials are chemically complex and are prone to exchange oxygen isotopes with their environments, the phosphate (PO 4 3− ) component of these materials is robust and retains its original oxygen isotopic composition. As a result, there are currently several methods for the isolation of phosphate oxygen through the precipitation of silver phosphate (Ag 3 PO 4 ). However, some of these techniques produce Ag 3 PO 4 of questionable purity, while nearly all are lengthy and/or require relatively large sample sizes. Methods Five milligrams of bioapatite from modern cow teeth (enamel and cementum) were pre‐treated for removal of organic material prior to digestion in 2 M HF. The digested samples were titrated with silver ammine solution at 50°C to precipitate Ag 3 PO 4 . Oxygen isotopic data were collected using a Thermal Combustion Elemental Analyzer (TC/EA) paired with a Delta V Plus isotope ratio mass spectrometer via a ConFlo III universal interface. Results The quality of Ag 3 PO 4 is dependent on effective removal of organic material and the volume of silver ammine solution used during titration. A two‐step pre‐treatment of 2.5% NaOCl, followed by a 0.125 M NaOH solution, is the most effective treatment for the removal of organic material from both enamel and cementum. Optimal yields of Ag 3 PO 4 were achieved using 1.8 mL of silver ammine solution. The reproducibility of the phosphate δ 18 O compositions ranges from 0.3 to 0.4‰ (1σ) for modern cow teeth. Conclusions We present a simplified method for phosphate extraction from organic‐rich phosphatic material. Our method gave reproducible δ 18 O values for enamel and cementum from cows' teeth.


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