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lumeng(½ð±Ò+2): 2010-03-23 09:00
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Determination of % NCO in Prepolymer
The method for the determination of the isocyanate level is based on that
given by Wright and Cummins (1969).
The NCO content of diisocyanates can be determined by the reaction with
an excess of a standard solution of dibutylamine in chlorobenzene (or dry
toluene) and titration of the excess with hydrochloric acid. The dibutylamine
is prepared by dissolving 129 g of freshly distilled dibutylamine in 871 g of
redistilled chlorobenzene and storing the resultant solution in the dark. The
solution is relatively stable, but it is advisable to determine the amine content
weekly by titration with 1 N hydrochloric acid in methanol.
In the determination, 2 g of the diisocyanate should be accurately weighed
out into a conical flask and 5 ml of chlorobenzene added. In the case of
naphthalene diisocyanate, it is recommended that the mixture be warmed
slightly to assist dissolution. To this mixture there is then added 25 ml of the
standard dibutylamine solution. The reaction is rapid and takes only a few
minutes for completion, when a clear solution is obtained. After adding 2 or
3 drops of a 1% alcoholic solution of bromophenol blue and 100 ml of methanol,
the excess dibutylamine can be titrated with 1 N hydrochloric acid.
If W = weight of sample in grams
V1 = volume in ml of HCl solution required for titration of the sample
V2 = volume in ml of HCl solution required for 25 ml of dibutylamine
solution (blank)
%NCO={[4.2*£¨v2-V1£©*N]/1000W}*100
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