The hydrolysis of tripolyphosphate ( pppi ) and trimetaphosphatern(mpppi ) at 10'3 M concentration byrn[tn 2Co(OH)(0H2 )]^, (tn = trimethylenediamine), usingrnEu2 f /H+ quenching was investigated. The europium quenchingrnwas adopted since other methods interfere with phosphaternanalysis. The reactions were monitored by measurement ofrnorthophosphate (pi ), pyrophosphate (ppi ), tripolyphosphatern( pppi ) and trimetaphosphate ( mpppi ) in the quenchedrnaliquots of the reaction mixtures of the reagents. Arnmethod was developed to separate and determine therndifferent phosphate species in the orthophos phate formrnusing acetone- phosphomolybdate complex as the analyticalrnreagent. The reactive species with regard to thernhydrolysis were found to be a 3: 1 tn2Co( 111)ppp i andrntn2Co( 111)mpppi complexes. The results showed largerrnamounts of hydrolytic products for the directly addedrnsystems than those of stepwise additions . The productionrnof phosphites in the reaction solution that containrn[tn2Co(OH )(0H 2)j* and tri metaphosphate was ob served .rnSpectrophotometric determination of the phosphite wasrndone by first oxidising it with iodine to orthophosphaternand using acetone-phospho molybdate complex as thernanalytical reagent . Factors affecting the formation andrndegradation of the reactive and unreactive species havernbeen discussed and plausible mechanisns formulated .