The report describes the research activities and scientific programs of the Microchemical Analysis Section of the Analytical Chemistry Division of the NBS Institute for Materials Research during the period July 1968 to June 1969. General activities are reported in the areas of gas analysis, polarography, potentiometry, coulometry, chemical microscopy, and classical microchemical analysis. Research activities described in some detail include: gravimetric preparation of gas analysis standards; polarographic determination of trace elements in glass; fabrication and performance of a microfluorine electrode; elucidation of the boric acid-borate-mannitol system; investigation of the relation between the equilibrium point and inflection point in acidimetric titrimetry; coulometric determination of trace quantities of chromium; and determiniation of trace elements by nuclear track measurements. A number of procedures which have been developed for the analysis of a variety of materials, utilizing the techniques mentioned above, are also included. (Author).