You are on page 1of 1

COPY

S.B.CHEMICALS

DETERMINATION OF FLUORINE BY DISTILLATION METHOD


OUT LINE OF THE METHOD: Fluorine is steam distilled from the solution of the sample containing perchloric acid & titrated with standard Thorium Nitrate solution. APPARATUS: The distillation apparatus consisting of a 250 ml distillation flask, side arm of which is connected with a condenser. The neck of the flask is fitted with a two-wholed rubber stopper carrying a thermometer & a 4 mm glass tube connecting the flask with a steam generator. The latter is equipped with two discharges, one tube to release steam and other tube to deliver steam into the distillation flask & a safety tube about 90 cm. The distillation is collected into a conical flask. REAGENTS: 1: Sodium Carbonate. 2: Potassium Carbonate. 3: Finely Ground Quartz. 4: Perchloric Acid 70% 5: Sodium Alizarin Sulphonate Indicator. 6: Sodium Hydroxide Solution 0.5 N. 7: Dilute Hydrochloric Acid. 20 ml cone HCl in 1000 ml d.w. 8: Buffer Solution. Dissolved 9.448 gm of Monochloric Acid in 100 ml of water. Add 50 ml of Sodium Hydroxide 1 N & mix well. 9: Standard Thorium Nitrate Solution. Weigh 13.806 gm ofThorium Nitrate, dissolved in d.w. & make up to one litre. 10: Standard Sodium Fluoride Solution. ( 1 ml = l mg ofFluorine.) Dissolved 2.211 gm of Sodium Fluoride, previously dried at 120 0C in one litre of d.w. in volumetric flask. PROCEDURE: Weigh accurately 0.25 gm of sample & fuse it with 1.1 gm of sodium carbonate & 0.6 gm of ignited silica in a platinum crucible. Transfer the melt with the aid of little water to a 250 ml distillation flask, containing 8 to 10 glass beads. Add 30 ml of perchloric acid. The temparature should not rise above 500C. Place a conical flask under the condenser. Distilled the solution until the boiling point reaches about 140 0C. While this is being done heat the water in the steam generator to boiling but do not allow the steam to get into the flask. When the temp. reaches 165 0C, admit steam into the flask. Maintain the temp. at about 140 0C by adjusting the steam flow & heating the flask. Continue distillation untill nearly 200 ml are collected in conical flask. Transfer the distillate in a 250 ml volumetric flask. Cool & make up the volume to the mark and mix well. Pipete out 50 ml aliquot into a 250 ml beaker. Add 50 ml d.w., 10 drops of sodium alizarin-sulphonate indicator and mix well. Add sodium hydroxide solution slowly with stirring till the solution become pink. Add dilute hydrochloric acid drop by drop with continous stirring till the pink colour is just discharged leaving the solution just acidic. Add from burette 2 ml of buffer solution & titrate with standard thorium nitrate solution with constant stirring till a permanent pink end point is reached. The colour intensity at the end point should be kept in mind & the titration should be stopped exactly at the same colour intensity for both the thorium nitrate standardization & the test solution titration. CACULATION:
% OF FLUORINE =

Volume in ml of Standard Thorium Nitrate Solution X Fluorine equivalent std Thorium Nitrate Solution in g/ml Weight in gm of the sample represented by the aliquot taken

You might also like