To assess and validate temperature measurement and data analysis techniques for a quasi-adiabatic calorimeter used to measure amplitude-dependent loss power of magnetic nanoparticles exposed to an alternating magnetic field (AMF) at radiofrequencies (160 ± 5 kHz). The data collected and methods developed were used to measure the specific loss power (SLP) for two magnetic iron oxide nanoparticles (IONPs) suspensions, developed for magnetic nanoparticle hyperthermia. Calibration was performed by comparing measured against calculated values of specific absorption rate (SAR) of a copper wire subjected to AMF. Rate of temperature rise from induced eddy currents was measured (n = 4) for a copper wire of radius 0.99 mm and length of 3.38 mm in an AMF at amplitudes (H) of 16, 20, 24, and 28 kA/m. The AMF was generated by applying an alternating current using an 80-kW induction power supply to a capacitance network containing a 13.5-cm vertical solenoid that held the calorimeter. Samples were taped to an optical fiber temperature probe and inserted into a standard (polystyrene, 5 ml) test tube which was suspended in the calorimeter. The sample was subjected to the AMF for 30 s or until the temperature of the sample, increased by 30 °C, recorded at 0.3-s intervals. The SAR of the sample was normalized by H2f1/2, averaged, and compared to theoretical values. Iron (Fe) normalized SLPs of two IONPs (JHU-MION and bionized-nanoferrite (BNF) particles (Micromod Partikeltechnologie, GmbH)) in aqueous suspension were measured in the same setup. We report experimental SAR values for the copper of 2.4 ± 0.1, 4.3 ± 0.2, 6.2 ± 0.1, and 8.5 ± 0.1 W/g compared to theoretical values 3.1 ± 0.1, 4.5 ± 0.2, 6.5 ± 0.1, and 9.2 ± 0.2 W/g at AMF amplitudes of 16 ± 0.1, 20 ± 0.2, 24 ± 0.1, and 28 ± 0.1 kA/m, respectively. Normalized experimental data followed a linear trend approximately parallel to theoretical values with an R2-value of 0.99. The measured SLPs of the JHU particles are higher than BNF particles within the tested AMF amplitude range of 15 kA/m to 45 kA/m. We demonstrated that copper can be used to calibrate magneto-thermal calorimetric systems used for SLP measurements of magnetic nanoparticles for a field range of 15–28 kA/m at 160 ± 5 kHz. We also note that the electrical conductivity, diameter of copper sample and accuracy, and response time of thermometry constrain calibration to lower amplitudes, highlighting the need for development of standard reference materials for such applications.