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Pervaporation is a method for separating liquid mixtures especially dehydration of organic solvents.Poly(vinyl alcohol)(PVA) is one of the most important commercial polymers used in pervaporation [1],and crosslinking reactions are one of the most general used techniques to improve the physical properties of it [2].Glutaraldehyde and glyoxal are the commonly crosslinkers for these reactions.This report will be describing the quantitative analysis of PVA.The membranes were tested at 40-70℃ for dehydration performance of 95% methanol aqueous solutions.Under the same experimental conditions,permeate flux decreased whereas the selectivity increased as the mole of crosslinkers increased.A convenient FTIR test has been established to analyze the degree of crosslinking in PVA.And DSC was used to analyze the glass temperature of them.