Dimethylglyoxime reacts with Ni in a buffered ammoniacal-citrate solution containing the detergent "Aquet" and hydroxylamine-hydrochloride. The resulting nickelous dimethylglyoxime is extracted with xylene. Visual comparison with standards permits the estimation of from 25 to 10,000 p.p.m. of Ni. Soil rock, or sediment samples may be decomposed by digestion with (1:3) nitric acid. About 70 determinations per man-day can be made. With minor modifications to the above procedure, sediments and soil may be semi-quantitatively analyzed for Ni at the sample site. The chemical equipment is easily portable and the analysis rapid because only 3 reagents are used and no heating is required, Two methods of sample digestion are employed yielding values reported as "available" M or "total" Ni, depending upon the severity of the digestion. Field trials were made at the Copper King mine, Gold Hill, Colorado. A nickeliferous amphibolite ore zone was clearly delineated after a soil traverse was made over it. A Ni train from the mine was traced for 1 1/2 mi. in the stream sediments.