This work discusses measurement of thermal conductivity (k) of films using a scanning hot probe method in the 3ω mode and investigates the calibration of thermal contact parameters, specifically the thermal contact resistance (RthC) and thermal exchange radius (b) using reference samples with different thermal conductivities. RthC and b were found to have constant values (with b = 2.8 ± 0.3 μm and Rthc = 44 927 ± 7820 K W−1) for samples with thermal conductivity values ranging from 0.36 W K−1 m−1 to 1.1 W K−1 m−1. An independent strategy for the calibration of contact parameters was developed and validated for samples in this range of thermal conductivity, using a reference sample with a previously measured Seebeck coefficient and thermal conductivity. The results were found to agree with the calibration performed using multiple samples of known thermal conductivity between 0.36 and 1.1 W K−1 m−1. However, for samples in the range between 16.2 W K−1 m−1 and 53.7 W K−1 m−1, calibration experiments showed the contact parameters to have considerably different values: Rthc = 40 191 ± 1532 K W−1 and b = 428 ± 24 nm. Finally, this work demonstrates that using these calibration procedures, measurements of both highly conductive and thermally insulating films on substrates can be performed, as the measured values obtained were within 1–20% (for low k) and 5–31% (for high k) of independent measurements and/or literature reports. Thermal conductivity results are presented for a SiGe film on a glass substrate, Te film on a glass substrate, polymer films (doped with Fe nano-particles and undoped) on a glass substrate, and Au film on a Si substrate. © 2015 The Royal Society of Chemistry. ; We gratefully acknowledge funding from the US Department of Energy, Office of Basic Energy Sciences through the S3TEC Energy Frontiers Research Center (T. B. T.) and NSF IRES grant #1028071 for financial support towards this work (A. A. W. and D. B. T.). We would also like to acknowledge support from ECR StG NanoTEC 240497, and PHOMENTA project MAT2011-27911 and NanoHiTEC project FP7-263306 (M. M. G.), and CSIC for a JAE Pre-Doctoral fellowship (M. M. R.). ; Peer Reviewed