0.1M Perchloric acid |
1.0 Scope: This procedure is applicable for preparation and standardization of 0.1M perchloric acid. 2.0 Apparatus: 2.1 1000 ml volumetric flask 2.2 250 ml glass-stoppered conical flask 2.3 25.0 ml and 50.0 ml volumetric pipette 2.4 100 ml volumetric flask 3.0 Reagents soln. preparation: 3.1 Perchloric acid of AR grade 3.2 Potassium hydrogen phthalate AR grade 3.3 Crystal violet soln.. 3.4 Glacial acetic acid AR grade 3.5 Acetic anhydride AR grade To read this SOP click here Preparation and Standardization of 0.1M Potassium hydroxide. 4.0 Preparation: Mix 8.50 ml of perchloric acid(HClO4) with 500.0 ml of glacial acetic acid (CH₃COOH) 25.0 ml of acetic anhydride, cool and add glacial acetic acid to produce 1000.0 ml. If the purified water content exceeds 0.05 %, add more acetic anhydride. If the solution contains no titrable water, add sufficient water to obtain a content of water between 0.02 % w/w & 0.05 % w/w. The soln. so obtained should contain between 0.02 % w/w and 0.05 % w/w of purified water. 5.0 Standardization: Weigh accurately about 0.35 gm or 350mg of potassium hydrogen phthalate(C8H5KO4), previously powdered lightly and dried at 120 degree Celsius for 2 hours and dissolve it in 50 ml of glacial acetic acid. Add 0.1 ml of crystal violet soln. and titrate with 0.1M perchloric acid solution until the violet colour changes to emerald-green. Performed a blank determination and make any necessary correction in qc. Each ml of 0.1M perchloric acid(HClO4) is equivalent. to 0.02042 gm. of C8H5KO4. 6.0 Calculation: Molarity = Weigh X 0.1 / Vol. cons. X 0.02042 Where: Molarity. = molarity. of perchloric acid solution Weight = weight of potassium hydrogen phthalate in g Vol. cons. = burette reading of 0.1M perchloric acid solution in ml 7.0 Storage: Store in a well fitted amber colour glass bottle. |