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A series of synthetic apatite crystals along the fluorapatite-chlorapatite Ca 5 (PO 4 ) 3 (F,Cl) join have been synthesized at 1220 to 1375 °C from Ca 3 (PO 4 ) 2  dissolved in a CaF 2 -CaCl 2  melt. The solid solutions have then been characterized both chemically and structurally. Because of well-known difficulties in measuring the chemical composition of apatites containing F and Cl by electron microprobe a new semi-micro wet chemical method has been developed. Apatite is relatively well dissolved in mineral acids including HNO 3 . Nitric acid digestion of apatite for analysis of F and Cl has not been applied in the past to our knowledge. One reason is the potential risk of losing gaseous HF and HCl during acid decomposition. We present an analytical procedure that enables the analyses of F, Cl, Ca, P, and trace elements after digestion of 10 mg apatite with a small amount of 1 N HNO 3  in gas-tight PTFE tubes at 80 °C. Analytical results from three independent closed acid digestions of 20 synthetic fluor-chlorapatites are presented. The reliability of this method was tested on the basis of charge balance, the Ca/P, Ca/(F+Cl), and P/(F+Cl) ratios, and the total cation sum. Independently derived Cl/F ratios by XRD using Rietveld refinement of apatite crystals from the same synthesis experiments are additionally presented.

A new semi-micro wet chemical method for apatite analysis and its application to the crystal chemistry of fluorapatite-chlorapatite solid solutions