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Abstract: An accurate determination of the valence band discontinuity of the lattice matched GaAs/InGaP heterostructure is performed by admittance spectroscopy measurements in p+/MQW/n+ structures grown by metal-organic vapour phase epitaxy (MOVPE) using tertiarybutylarsine and tertiarybutylphosphine as alternative precursors for the V group elements. Through the analysis of the temperature dependence of the resonance frequency ϖ at which the isothermal curves of the conductance over frequency G(ω)/ω have the maximum, the energy separation of 336±5meV between the lowest heavy hole quantum level in the GaAs wells and the InGaP valence band top is obtained. A valence band discontinuity of ΔE V =346±5meV is then derived by accounting for the calculated confinement energy of heavy holes (). Experimental values of ΔE V previously reported in the literature spread over the wide range of 300–400meV. [Copyright &y& Elsevier]