In vacuo reduction of silver orthophosphate with graphite for high-precision oxygen isotope analysis.
The reduction of silver phosphate with graphite under vacuum conditions was studied at final reaction temperatures varying from 430 to 915°C to determine: (i) the CO(2) extraction yield, and (ii) the oxygen isotopic composition of CO(2). The CO(2) yield and oxygen isotopic composition were determined on a calibrated dual inlet and triple collector isotope ratio mass spectrometer. We observed the following three stages of the reduction process. (1) At temperatures below 590°C only CO(2) is formed, while silver orthophosphate decays to pyrophosphate. (2) At higher temperatures, 590-830°C, predominantly CO is formed from silver pyrophosphate which decays to metaphosphate; this CO was always converted into CO(2) by the glow discharge method. (3) At temperatures above 830°C the noticeable sublimation of silver orthophosphate occurs. This observation was accompanied by the oxygen isotope analysis of the obtained CO(2). The measured δ(18)O value varied from -11.93‰ (at the lowest temperature) to -20.32‰ (at the highest temperature). The optimum reduction temperature range was found to be 780-830°C. In this temperature range the oxygen isotopic composition of CO(2) is nearly constant and the reaction efficiency is relatively high. The determined difference between the δ(18)O value of oxygen in silver phosphate and that in CO(2) extracted from this phosphate is +0.70‰.
Pelc
Andrzej
A
Mass Spectrometry Laboratory, Institute of Physics, Marie Curie-Sklodowska University, 20-031 Lublin, Poland. andrzej.pelc@poczta.umcs.lublin.pl
Halas
Stanislaw
S