In connection with first report, details of precipitation of zinc pyrophosphate have been investi gated. Some discussions have also been centered on the preparation of metaphosphate and a pure trimetaphosphate has been prepared for analytical work. A new volmetric determination of pyrophosphate has been performed within the error in usual volumetric analysis in the presence of ortho-and trimetaphosphates. The results were very satisfactory in comparison with the other methods.