This document: a) specifies a general test procedure for quantification of the spontaneous heat generation from solid biofuel pellets using isothermal calorimetry; b) specifies a screening test procedure for wood pellets using an instrument temperature of 60 °C; c) establishes procedures for sampling and sample handling of solid biofuel pellets prior to the analysis of spontaneous heat generation; and d) gives guidance on the applicability and use of isothermal calorimetry for calculation of the net reaction rate of the heat producing reactions of solid biofuel pellets. The test procedure given in this document quantifies the thermal power (heat flow) of the sample during the test, it does not identify the source of self-heating in the test portion analysed. Data on spontaneous heat generation determined using this document is only associated with the specific quality and age of the sample material. The results are product specific. This document is applicable to solid biofuel pellets only. The information derived using this document is for use in quality control and in hazard and risk assessments related to the procedures given in ISO 20024:2020.