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Soils and the vadose zone are the major terrestrial repository of carbon (C) in the form of soil organic matter (SOM), more resistant black carbon (BC), and inorganic carbonate. Differentiating between these pools is important for assessing vulnerability to degradation and changes in the C cycle affecting soil health and climate regulation. Major monitoring programs from field to continent are now being undertaken to track changes in soil carbon (SC). Inexpensive, robust measures that can differentiate small changes in the C pools in a single measurement are highly desirable for long‐term monitoring. In this study, we assess the accuracy and precision of thermo‐gravimetric analysis (TGA) using organic matter standards, clay minerals, and soils from a national data set. We investigate the use of TGA to routinely differentiate between C pools, something no single measurement has yet achieved. Based on the kinetic nature of thermal oxidation of SC combined with the different thermodynamic stabilities of the molecules, we designed a new method to quantify the inorganic and organic SC and further separate the organic biogeochemically active SOM (as loss on ignition, LOI) from the resistant BC in soils. We analyze the TGA spectrums of a national soil monitoring data set (n = 456) and measure total carbon (TC) using thermal oxidation and also demonstrate a TC/LOI relationship of 0.55 for soils ranging from mineral soils to peat for the United Kingdom consistent with previous monitoring campaigns. Core Ideas: Using thermo‐gravimetric analysis we quantify soil organic matter and inorganic carbon in a single measurement.In addition, we separate between readily decomposable organic carbon and resistant black carbon.Twenty five years of monitoring data show a consistent total carbon/loss on ignition ratio of 0.55 in British soils.Thermogravimetry is an excellent method for long time monitoring programs. [ABSTRACT FROM AUTHOR]