A highly sensitive and rapid procedure is described for submicro quantitation of copper and zinc contents from the nitric acid extract of fat free-dry-tissue (FFDT) by a double beam atomic absorption spectrophotometer using stoichiometric air-acetylene flame. Simultaneous background correction was afforded with a deuterium lamp for Zn analysis to eliminate interferences from non-atomic absorption at 213.9 nm. Cu and Zn standards, as well as the muscle extracts, were prepared in an aqueous medium containing 0.75 M Ultrex quality HNO3for spectral analysis which did not quench or enhance the relevant absorbance signals. Inherent mineral constituents of muscle such as Ca, Mg, Na, K, and P, when added upto ∼10-60 fold greater than the physiological concentration, did not cause either analytical or chemical interferences. Muscle specimens weighing between 0.8-12.0 mg FFDT were extracted in 5 ml of 0.75 M HNO3and directly aspirated into the flame. Muscle Cu and Zn contents were expressed in mg/kg FFDT. The smallest sample size confidently analyzed using this technique was ∼0.4 mg FFDT which corresponds to 2.0 mg of fresh tissue and can be safely obtained from a patient by muscle needle biopsy. Recovery studies from the inherent muscle matrix revealed 100.01 ± 0.399 and 99.64 ± 0.13% precisions for Cu and Zn respectively.