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This book focused on the environmental pollution control through analysis of hydrogen peroxide and hydrazine through the electrochemical methods. These methods are attractive for biological and environmental analysis because they are cheap, simple, fast, sensitive, and selective. The double character of DAN (a hollow film) and PdNPs improved the electrochemical redox response toward H2O2 via increasing the effective surface area and electron transfer. The PdNPs/p1,5-DAN/CPE has become a promising sensor to determine H2O2 and HZ in real samples, environmental samples, and in enzymeless catalyzed reactions due to its advantages of high sensitivity, reproducibility, good stability and anti-interference ability against many interferents.