In this study, efforts are dedicated to studying the influence of hydrogen charging and oxidation solutions on the electrochemical measurement of hydrogen permeation in microalloyed steel API X52. It was found that by incorporating 4×10-4 mol/L Pd(NO3)2 into 1M NaOH hydrogen oxidation solution, an in-situ Pd layer was able to be deposited onto the exit side surface of the sample membrane which eliminates the necessity of depositing an electrocatalytic Pd layer prior to the permeation experiments and has potential advantages for the industrial application because of the simplified process. In comparison with the case of using only 1M NaOH as the hydrogen oxidation solution, the hydrogen oxidation solution with in-situ Pd coating could oxidize hydrogen atoms more effectively and was able to yield reproducible hydrogen permeation current. In addition, the effect of combinations of different hydrogen recombination poisons, such as thiourea and NaAsO2, and various charging solutions, such as NaOH, H 2SO4and acetic acid and sodium acetate buffer solution, is discussed. In most cases, the acetic acid and sodium acetate buffer solution with thiourea yielded the best permeation results with repeatable peak hydrogen permeation curves.