NAME: Felix Saber SAMPLE: Potassium Bromide 1) IDENTIFICATION REACTIONS OF IONS - CATIONS (describe briefly reactions): Solutions S gives the reactions of potassium - Dissolve 0.1 g of the substance to be examined in 2 mL of water R or use 2 mL of the prescribed solution. Add 1 mL of sodium carbonate solution R and heat. No precipitate is formed. Add to the hot solution 0.05 mL of sodium sulfide solution R. No precipitate is formed. Cool in iced water and add 2 mL of a 150 g/L solution of tartaric acid R. Allow to stand. A white crystalline precipitate is formed. - b) Dissolve about 40 mg of the substance to be examined in 1 mL of water R or use 1 mL of the prescribed solution. Add 1 mL of dilute acetic acid R and 1 mL of a freshly prepared 100 g/L solution of sodium cobaltinitrite R. A yellow or orange-yellow precipitate is formed immediately. - ANIONS (describe briefly reactions): - Dissolve in 2 mL of water R a quantity of the substance to be examined equivalent to about 3 mg of bromide (Br–) or use 2 mL of the prescribed solution. Acidify with dilute nitric acid R and add 0.4 mL of silver nitrate solution R1. Shake and allow to stand. A curdled, pale yellow precipitate is formed. Centrifuge and wash the precipitate with three quantities, each of 1 mL, of water R. Carry out this operation rapidly in subdued light disregarding the fact that the supernatant solution may not become perfectly clear. Suspend the precipitate obtained in 2 mL of water R and add 1.5 mL of ammonia R. The precipitate dissolves with difficulty. 2) ASSAY Volumetric solutions: 0,1 M AgNO3 Titre of volumetric solutions: 0.9998 Titration No. m [g] (4 decimal places) Consumption of VS [ml] ASSAY 1. 2.0014 8.45 98.866 2. 2.1054 7.89 97.139 3. 2.0456 8.38 97.157 4. 1.9985 8.34 99.683 Average 98.211 CALCULATION PROCEDURE: X1=(25x0.9998-8.45x0.9897)x11.90x100/200.19=98.866 X2=(25x0.9998-7.89x.09897)x11.90x100/210.54=97.139 X3=(25x0.9998-8.38x0.9897)x11.90x100/204.56=97.157 X4=(25x0.9998-8.34x0.9897)x11.90x100/199.85=99.683 = 98.211 STATISTICAL EVALUATION: Range: R = 2.544 Standard deviation (estimated from range): sd = 1.2722563617452 Relative standard deviation: RSD = 1.30% CONCLUSION (does your sample meet/not meet Ph. Eur): yes