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An analytical approach is proposed to optimize the thickness of petroleum coke for achieving maximum microwave power absorption in microwave heating based on analysis of reflection loss (RL). The microwave RL of the petroleum coke layer was studied over the moisture content range of 1%–5% at 20 °C and the petroleum coke (10% moisture content) in the temperature range of 20 to 100 °C at 2.45 GHz. The results show that RL depends sensitively on the thickness of the petroleum coke and the absorption peak shifts towards a larger thickness as the moisture content of the petroleum coke increases. There exists a matching thickness corresponding to the maximum microwave absorption, the maximum absorbing peak decreases when the thickness of petroleum coke exceeds the matching thickness. We also show that the absorption peak is found to move towards a smaller thickness region with increasing petroleum coke temperature.