Whole blood is a complex mixture of biological and chemical species. Its pretreatment, which is often conducted by dry ashing, is needed before the analyses of trace metals in whole blood. Recently photo-Fenton Advanced Oxidation Process (AOP) process has been used in the pretreatment of whole blood. Two new AOP processes using simple heating and microwave irradiation have been developed in the current work to pretreat blood samples. The treatments are based on a Fenton-like AOP with acid deactivation of the enzyme catalase. The first treatment is performed with a lab oven over 5 h, while the second uses microwave irradiation for 6 min. These methods allow for either cost-effective pretreatment through the use of the lab oven, or time savings through the use of the microwave oven. The degradations of blood and pure hemoglobin samples are compared through UV/visible spectroscopy, and the copper concentration in the treated samples were analyzed via anodic stripping voltammetry as a demonstration of analyzing trace metals in the pretreated whole blood.