Limit Test Chloride And Sulphate |
1.0 PROCEDURE 1.1 Apparatus : • 50 ml Nessler’s cylinder • 1 ml pipette • 10 ml pipette • 1 ml graduated pipette • 25 ml measuring cylinder • Glass rods. 1.2 Reagent : • 5M acetic acid • 25% w/v barium chloride solution • 10 ppm ethanolic sulphate standard solution • 10 ppm sulphate standard solution • Chloride Standard solution • Dilute nitric acid • Silver Nitrate Solution To read this GTP Click here Preparation and Standardization of 0.1M Ceric Ammonium Sulphate. 1.3 Preparation of Reagents for sulphate🙁Limit Test Chloride And Sulphate) 5M acetic acid : Dilute 28.5 ml of glacial acetic acid to 100 ml with purified water. 25% w/v barium chloride solution : Dissolve 25.0 g of barium chloride in 100 ml of purified water 10 ppm sulphate standard solution : Dilute 1 volume of a 0.181 % w/v solution of potassium sulphate in purified water to 100 ml with the same solvent. 10 ppm ethanolic sulphate standard solution : Dilute 1 volume of a 0.181% w/v solution of potassium sulphate in ethanol (30% v/v) to 100 ml with ethanol (30% v/v). Dilute nitric acid (2.0 M): Take the 50.0 ml of purified water in 100 ml volumetric flask add 12.6 ml of the nitric acid drop by drop and dissolved, finally make the volume up to the mark with purified water. Silver Nitrate Solution: 1.7% w/v solution of silver nitrate with purified water. (0.1M). Store protected from light. 1.4 Method for sulphate:(Limit Test Chloride And Sulphate) 1.4.1 Sample Preparation: To 1.0 millilitre of a 25.0 % w/v solution of barium chloride(BaCl2) in a Nessler cylinder add 1.5 ml of ethanolic sulphate standard soln. (10 ppm. SO4), mix and allow to stand for 1 minute. Add 15 ml of sample soln. prepared as directed in STP and transfer to a Nessler cylinder and 0.15 ml of 5M acetic acid. Add sufficient purified water to produce 50 millilitre, stir with a glass rod and allow to stand for five minutes. View transversely against a black background. 1.4.2 Standard preparation : To 1.0 millilitre of a 25.0 % w/v soln. of barium chloride(BaCl2) in a Nessler cylinder add 1.5 ml of ethanolic sulphate standard soln. (ten ppm.), mix well and allow to standing for one minute. Add 15 millilitre of sulphate standard sol. (10 ppm.) and 0.15 ml of 5M acetic acid. Add water to produce 50.0 millilitre, stir with a glass rod and allow to standing for five minutes. View transversely against a black background. 1.5 Method for chloride: 1.5.1 Dissolve the specified quantity of the substance under examination in purified water, or prepare a solution as directed in the individual monograph. 1.5.2 Transfer the solution into a Nessler cylinder. Add 10 ml of dilute nitric acid (2.0 M), except when nitric acid is used in the preparation of the solution, dilute to 50 ml with purified water. 1.5.3 Add 1 millilitre of 0.1 M silver nitrate. 1.5.4 To preparation of the standard solution take a mixture of 10.0 ml of the chloride standard solution (25 ppm Cl) and 5.0 ml of purified water in place of substance solution to be examined and treating in the same manner. 1.5.5 Result: When viewed transversely against a black background any opalescence produced in the test solution is not more intense than that of the standard solution. |