Various hybrids or inbred lines of corn kernels and their corresponding soils were sampled from Sichuan, China, for the investigation of cadmium and zinc transfer from soil to corn. A new analytical procedure based on closed-vessel microwave-assisted digestion and chemical vapor generation atomic fluorescence spectrometry (CVG-AFS) was investigated for the determination of total trace cadmium in the corn samples, with accuracy confirmation by inductively coupled plasma atomic emission spectrometry (ICP-AES). Flame atomic absorption spectrometry (FAAS), also with accuracy confirmation by ICP-AES, was used for the determination of total Zn in the corn, also after the microwave digestion. For the corresponding soil samples, an incomplete digestion procedure (leaching or extraction) by 3 mL HNO3 and 3 mL H2O2 proved to be adequate for the determination of zinc by FAAS, whereas a complete decomposition of the samples by the combination of 4 mL HNO3 , 3 mL HF, and 2 mL H2O2 was needed for the determination of cadmium by ICP-AES. A linear correlation was found between zinc content in corn kernels and that in the corresponding soil samples.