In order to determine the structure parameters of the reaction intermediate formed during the reduction process of chromate(VI) ion by hydrogen peroxide, a laboratory stopped-flow X-ray absorption fine structure (XAFS ) apparatus, which was constructed by a rotating anode X-ray generator, an energy scanning spectrometer, a stopped-flow assembly, and X-ray detectors, was newly developed. Using the apparatus, the Cr K -edge XAFS spectrum of the reaction intermediate was measured. One oxo group, two peroxo groups, and one water molecule are coordinated to the Cr(VI) center in the intermediate, CrO(O2)2(H2O ) , with Cr - O bond lengths of 157, 168, and 193 pm, respectively. The geometry around the Cr(VI) center is probably 6-coordinate pentagonal pyramidal.