The invention aims at providing an analytical method for the total content of free organic acid and organic acid radical ions in a rubber and steel wire bonding agent, which is simple to operate, high in accuracy of analysis result and small in error. The chemical properties of the organic acid in the cobalt salt are greatly different due to the different lengths and branching degrees of the carbon chains, so that the organic acid is difficult to quantitatively test through a single process. The analytical method is realized by the following technical scheme: when the carbon number of the organic acid is C2-C8, selecting an organic acid with the carbon number of C2-C8 as an internal standard substance, and selecting monohydric alcohol with the carbon number of C3-C8 for esterification, preferably monohydric alcohol with the carbon number of C3-C5; when the organic acid is the organic acid with the carbon number of C8-C22, selecting monohydric alcohol with the carbon number of C8-C22 as an internal standard substance, and selecting monohydric alcohol with the carbon number of C1-C8 for esterification, preferably monohydric alcohol with the carbon number of C1-C4; and when the organic acid is isocaprylic acid and neodecanoic acid, selecting the organic acid with the carbon number of C6-C18 as an internal standard substance to realize the aim of using a gas chromatography to perform compartment analysis.