A technique for the determination of major concentrations of SiOz, AI,O,, Fe203, MgO, CaO, Na,O, and K,O, minor levels of Ti O,, P,O,, and MnO, and trace concentrations of Ba, Cr,Cu, Ni, Sr, V, and Zn, in semi-microsamples (200 mg) of powdered whole rock, is described. Chemically diverse standard reference rocks are used both for calibration and assessment of accuracy. A lithium metaborate fusion melt of each standard or sample is dissolved in dilute HNO, containing CS+ at a level of 0.2% (w/v). The resulting solution is used to perform all analyses except those for NapO and K20, which are determined in a portion of the original sample solution wherein the Cs' concentration has been raised to 0.32% (w/v). Analyses of both portions of each sample solution are performed using an optical emission spectrometerhpectrograph equipped with an echelle monochromator and a dc argon plasma excitation source. Trace element detection limits ranged from 2 ppm for Cu to 15 ppm for Zn. A study of precision based on replicate determinations in three splits of the proposed USGS reference basalt BHVO-1 yielded the following results: (1) For analyses of the major and minor oxide constituents, values of the percent relative standard deviation (RSD) ranged from 1 for CaO, to 21 for P,O,. (2) For trace element determinations, values of the RSD ranged from 2 for Cu, to 19 for Zn.Instrumental determinations of the bulk oxide and trace element compositions of silicate rocks of various types are commonly beset by several problems. It often happens that many analyses must be made of each sample unknown, of which only a smail amount is available, and that several of the trace elements are present a t concentrations in the low ppm range. Moreover, since any specimen of rock is a more or less heterogeneous mixture, the representativeness of its analyzed subsample can legitimately be questioned. In addition, the great complexity and variability of the major and minor element constituencies of silicate rocks engender matrix effects.Since 1970, X-ray fluorescence (XRFs) and atomic absorption spectrometry (AAS) have provided the instrumental techniques most widely employed for the analyses of metals and metalloids in geological materials (1,Z). The use of XRFs for this purpose, however, has two principal disadvantages: it is unsuitable for the determination of any trace element for which 2 < io, and, for routine bulk analysis ( S O 2 , Al2O3.FeLO,, MgO. CaO, Na70, K@, TiOL, P205, and MnO) and /or