Quick scanning X-ray absorption fine structure (QXAFS) spectroscopy is applied to an examination of the pyrolytic decomposition of nickel formate dihydrate. Experimental QXAFS data reveal good quality edge and extended XAFS spectra being obtained in ca. 4 and 30 s, respectively. Comparison of data with normal (step/count) techniques reveals no adverse effect on the structural parameters derived using quick scanning. Temperature-programmed and isothermal decomposition studies are consistent with a pyrolysis mechanism involving rapid initial dehydration of the dihydrate followed by subsequent decomposition of the anion, via a nickel oxide intermediate, to yield a finely divided nickel metal (mean particle diameter ca. 12 Angstrom). These data confirm the nature of the principle intermediate and final product, both previously uncertain.