ASTM D563-88 pdf free.Standard Test Method for Phthalic Anhydride Content of Alkyd Resins and ResinSolutions.
Weigh by difference,from a closed container into the500-mL Erlenmeyer flask, a specimen of resin or resin solutionsufficient to yield from 0.8 to 1.2 g of potassium alcoholphthalate. Add 150 mL of benzene， warming slightly on thesteam bath if necessary,to effect solution. Add 60 mL ofalcoholic KOH solution and attach the condenser. Place theflask in a water bath to a depth approximately equal to that ofthe contents of the flask. Warm the bath,maintaining atemperature of 40°C for 1 h, then gradually raise the tempera-ture until the alcoholic solution boils gently. Reflux for 1 1/ h.
Remove the flask from the bath and wash down theinside of the condenser with a few millilitres of alcohol-benzene wash solution. Remove the condenser，cap the flaskwith the soda-lime guard tube, and cool by means of runningwater or an ice bath.
When cool, filter immediately and as rapidly as possible,through a fritted-glass crucible that previously has been tared,using the alcohol-benzene wash solution for transferring theprecipitate and washing the reaction flask. Wash the precipitatewith successive portions of alcohol-benzene wash solutionuntil a few millilitres of washings collected in a second suctionflask are no longer alkaline to phenolphthalein. (Normallyabout 75 mL of wash solution are sufficient.) Do not allow airto be drawn through the crystals，as they are hygroscopic.Finally pour 25-mL of ether into the crucible and draw throughthe precipitate with the aid of suction.Wipe the outer surface of the crucible with a clean clothand place in a gravity convection oven at 60°C for 1 h (Note 3).Cool to room temperature in a desiccator and weigh.The precipitate is the alcoholate(C.H(COOH)2(CH,OH)),and the alcohol of crystallization will be slowly driven off on prolongedheating. It is safe，however, to dry the alcoholate at temperatures up to60°C for as long as 1 h.Correction for Carbonates—Coprecipitation of potas-sium carbonate (K,CO, ) with the potassium alcohol phthalate may be a source of error. If a correction for K CO; is desired,proceed as follows: Dissolve the weighed precipitate in about50 mL of distilled water that has been neutralized to phenol-phthalein. Add 3 to 4 drops of phenolphthalein indicatorsolution, and if the solution is alkaline, titrate with 0.1 N HCl.ASTM D563 pdf download.