using test method 5 with the resulting data in tables 13a and 13b phosphorous pentoxide 1 11 g 0 008 mols was added to 5 g 0 018 mols of c 2 f 5 ocf 2 cf 2 ch 2 ch 2 oh prepared as in example 2 at 85 u00b0 c and reaction was heated to 100 u00b0 c after 14 hours 6 ml of isopropyl alcohol was added to the reaction mixture at 65 u00b0 c stirred for 1 hour at 50 u00b0 c followed by the addition of 7 6 ml of di water after 5 minutes 1 2 ml ammonia 30 aqueous solution 0 017 mols was added and the reaction was stirred for 1 hour at 32 u00b0 c to provide the ammonium salt of the resulting polyfluoropolyether phosphate of formula i wherein j q and r were each 1 and r f was c 2 f 5 31 p nmr of the final product showed 47 5 mol bis fluoroalkyl phosphate x 2 30 1 mol fluoroalkylphosphate x 1 and minor amounts of several other components including phosphate a penetrating solution was prepared containing a fluorine concentration of 0 8 fluorine by weight and was applied to limestone saltillo and granite substrates as described in test methods 6 and 7 the substrate samples and untreated controls were tested for water repellency and oil repellency.