A simplified silver phosphate extraction method for oxygen isotope analysis of bioapatite. (21st June 2018)

• Record Type: Journal Article
• Authors: Shabaga, Brandi M.; Gough, Hilary; Fayek, Mostafa; Hoppa, Robert D.
• Is Part Of: Rapid communications in mass spectrometry. Volume 32:Number 15(2018)
• Page Start: 1237
• Page End: 1242
• Publication Date: 2018-06-21
• Subjects: Mass spectrometry -- Periodicals; 543.65
• DOI: 10.1002/rcm.8149
• Languages: English
• ISSNs: 0951-4198

Abstract

Abstract : Rationale: Although phosphatic materials are chemically complex and are prone to exchange oxygen isotopes with their environments, the phosphate (PO4 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 (Ag3 PO4 ). However, some of these techniques produce Ag3 PO4 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 Ag3 PO4 . 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 Ag3 PO4 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 Ag3 PO4 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.