Experiment 1 QUANTITATIVE DETERMINATION OF HYDROXYL GROUPS BY VARIOUS METHODS

Aim: To determine the number and percentage of hydroxyl groups by various methods. Chemicals Required: For PThalation: pthalic anhydride in pyridine Aq. Sodium hydroxide o.s N Potassium hydrogen phalati pneopthalein indication Potassium bromate bromide solution 0.2v Sodiumthisulphate 0.1N Starch indicator Potassium iodate Potassium iodide Acetic anhydride Pyridine Sodium hydroxide Axalic acid

For Bromination:

For Acetylation

Procedure: Pthalation: Weigh accurately 0.25mg of glycerol sample containing of about 1.5 molar of hydroxyl groups into 250ml iodine flask and add 50ml pyridine reagent moisten the glass stopper : E=1.22% No. of hydroxylgroups = 1% of hydroxyl groups= Bromination: Sno Contents of Flask Butette Volume of Readings titrane Initial Final 0.0ml 27.08ml 27.08ml Indicator End Point

1.

2.

0.2mg phenol +5ml 10%Naoh Solution +25ml bromate bromide Solution+ConcHCL+Starch Indicator 25ml bromate bromide solution +conc. HCL+starch indicator

Starch

Colourless To Pink color

0.0ml 0.10ml

0.10ml

Titer value=27.7ml Blank=0.10ml

No. of hydroxylgroups = = =10.4 1% of hydroxyl groups= = =47.11% Pyridina and heat it on steam bath for one hour and add 5-6ml of distilled water and shake it occasionally heat the flask for further 4-5 minutes, cool it at room temperature by opening the stopper partially. Rinse the stopper with further 5ml of water and add few drops of phednapthalin indicator Titrate the contents with 0.5N NaoH. (mannital) 0.1N NaoH(Glycerol). Perform blank titration. Bromination: Weigh 0.25mg of phenol. Disolve in 5ml of 10%NaoH solution and dilute the solution to 250ml of phenol solution into 500ml of iodine flask and add 25ml of bromate bromide solution and dilute with 25ml water. Add 5ml of conc.HCL, shake it for 1min and allow to stand for 30min. with occasional shaking. Titrate the free iodine which is equivalent to excess of bromine taken with 0.1N sodium thiosulphate by taking the starch solution as an indicator. Perform the blank titration. Acetylation: Take two 250ml round bottomed flask, mark it as A&B. Take 200-300mg of resorcinol in flask A and add the mixture of acetic anhydride in pyridine of about 10ml into each flask, then heat in water bath for 30min Allow the reaction mixture to cool and add 20ml of water and mix the flask for few minutes and heat it again for 2 min. Cool the contents of each flask at room temp. and allow to stand for 10-15min. Then titral against 1N NaoH solution using phenapthalien as an indicator. (10ml of 1:3 of acetic anhydride in pyridine i.e., 2.5ml of acetic anhydride and 7.5ml of pyridine. Report:

Experiment 2 QUANTITATIVE DETERMINATION OF CARBOXYLIC GROUP IN GIVEN SAMPLE

Aim : To estimate the no of carboxylic groups present in given samples Procedure: Standardisation 0.1N sodium hydroxide: 0.63gm of oxalic acid is taken in 10ml of distilled water and dissolved and made the volume upto 100ml. From this pipette out 20ml into conical flask and add phenopthalein indicator and titrate it against 0.1N sodium hydroxide. Assay: Weigh 0.14gm of unknown sample and add 20ml distilled water and add few drops of phenopthalein indicator and titrate it against 0.1N NaoH.