Abstract: Two kinds of methods are used to measure the content of humic acids in weathered coal, cultivated horizon soil (limy cinnamon soils) and mined soil (castanozems), they are the volumetric method in the national standard measurement and the humic acids composition measurement. The paper includes comparisons of the content of humic acids in three samples measured by two kinds of methods, the differences in two experiments processes, and the dose of samples. It also compared which concentration is better for K2Cr207 in the humic acids composition measurement. The results show that the content of humic acids in the weathered coal and cultivated horizon soil (limy cinnamon soils), measured by the volumetric method, is about 4 times of the result measured by the humic acids composition measurement, but they get the similar results when the sample is mined soil (castanozems). Moreover, the volumetric method is easier and more reliable than the humic acids composition measurement when the samples contain more humic acids. The paper has also measured the suitable doses of two samples in different experiments, and 0.4000 mol/L is the suitable concentration of K2Cr2O7 in the humic acids composition measurement.