Abstract: To study The MALDI-TOF- Mass Spectfometry of silver phenylacetylide in order to investigate The state of aggregation of The functionalized transition metal coordinated compounds including clusters and determine The degree of ploymerization of the Silver phenylacetylide. Methods: The silver phenylacetylides were analyzed by The method of MALDI-TOF-MS. Results: The main members of The silver phenylacetylide were tetramer and pentamer The degree of polymerization was found to be up to twelve. Conclusion: The polymerization series of The silver phenylacetylide are according to The formula: Mn= nM+ Ag, (n = 1.2.3... ).