The methods of ion exchange-elcctrodcposition, ion exchange-precipitation for source-making, and for determining 65Zn in marine environment have been studied in detail.The chemical and radiochemical yields are 90% for organism and sediment, and 85% for seawater.They have good repeatability with a precision of 3%.The decontamination factors for radioactive nuclides are larger than 103.The preconcentration of seawater and the electrode position for source-making are significantly improved and can be used on thin and even source-measucing, applicable to low background β counting.