This paper describes the evaluation of a time-resolved graphite spark source emission spectrometer built for the purpose of determining Ca, Na, and K in nanoliter volume samples of renal fluid. Subnanogram detection limits calculated from the working curve slope and the uncertainty of the sample signal are reported for Ca, Na and K; these detection limits are some three orders of magnitude higher than the shot noise limit. With the use of Li as an internal standard, working curves from 0 to 1 ng of Na, K, and Ca are shown. System performance data are given, and the utility of the analysis is discussed.