.+z, 78.70.BjRare and exotic annihilations of free positrons have been investigated extensively since the first discovery of positrons. The annihilation into three photons, however, has been neglected following theoretical work by Øre and Powell and several experimental studies using radioactive sources. Øre and Powell predicted that only one in 372 annihilations would result in the emission of three photons due to the parallel spin alignment of the electron-positron pair. A number of approximations were made to make the calculation tractable most notably the assumption of low momentum. No material dependence was expected. Subsequent experiments showed some dependence on material properties, notably on Z and density. We have set up an experiment to measure the annihilation into two and three photons with a five detector coincidence technique. Our results for low Z targets of Kapton, silicon and carbon, indicate no material dependence. The simplicity of the experiment and the high sensitivity for three photon annihilations render this method suitable for the characterization of porosity particularly when the concentration of pores is small. 1 Introduction The most common mode of annihilation of free unbound positrons is the emission of two gamma rays. Energy and momentum conservation require annihilations into at least 2 photons, and in the case of opposite spin alignment of electrons and positrons, the number has to be even. This is the basis for positron annihilation as a tool for the study of electron momentum distributions in materials as initially demonstrated by deBenedetti et al. [1]. Since then the field of Doppler broadening has become a powerful tool for materials studies of Fermi surfaces and defects.In the case of spin alignment the number of photons has to be odd (in the absence of angular momentum) to accommodate the total spin of 1 for the pair. As a higher order process, this rarely occurs when a vast number of electrons with all spin orientations are present, such as in metals. Shortly after the prediction and discovery of the positrons, Øre and Powell predicted the ratio of three photon annihilations over two photon events in the case of nearly free electrons and low energy positrons [2,3]. Earlier work by Lifshitz [4] and Ivanenko and Sokolov [5] is now considered wrong. Øre and Powell obtained the ratio of three photon annihilation vs. two photon annihilation rates ( i λ) the spin averaged inverse ratio R of the lifetimes ( i τ) of triplet positronium (ortho-Ps, spins parallel, i = 3) to that of singlet positronium (para-Ps, spins antiparallel, i = 1). Using current theoretical lifetime values by Adkins, et al. [6,7]. the ratio is