In the inspective process of chloride that existed in hydrogen peroxide (30%) solution manufactured by ionic exchange technique, an abnormal phenomenon was discovered. After testing repeatedly and comprehensive analyzing, the best innovational inspective method were provided and verified. This method not only touched closely productive practical, but also conformed and perfect to the GB of China (issued The China National Standards). Authors had already announced a proposal report about improve manufacturing technol., and have obtained excellent effect in productive practice.