EXPERIMENT 5 : DETERMINATION OF ACETYLSALICYLIC ACID IN ASPIRIN USING BACK TITRATION METHOD.

OBJECTIVE To determine the amount of acetylsalicylic acid in aspirin tablet. APPARATUS Weighing boat Filter Funnel Pipette (25mL) Burette Dropper Volumetric flask (250mL) Retort stand and white tile 3 Conical flasks (250mL) CHEMICAL REAGENTS Aspirin tablet 1.0 M NaOH solution 0.1 M HCl solution Phenol red indicator PROCEDURE A. Hydrolysis of Aspirin 1. One aspirin tablet is weight accurately in a weighing boat and this tablet is transferred into a 250 mL conical flask containing 25.0 mL of distilled water. 2. 25.0 mL of 1.0 M NaOH is pipette to the conical flask and this mixture is heated until boiling. The mixture is allowed to boil for about 10 minutes in order to hydrolyse the aspirin. 3. The solution is cooled the solution is transferred quantitatively into a 250 mL volumetric flask and the solution is diluted to the mark with distilled water. B. Back Titration 1. 25.0 mL of the aspirin solution is pipette into a 250 mL conical flask and then 2-3 drops of phenol red indicator is added. 2. The aspirin solution is titrate steadily in the 250 mL conical flask against 0.1 M HCl solution from a burette and the flask in kept swirling until there a colour change. The reading at the end point of the titration is recorded. 3. The titration is repeated until student obtain consistent readings and titration data is recorded in Table 5.0 as shown in datasheet for experiment 5.

C. Blank Titration 1. 25.0 mL of 1.0 M NaOH is diluted with distilled water in a 250 mL volumetric flask. 2. 25.0 mL of the diluted NaOH solution is pipette into a 250 mL conical flask. Then, 23 drops of phenol red indicator is added. 3. The NaOH solution is titrate steadily in the conical flask with 0.1 M HCl solution from the burette and the flask is kept swirling until there is a colour change. The reading at the end point of the titration is recorded. 4. The titration is repeated until student obtain consistent readings and the titration data is recorded in Table 5.1 as shown in datasheet for experiment 5.

RESULTS DATASHEET FOR EXPERIMENT 5 Weight of aspirin tablet = 0.7541 g Commercial name of the tablet is Ispirine. Manufacturer of the tablet is Reckitt Benckiser Health Care (UK) LTD. Date of manufacturer is November 2009. 1. To determine the excess amount of acetylsalicylic acid after hydrolysis of aspirin tablet. Molarity of NaOH solution = 1.0 M Volume of hydrolysed solution = 25.0 mL Table 5.0 : Back titration of excess NaOH with HCl solution Titration number 1 2 3 Burette reading Final reading 24.40 24.50 24.20 Initial reading 0.00 0.00 0.00 Volume of HCl used (mL) 24.40 24.50 24.20 Average volume of HCl used = 24.375 mL 2. To determine the volume of HCl required to react with NaOH solution without any aspirin sample.

4 24.40 0.00 24.40

Table 5.1 : Blank titration of NaOH solution with HCl Titration number 1 2 3 Burette reading Final reading 30.10 30.30 30.20 Initial reading 0.00 0.00 0.00 Volume of HCl used (mL) 30.10 30.30 30.20 Average volume of HCl used = 30.225 mL Reaction : NaOH(aq) + HCl(aq) NaCl(aq) + H2O(l)

4 30.30 0.00 30.20

Calculation : 1. Calculate the no. of moles of NaOH which actually reacting with the acetylsalicylic acid during the hydrolysis. Since 1 mol H+ ions react with 1 mol OH- ions, the no. of moles of NaOH reacting with acetylsalicylic acid in aspirin during hydrolysis, = no. of mol of NaOH blank titration - no. of mol of NaOH back titration = (MHCl VHCl )(blank titration) - (MHCl VHCl)(back titration) = ( 0.10 0.030225) (0.10 0.024375) = 5.85 10-4mol of HCl

2. From equation 1, the mole ratio of NaOH reacting with acetylsalicylic acid is given as no. of moles of NaOH = 2 (no. of moles of acetylsalicylic acid). Calculate the no. of moles of acetylsalicylic acid hydrolysed. = CH3COO-C6H4-COOH = 1 NaOH 2 CH3COO-C6H4-COOH = 1 5.85 10-4 2 CH3COO-C6H4-COOH = 2.925 10-4 mol

3. Calculate the mass of acetylsalicylic acid. Mass = mol RMM = 2.92510-4 180 =0.05265 g

4. Calculate the % (w/w) of acetylsalicylic acid present in your aspirin tablet. = 0.05265 100 0.74150 =7.10%

DISCUSSION The apparatus is set up to determine the amount of acetylsalicylic acid in aspirin tablet. The aspirin tablet is weigh accurately and the weight of aspirin is 0.7541 g. The molarity of NaOH used is 1.0 M. The average volume of HCl used in back titration is 24.375 mL and the average volume of HCl used in blank titration is 30.225 mL. The conical flask must be

keep swirling while titrate until the colour change from purple to yellowish. The parallex error must be avoid to achieve the accurate reading. The eyes must be perpendicular to the burette reading.

QUESTIONS 1. Tabulate the class result of the % (w/w) of acetylsalicylic acid present in aspirin tablet analysed and determine the confidence limit of the mean of the % (w/w) of acetylsalicylic acid at 95% confidence level. Student 1 2 3 4 Mean, = 5.03+6.48+7.08+8.25 4 = 26.84 4 = 6.71 CL, = Result(%w/w) 5.03 6.48 7.08 8.25

= 6.71 (3.182) (1.16) = 6.71 1.84

2. Comment on the overall result of % (w/w) of acetylsalicylic acid obtained. -The result obtained is different because have the error like systematic error random error -The result also different because have affected by different mass of aspirin tablet.

and

CONCLUSIONS The experimentally obtained value of % (w/w) of acetylsalicylic acid in an aspirin tablet
is 7.10% . The confidence limit of the mean of the % (w/w) of acetylsalicylic acid at 95% confidence level is 6.71 1.84.

REFFERENCES Handout Chapter 1- Introduction : Analytical Chemistry Handout Chapter 2 Evaluation of Experimental Data