Engineering Chemistry Lab Manual

(I B.Tech Common to All)

Experiment-1 ESTIMATION OF HARDNESS OF WATER BY EDTA (COMPLEXOMETRY) Aim: To estimate the hardness of the given Sample water using a standard solution of EDTA. Apparatus: 100 ml standard flask, Burette, 250 ml Conical Flask, 20 ml Pipette, & Simple balance with weights, Chemicals Required: Ethylene di-amine tetra acetic acid (EDTA), Solo-chrome (EBT) Indicator, Ammonia Buffer solution, Hard-water & distilled water. Principle: Hard water which contains calcium and magnesium ions forms a wine red colored complex with the indicator, Eriochrome Black-T. Ethylene diamine tetra acetic acid (EDTA) forms a colourless stable complex with free metal ion like Ca, Mg. i.e., Metal + Indicator Metal indicator complex (wine red colour) When EDTA is added from the burette, it extracts the metal ions from the metal ion-indicator complex thereby releasing the free indicator. (The stability of metal ion-indicator complex is less than that of the metal ion- EDTA complex, and hence EDTA extracts metal ion form the ion-indicator complex.) EDTA + Metal indicator complex Metal ion-EDTA + Indicator (Wine red color) (Blue) The reactions take place at a pH = 10 and the buffer is made by ammonium chloride and ammonium solution. Procedure: Preparation of standard hard water: Dissolve 1g of pure, dry CaCO3 in minimum quantity of dil.HCl and then evaporate the solution to dryness on a water bath. Dissolve the residue in distilled water to make 1 Liter solution. Each mL of this solution thus contains 1mg of CaCO3 equalent hardness. 1 mL hard water solution = 1mg of CaCO3 equivalent hardness. Standardization of EDTA solution: Rinse and fill the burette with EDTA solution. Pipette out 50 mL of standard hard water in a conical flask. Add 10-15 mL of buffer solution and 4 to 5 drops of EBT-indicator. Titrate with EDTA solution till wine-red colour changes to clear blue. Let volume EDTA solution used be V1 mL. Titration of Unknown Hard water: Rinse and fill the burette with EDTA solution. Pipette out 50 mL of Sample hard water in a conical flask. Add 10-15 mL of buffer solution and 4 to 5 drops EBT-indicator. Titrate with EDTA solution till wine-red colour changes to clear blue. This marks the end point of the titration. Repeat the titrations for constant titer values. Let volume of EDTA solution used be V2 mL. __________________________________________________________________________________ SV Group of Institutions 1

Engineering Chemistry Lab Manual (I B.Tech Common to All) Titration of Permanent hardness: take 250 mL of the water sample in a large beaker. Boil it. Till the volume is reduced to about 50 mL, filter it, wash the precipitate with distilled water, collecting filtrate and washing in a 250 mL measuring flask. Finally makeup the volume to 250 mL with distilled water. Rinse and fill the burette with EDTA solution. Pipette out 50 mL of Boiled hard water in a conical flask. Add 10-15 mL of buffer solution and 4 to 5 drops EBT-indicator. Titrate with EDTA solution till wine-red colour changes to clear blue. This marks the end point of the titration. Repeat the titrations for constant titer values. Let volume EDTA solution used by V3 mL.

Preparation of primary Standard hard water solution: Molarity (M) = Weight of CaCO3 X 1000 M. Wt of CaCO3 1000 Weight of CaCO3 = M X M. Wt of CaCO3 Dissolve ________ grams of pure, dry CaCO3 in minimum quantity of dil.HCl and then evaporate the solution to dryness on a water bath. Dissolve the residue in distilled water to make 1 Liter solution. Each mL of this solution thus contains 1mg of CaCO3 equalent hardness. 1 mL hard water solution = 1mg of CaCO3 equivalent hardness. Standardization of EDTA using standard hard water S.No Volume of Standard Hard water (ml) Vs 1 10 ml 2 3 10 ml 10 ml Vs = 10 ml V1= V1= 10 ml (10 ml Standard hard-water reacting with 10 ml 0.01M EDTA solution) Titration of Sample Hard water: S.No Volume of Sample Hard Burette Reading water (VH) Initial Final 1 50 ml V1 = Burette Reading Initial Final Volume of EDTA solution consumed (V1)

Volume of EDTA solution consume (V2)

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Engineering Chemistry Lab Manual 2 50 ml 3 50 ml VH = 50 ml V1= V2 = Total hardness of water V2 =

(I B.Tech Common to All)

= 1000XV2 V1 Estimation of total hardness present in water sample: Molarity of EDTA = M Indicator EBT Colur change Wine red to Pale blue 50 ml of water sample + 2 ml buffer solution + 1 drop EBT S.No Volume of water sample taken(ml) 1 50 ml 2 50 ml 3 50 ml VB = 50 ml V3 = Burette Reading Initial Final Volume of EDTA solution consume (V3)

V1= 50 ml V3 = Permanent hardness = 1000XV3 V1

Temporary hardness = 1000 X [(V2-V3)] = V1

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Engineering Chemistry Lab Manual

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Result: The Temporary hardness of the given water sample _________ ppm. The Permanent hardness of the given water sample _________ ppm. The Total hardness of the given water sample _________ ppm.

Experiment-2

DETERMINATION OF PERCENTAGE OF COPPER IN BRASS

MINERAL ANALYSIS (IODOMETRY) Aim: To determinate the percentage of Copper present in the given Brass sample using a standard solution of Potassium Dichromate and Hypo as the link solution. Apparatus: 100 ml standard flask, Funnel, Burette, Iodometric flask, Conical Flask, 20 ml Pipette & Simple balance with weights, Chemicals Required: Brass sample, Potassium Dichromate (K2Cr2O7), Hypo (Na2S2O3), Potassium Iodide (KI), 6N Conc.HNO3, NaHCO3, 6N Sulphuric Acid (H2SO4), Syrupy Phosphoric Acid (H3PO4), Ammonia solution, Potassiun thiocyanate (KSCN) Starch & distilled water. Principle: Brass in an alloy which consists mostly of copper (60 to 80 %) and zinc ( 20 to 40% ) along with small amounts of lead ( 0 to 2% ) , tin ( 0 to 6% ) and iron ( 0 to 1% ). The experiment consists of dissolving a known quantity of brass in nitric acid, removing the nitrate by fuming with sulfuric acid, adjusting the pH by ammonium hydroxide, complexion the iron present using phosphoric acid, and finally titrating the copper ions with hypo by the iodo-metric method. __________________________________________________________________________________ SV Group of Institutions 4

Engineering Chemistry Lab Manual (I B.Tech Common to All) When the brass sample is dissolved in nitric acid, the copper present is brought into solution in the form of cupric ions. At the same time, tin is converted to meta-stannic acid (SnO2.4H2O ), lead and zinc are oxidized to their respective soluble divalent ions, while iron is converted to ferric ions. During the treatment with sulfuric acid, nitrate is eliminated, the meta-stannic acid is re-dissolved and lead ions are precipitated as PbSO4 while all other metals go into solution as their respective sulfates. Out of all the metal ions present in solution, only Cu2+ and Fe3+ are reducible by iodide. The interference by iron is eliminated by titrimetrically determined by the iodometric method. Chemical reactions: 2Cu2+ + 4I- 2CuI + I2 2S2O3 + I2 S4O6- + 2ICu = I = S2O3Procedure: 1. Preparation of standard potassium dichromate: Weigh out accurately about 0.490 gm or 490 mg of the given pure crystalline sample of potassium dichromate and transfer into 100 ml standard (volumetric) flask provided with a funnel. Dissolve the dichromate in a small quantity of distilled water, and make upto the mark. The contents in the flask are shaken well for uniform concentration. Calculate the normality of potassium dichromate. 2. Standardization of sodium thiosulphate: Rinse the burette and fill it up with hypo solution without any air bubbles. Note the burette reading. Take about 20 ml of 10%KI solution in a clean conical flask and add 2 grams of sodium bicarbonate followed by 5 ml of concentrate HCl gently rotate the flask for mixing the liquids. Rinse the pipette with a little of potassium dichromate solution and then transfer 20 ml of the same to the conical flask. Shake it well, stopper it, and keep it in dark place for 5 minutes. Titrate the liberate iodine by running down hypo from the burette with constant stirring. When the solution attains a pale yellow colour add 2 ml of freshly prepared starch solution. The colour changes to blue. Continue the titration drop-wise till the colour changes from blue to light green indicating the end point. Repeat the titration for concurrent values. 3. Estimation of copper: About 0.25 g or 250 mg of clean and dry brass sample is accurately weighed and transferred into a conical flask. Add bout 10ml of 6 N HNO3 and the flask is gently heated until the brass sample is completely dissolved. Then 10ml of conc. H2SO4 added and the solution is evaporated on a sand bath to copious white fumes. The mixture is then allowed to cool and 20ml of water very carefully add from the sides of the flask, in instalments of 1ml at a time while cooling under a tap. Boil the solution for 2 minutes and cool. Add liquor ammonia drop-wise while shaking the flask vigorously until the appearance of blue cupric ammonium complex. Now, 6N H2SO4 is slowly added drop wise until the dark Blue colour disaapears. Then add 2 ml of syrupy phosphoric acid is added. The solution is cooled and transferred to a 100ml volumetric flask. The volume is made up to the 100ml mark using distilled water. 25 ml of this solution is pipette out into a 150ml conical flask and add about 1 g of solid (KI) potassium iodide. The flask is shaken and the solution is immediately titrated with standard sodium thio-sulphate solution until the solution assumes a faint yellow colour of iodine. About 3 ml of 1% starch solution are added and the titration is continued until the blue colour begins to fade. At this stage, about 0.5g or 500 mg of potassium thiocyanate (KCNS) is added and the titration is continued until the blue colour just disappears. The titration is repeated twice with fresh 25ml portions of the solution to confirm the titer value. 4. Weight of Brass Sample (B): __________________________________________________________________________________ SV Group of Institutions 5

Engineering Chemistry Lab Manual (I B.Tech Common to All) W1 = Weight of bottle + Brass sample = ____________ gms W2 = Weight of bottle = ____________ gms Weight of Brass Sample = B = (W1-W2) = ____________ gms. Weight of the Brass Sample = B = 5. Preparation of Standard (K2Cr2O7)solution: W1 = Weight of bottle + substance = ____________ gms W2 = Weight of bottle = ____________ gms Weight of substance = (W1-W2) = ____________ gms. Normality of the solution = (W1-W2) X 10__ = (W1-W2) X 10 Equivalent Weight 49 S.No Volume of standard (K2Cr2O7)solution (V1) 1 2 3 20 ml 20 ml V2 = Burette Reading Initial Final Volume of consume (V2) =

20 ml V1 = N1 = Normality of Potassium dichromate = V1 = volume of Potassium dichromate = 20 ml N2 = Normality of Hypo =? V2 = Volume of Hypo = N1V1 = N2V2 N2 = N1V1 = V2 N2 = Normality of Hypo = S.No Volume of Copper solution (V3) 1 2 3 20 ml 20 ml 20 ml V3 = 20 ml Burette Reading Initial Final

Volume of consume (V4)

V4 =

N3= Normality of Copper solution = ? V3 = volume of Copper Solution = 20 ml N4 = Normality of Hypo = V4 = Volume of Hypo = __________________________________________________________________________________ SV Group of Institutions 6

Engineering Chemistry Lab Manual N3V3 = N4V4 Normality of Copper solution = N3= N4V4 V3

(I B.Tech Common to All)

The amount of copper present in the solution can be calculated on the basis that 1ml of 1N Na2S2O3 = 0.06354 g of Cu. Amount of Copper present in the whole of the given solution (100 ml) = Z = N3 X 63.54 100 Weight of the Brass Sample = B = Percentage of Cu in the brass sample : (% of Cu in brass) = Z X 100 B Result: Percentage of Copper present in the whole of the given Brass sample(100 ml) = ______ %. Experiment-3 ESTIMATION OF MANGANESE DIOXIDE IN PYROLUSITE. MINERAL ANALYSIS Aim: To estimate the amount of MnO2 present in the given sample and hence percentage purity of Pyrolusite. Apparatus: 100 ml standard flask, Burette, Conical Flask, 20 ml Pipette, Funnel, Simple balance with weights, Heating equipment. Chemicals Required: Pyrolusite, 4N Sulphuric acid (H2SO4), 0.1 N Di Sodium oxalate solution, 1M Sulphuric acid (H2SO4), Potassium permanganate (KMnO4), Distilled water. Principle: The MnO2 present in the pyrolusite sample is reduced by a known excess of standard sodium oxalate in acid medium. The unreacted sodium oxalate is titrated against a standard KMnO4, until pale pink coloured end point is obtained. MnO2 + H2SO4 + H2C2O4 2CO2 + 2H2O + MnSO4 1ml of 1N KMnO4 = 1 ml of 1N Na2C2O4 = 0.04346 gm of MnO2 = 0.01099 gm of Mn 1 ml of 1N KMnO4 = 1 ml of 1N As2O3 = 0.04346 gm of MnO2 Preparation of Standard Di-Sodium Oxalate solution: Weigh accurately 0.67 gm of Di-Sodium Oxalate and transfer into 100 ml standard flask through a funnel. Dissolve the compounds small __________________________________________________________________________________ SV Group of Institutions 7

Engineering Chemistry Lab Manual (I B.Tech Common to All) amount of distilled water and make up to the mark with distilled water. Shake the flask vigorously for uniform standard Di-Sodium Oxalate solution. Standardization of KMnO4 solution: Take 25 ml of the 0.1N sodium oxalate solution in a conical flask, add 150 ml of 1M H2SO4 solution. Titrate with the KMnO4 solution at room temperature until the faint pink colour appears. Warm the solution to 60 to 700 C and continue the titration to a faint permanent pink colour. Estimation of MnO2: Weigh out accurately about 0.2 gm or 200 mg of the given powdered pyrolusite sample into a clean dry conical flask and add 50 ml of standard sodium oxalate solution and add 50 ml of 4N (H2SO4) sulphuric acid, put a small funnel into the mouth of the conical flask. Heat with small flame till particles are MnO2 disappear in the conical flask. Rinse the funnel with distilled water into the conical flask, titrate the hot solution, containing the unreacted sodium oxalate with standard KMnO4 solution till there is a pale pink colour. Result: Percentage purity of the given sample of Pyrolusite = Preparation of Standard sodium oxalate solution: W1 = Weight of bottle + substance = ____________ gms W2 = Weight of bottle = ____________ gms

Weight of substance = (W1-W2) = ____________ gms. Normality of the solution = (W1-W2) X 10 = __________X 10 Equivalent Weight 67

Standardization of KMnO4 solution: S.No Volume of Burette Reading standard di Final sodium oxalate Initial solution (V1 ) 1 2 3 25 ml 25 ml 25 ml V1= N1 = Normality of di sodium oxalate = V1 = volume of di sodium oxalate = 25 ml

Volume of KMnO4consume (V2)

V2 =

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Engineering Chemistry Lab Manual N2 = Normality of KMnO4 =? V2 = Volume of KMnO4 = N1V1 = N2V2 N2 = N1V1 = V2 N2 = Normality of KMnO4 =

(I B.Tech Common to All)

Weight Of the Pyrolusite Sample: W1 = Weight of bottle + Pyrolusite = ____________ gms W2 = Weight of bottle = ____________ gms

Weight of Pyrolusite = (W1-W2) = ____________ gms.

S.No Volume of standard solution 1 2 3 50 ml 50 ml 50 ml

Burette Reading Initial Final

Volume of consume (V)

V= Calculations: Weight of the Ore taken = Volume of 0.1N Di sodium oxalate solution added in the experiment = 50 ml Volume of 0.1N KMnO4 run down = V = Volume of 0.1N KMnO4 consumed = (50 V) = 1 ml of 1N KMnO4 = 1N Na2C2O2 = 0.04346 g of MnO2 __________________________________________________________________________________ SV Group of Institutions 9

Engineering Chemistry Lab Manual

(I B.Tech Common to All)

Percentage of MnO2 = (50 - V) X Normality of KMnO4 X 0.04346 X 100 Weight of the sample

Result: Percentage purity of the given sample of Pyrolusite = Experiment-4 DETERMINATION OF FERROUS IRON IN CEMENT BY COLORIMETRIC METHOD (Colorimetric Estimation) Aim: To estimate the amount of Iron (Ferric) present in a sample of cement by calorimetrically using ammonium thiocyanate as a reagent. Apparatus: 250 ml beaker, Glass rod, Watch glass, 100 ml standard flask, Burette, 10 ml Pipette, Simple balance with weights Colori-meter, Heating-equipment. Chemicals Required: Cement sample, Conc. Nitric acid (HNO3), Hydrochloric acid (HCl) Ammonium thio-cyanate & Distilled-water. Principle: Ammonium thio-cyanate yields a blood red colour with ferric iron and the colour produced is stable in nitric acid medium. Its optical density is measured in a photo colorimeter and the concentration of ferric iron is found from a standard calibration curve. Procedure: 1. Dissolution of the sample: Weight out accurately about 0.1 gram of the cement sample into a clean 250 ml beaker add about 5 ml of water to moisten the sample. Place a glass rod and cover the beaker with a watch glass add about 5 ml conc. Hydrochloric acid (HCl) drop-wise and heat the solution till the sample dissolved. Keep the beaker on a small flame and evaporate the solution to almost dryness to expel the excess acid. __________________________________________________________________________________ SV Group of Institutions 10

Engineering Chemistry Lab Manual (I B.Tech Common to All) Take the beaker out of the flame and add about 20 ml distilled H2O to dissolve the contents. Transfer the solution into 100 ml standard flask. Wash the beaker twice with small portions of distilled water, and add the washings to the standard flask. Make up the solution to 100 ml with distilled water. Shake the flask well uniform concentration. 2. Development of Colour: pipette out 10 ml of the solution prepared above, into a 100 ml standard flask, add 1 ml of conc. Nitric acid (HNO3) and 5 ml of 40% ammonium thiocyanate. Make up the solution to 100 ml with distilled water and shake the flask well for uniform concentration. Find out the optical density of the solution using the photo colorimeter and the concentration of the ferric iron from the calibration curve. Result: Percentage of Ferric iron present in the cement sample = Weight of the sample: W1 = Weight of bottle + sample = ____________ gms W2 = Weight of bottle = ____________ gms

Weight of sample = (W1-W2) = ____________ gms.

Standard value for calibration curve Concentration in Milligrams 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 O. D 0.11 0.22 0.32 0.40 0.50 0.62 0.70 0.80

X = corresponding amount of from the calibration curve = Calculation: Percentage of Fe3+ present in the given cement sample = X x 10 x 100 __________________________________________________________________________________ SV Group of Institutions 11

Engineering Chemistry Lab Manual (W1 W2) mg

(I B.Tech Common to All)

Result: Percentage of Ferric iron present in the cement sample =

Experiment-5 CONDUCTOMETRIC TITRATION OF STRONG ACID Vs STRONG BASE (CONDUCTOMETRY) Aim: To estimate the amount of HCl present in given solution. Apparatus: Conductivity meter, Conductivity cell, Burette, Pipettes, Beakers, stirrer. Chemicals Required: Pure sample of Oxalic acid, 0.02M HCl and 0.1M NaOH. Theory: Electrolytic conductivity is a measure of the ability of a solution to carry electric current. Solutions of electrolytes conduct electric current by the migration of ions under the influence of applied field. Like metallic conductors they obey ohms law. At a given temperature the conductivity depends upon the concentration of the electrolyte. Conductivity cell: The electrolytic conductance of an electrolyte is measured in conductivity cells, which are specially designed. These are available in various sizes and shapes consisting of 2 electrodes. Each electrode is a pH disc or plate coated with finely divided Pt black. The electrode is welded to a Pt wire which is fused to a glass tube. The glass tubes are firmly fixed in the cell so that the distance between the electrodes would not change during the experiment. The cell is open at one end; the electrolyte whose conductivity is to be measured is dissolved in water and is taken in a beaker. The conductivity cell is placed in the solution and is connected to the conductometer. Cell constant X: X of a conductivity cell is the ratio of distance between the 2 electrodes and the exposed area of one of the electrodes. X=1 a Specific conductance: It is the conductance of ions present in one cubic centimeter of the solution. If the cell constant of a conductivity cell is 1.0 the measured conductivity of an electrolyte is its specific conductivity. The cell constant of a conductivity cell is seldom 1.0 cm-1, also measuring l and a are troublesome. Hence the given cell is calibrated for its cell constant, with the help of an electrolytic solution normally, a standard KCl whose specific conductivity is known. Cell constant = known specific conductance / measured conductance Principle: The electrical conductance of an electrolytic solution is proportional to a) the ionic concentration i.e. number of ions present in the solution and b) the ionic mobilies. The ionic motilities __________________________________________________________________________________ SV Group of Institutions 12

Engineering Chemistry Lab Manual (I B.Tech Common to All) -4 -1 in aqueous solutions are generally of the order of 6.0 x 10 cm2, sec volt-1. But the ionic mobilities of H+ and OH- are abnormally high, H+ = 36.3 x 10-4 and OH- = 20.5 x 10-4 cm2 sec-1 volt-1. Thus the conductance of an electrolyte is quite sensitive to concentration of H+ and OH- ions. Titration of strong acid HCl with strong base NaOH: In solution HCl is completely ionized. The mobility of H+ ions is high; hence the conductance of HCl solution will also be high. As NaOH is added to HCl, the fast moving H+ ions are removed by OH- ions of the base as water. H3O+ + OH- = 2H2O + In solution water is little ionised and Na added are slow moving compared to H+ ions of acid. Hence as the titration proceeds, the conductance of titrand HCl decreases gradually till the equivalent point is reached. At the equivalence point the conductance of the solution will be the minimum addition of the base beyond end point adds Na+ and fast moving OH- ions, resulting in a gradual increase in conductance. Standardization of NaOH solution: Pipette out 20 ml of prepared NaOH solution in a conical flask. Add 1-2 drops of methyl orange indicator and titrate against standard oxalic acid solution. Determination of Cell constant: Take a conductivity cell and determine its cell constant using a 0.1 N KCl solution. Conduct metric titration: The burette is rinsed and filled with 0.1 M NaOH, 40 ml of given acid is placed in a 100 ml beaker. The cell is washed with conductivity water which is placed in HCl solution and see that the electrodes of cell are completely immersed in the solution. The cell is fixed in a cell holder and is connected to the conductivity bridge. The conductance of HCl solution is noted at a time when 1 ml of NaOH from the burette is added into HCl solution. After each addition the solution is stirred gently with a glass rod and the conductance of HCl is noted. The titration is continued till 20 to 25 ml of NaOH is added. Graph: Plot a graph between the conductances measured on Y-Axis and volume of alkali added (XAxis) we get a V shaped graph the point of intersecting will be the End-Point of titration and will determines the volume of alkali required for neutralization of the acid. Preparation of Standard Oxalic acid solution: W1 = Weight of bottle + substance = ____________ gms W2 = Weight of bottle = ____________ gms Weight of substance = (W1-W2) = ____________ gms. Normality of the solution = (W1-W2) X 10 = __________X 10 Equivalent Weight 63.03 Standardization of NaOH solution: S.No Volume of Burette Reading standard oxalic Initial Final acid solution (V1 ) 1 2 3 25 ml 25 ml 25 ml Volume of NaOH consume (V2)

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Engineering Chemistry Lab Manual V1= N1 = Normality of Oxalic acid = V1 = volume of Oxalic acid = 25 ml N2 = Normality of NaOH =? V2 = Volume of NaOH = N1V1 = N2V2 N2 = N1V1 = V2 N2 = Normality of NaOH = V2 =

(I B.Tech Common to All)

S.No 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23

Volume of NaOH solution added (ml) 0.0 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0 14.0 15.0 16.0 17.0 18.0 19.0 20.0 21.0 22.0

Conductivity of the solution (ohm-1)

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Engineering Chemistry Lab Manual

24 25 26 23.0 24.0 25.0

(I B.Tech Common to All)

Volume of the Hydrochloric acid (HCl) used = 40 ml Volume of NaOH required to reach Equivalent Point = V = Normality of NaOH = Strength of HCl = End point titer valve (V) X Normality of NaOH = Volume of HCl used Result: The strength of HCl calculated is __________ N. Experiment-6 TITRATION OF STRONG ACID VS STRONG BASE BY POTENTIOMETRY
(POTENTIOMETRY)

Aim: To estimate the amount of HCl present in given solution. Apparatus: Saturated calomel electrode, Platinum electrode, Quinhydrone electrode, Potentiometer, Salt bridge, Burette, Pipette, Beakers & glass rod etc. Chemicals Required: Pure sample of Oxalic acid, 0.1M HCl and 0.1M NaOH. Principle: Quinhydrone (Q) is an equi-molar mixture of quinine C6H4O2 and Hydroquinone C6H4(OH)2. In acidic medium the following redox equilibrium is established. Q +2H+ + 2e- -- QH2 A pinch of quinhydrone added to an acid solution and a Pt wire or foil dipped in it constitutes a half cell such electrodes are called indicator electrodes. This is coupled with a reference electrode through a salt bridge making it an electrochemical cell. Ex: (-)saturated calomel electrode / salt bridge / Qunihydrone + Acid solution / Pt + (or) (-) Pt, Hg / Hg2Cl2 (s) / KCl (saturated) // H+ , QH2, Q/Pt (+) CELL REACTION: 2 Hg(s) + Q + 2Cl-(aq) - Hg2Cl2(s) + QH2 Ecell = Eright Eleft in terms of reduction potentials Ecell = EQE 0.242 ---------(1) The left hand half cell is fixed i.e., its potential is constant. Now the right hand half cells potential depends on H+ activity. The fundamental equation governing the effect of activity of the ions on the voltage of an electrode or a cell is Nernst equation given by Ecell = Ecell - (RT / nF ) lnk Where k is equilibrium constant of a general reaction aA + bB - cC + dD The potential will be EQE + nE0QE (RT /2F ) ln (QH2) / (Q) (H+)2 __________________________________________________________________________________ SV Group of Institutions 15

Engineering Chemistry Lab Manual EQE = E0QE + 0.0591 log (H+) 0.242 Ecell = 0.458 0.0591 pH

(I B.Tech Common to All)

During the titration, against and alkali, H+ ion concentration in the half cell containing QH2 will decrease correspondingly the Ecell decreases. The emf will change slowly in the beginning how ever at the end point relatively higher potential difference will be obtained and then again it will change slowly. After the end point 5 or 6ml more of the bas is added, quickly and EMF is recorded. Repetition of titration is done by adding 0.2ml of Na OH at a time near the end point. A graph is plotted between EMF and volume of base added. The point of inflection where the graph changes its direction is the end point. A differential plot of ( E/ V) against V* give s a curve whose peak indicates equivalent point. PROCEDURE: 1) Calibrate the instrument before starting the experiment. 2) Take 20 ml of acid solution in a 100 ml beaker and immerse the pH electrode in to the solution. 3) Firist carry out the rough titrations by adding 1 ml of NaOH and measure the EMF at each stage. 4) After finding the range of end point, then take fresh sample of acid solutions in a beaker and carry our the titrations repeatedly by adding 5 ml, 3ml, 2ml, 0.5ml, 0.2ml and 0.1ml successively. 5) After the end point, the volume of alkaline added is increased to 1 or 2 ml. Near the end point smaller addition should be added by micro burette. 6) Plot pH values or EMF values against the volume of NaOH added. Draw a smooth curve, the point of intersection gives the equivalence point. 7) Plot another graph between E / V values against the titre readings abscissa. The maximum of the curve represents the equivalence point. Graph: Plot a graph between cell EMF on Y-Axis and Volume of NaOH on X-Axis. For getting the exact neutralization point another graph drawn E/ V Vs Volume of NaOH from this graph the volume required for neutralization is known.

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Engineering Chemistry Lab Manual

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TABLER FORM:

S.No 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26

Volume of NaOH (ml) 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25

EMF value (mv)

E/ V

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Engineering Chemistry Lab Manual Volume of NaOH (Eqv.point) = Normality of NaOH = Volume of HCl taken =

(I B.Tech Common to All)

Normality of HCl = volume of NaOH (Eqv.point) X Normality of NaOH Volume of HCl taken

RESULT: the normality of HCl by titrating with NaOH using potentiometer is ________ N . Experiment-7 DETERMINATION OF VISCOSITY OF SAMPLE OIL BY REDWOOD VISCOMETER. OBJECTIVE:1. To determine the Absolute and Kinematic Viscosities of a given sample of oil at various temperatures starting from room temperature. 2. To draw the following graphs. Absolute viscosity Vs Temperature.
Kinematics Viscosity Vs Temperature.

APPARATUS:Red wood Viscometer-I, Thermometers 2No. (0--1100), Stop watch, Measuring flask (50ml), Energy regulator and sample oil.

THEORY:Viscosity is one of the important properties of a lubricant, which helps in selection of oils for their suitability for lubricating purposes. A lubricant when used is aimed at reducing friction between different moving parts of a machine by avoiding direct metal-to-metal contact. The thin film of oil, formed between the moving surfaces, keeps them apart and thus the frictional resistance is entirely on account of the shearing of the liquid. The viscosity of the fluid measures the amount of the internal friction. The objective of this experiment is determining the viscosities, therefore, is to ascertain whether the oil is sufficiently viscous, under the high pressure and temperature conditions of the __________________________________________________________________________________ SV Group of Institutions 18

Engineering Chemistry Lab Manual (I B.Tech Common to All) machine, to adhere to the bearing. The variation of viscosity with temperature is of great importance to the engineer in all problems of fluid flow and fluid friction and also in pumps, fans and all types of bearings. Absolute Viscosity:It is the shear force required to move a layer of the oil of one-centimeter thickness over an area of one square centimeter thickness. In C.G.S system it is expressed in poise and in SI system it is expressed in 1N-Sec/m2 1N-Sec/m2 = 10 poise; dyne-sec/cm2=poise Kinematic Viscosity:The ratio of Absolute Viscosity to the density is called Kinematic Viscosity. In C.G.S system it is expressed in Stokes and in SI system it is expressed in m2/sec 1m2/sec = 104 stokes; stoke = cm2/sec Effect of temperature on Viscosity: Increase in temperature causes a decrease in the viscosity of a liquid; where as viscosity of gases increase with temperature the viscous forces in a fluid are the outcome of inter molecular cohesion and molecular momentum transfer. In liquids the molecules are comparatively more closely packed, molecular activity is rather small and so the viscosity is primarily due to molecular cohesion. Since the rate, at which a fluid will flow through an aperture, increase as the internal friction of the fluid decreases, the rate of flow through an orifice or short tube may be used as a means for measuring viscosity. This is the principal involved in Redwood Viscometer-I, which is used in United Kingdom for measuring viscosity. The time in seconds required for 50ml of oil to gravitate through the Redwood Viscometer at a given temperature is expressed as its viscosity in Redwood seconds at that temperature. The Kinematic and Absolute viscosities can be determined from Redwood seconds by using the following formulae Kinematic Viscosity () = At B/t Absolute Viscosity () = . Where A and B are constants, t is Redwood seconds and is the density of the fluid. Redwood Viscometer-I is used for determining the viscosity for low viscosity oils. It has an orifice of diameter 1.62 mm with a length of jet of 10mm. The values of A and B for Redwood Viscometer-I are as follows Viscosity range in R.I A B seconds 40-85 0. 264 190 85 to 2000 0. 247 65 DESCRIPTION OF APPARATUS: The Redwood Viscometer consists of a heavily silver plated oil cup with a dish shaped bottom with a standard hole in hemispherical seating. A spherical ball valve is placed to close __________________________________________________________________________________ SV Group of Institutions 19

Engineering Chemistry Lab Manual (I B.Tech Common to All) the orifice. The oil cup is surrounded by a bright chrome plated water bath. The water bath is mounted on a stand with leveling screws. The level to which the oil is to be filled into the cup is given by an index fixed to the inside wall of the oil cup. A standard size stainless steel jet is fitted at the center of the bottom of the cup for the flow of oil to be measured. The cylindrical water bath is provided with a tap for emptying. The water bath surrounding the oil cup provided with three vanes, having their upper and lower positions rotated in opposite directions to facilitate stirring, which is carried out manually. For ascertaining the level of equipment a flat circular spirit level is used. The flow of oil is regulated by the ball value. The oil cup cover is fitted with an insulated handle, and has suitable arrangement to facilitate thermometer and value rod. The circular spirit level is mounted on a plate to fit on the upper end of the oil cup. PROCEDURE:i. Clean the oil cup and dry it. Examine the jet and ensure that it is clean and not obstructed. ii. Mount the bath on the stand and level it with the help of spirit level and leveling screws. iii. Fill the water bath with water until the heating element is below the water surface. Fill the oil cup with oil up to the mark. iv. Fix the thermometers in the provided space intended for measuring water and oil temperatures. v. Press the connector to the water bath heater pin and the three-pin plug to the plugged to the socket of the energy regulator box. The three-pin plug from the energy regulator is connected to the socket of the main supply. Keep the energy regulator knob at the eighty marks and switch ON the main supply.
vi. Water gets heated and the water temperature reaches 600C stir them well and ensure that the

water and oil temperature are nearly equal. vii. Place the clear dry 50ml receiving flask centrally below the jet with the top of the neck a few mm from the bottom of the jet. Open the orifice by lifting the ball valve and note the time taken for the collection of 50ml oil with the help of stop watch. Note down the time taken is seconds for the oil to get filled in the flask up to the red mark also note down the water and oil temperature repeat the procedure for various temperatures using the same oil and tabulate the readings.

OBSERVATIONS:-

Type of oil used:

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Engineering Chemistry Lab Manual Calculation of Density: S.NO Weight of the empty jar W1 g Weight of the jar with fluid W2 g Volume of the jar in cc

(I B.Tech Common to All) Net weight of fluid W= W2- W1 g Density = W/V g/cc

1 2 3 4 5

S.No

Temperature in 0C Water Oil

Density of oil (g/cc)

Time taken in Sec.

Kinetic Viscosity in Stokes

Absolute Viscosity in poise

1 2 3 4 5

SAMPLE CALCULATIONS:-

The values obtained are

Temperature of the oil =

Density ( ) of the oil =

Time for filling the 50ml of the oil = __________________________________________________________________________________ SV Group of Institutions 21

Engineering Chemistry Lab Manual Then Kinematic Viscosity () = At B/t centistokes Where A & B are viscometer contains

(I B.Tech Common to All)

A = 0.26, B= 171.5, t = time in seconds for collection of 50 ml of oil in the flask

The Absolute Viscosity = kinematic viscosity X Density = X in centipoises

Experiment-8

DETERMINATION OF SURFACE TENSION

Aim: To determine the effect if soap and detergent on the surface tension of water using a Stalagmometer Apparatus: 1. Stalagmometer 2. Volumetric flask 3. Small rubber tubing 4. Screw type pinch cock Chemicals: 1. Detergent solution 2. Soap solution Principle: The size of the drop falling off from the end of tube depends on the surface tension of the liquid and the size of the capillary end, which provides the line of attachment for the drop. Thus when a liquid is allowed to flow through a capillaty tube, a drop will increase in size to a certain point and then fall off. The total surface tension supporting the drop is 2r where r is the radius of the outer circumference of the dropping end of the capillary tube. It is along this line that liquid, glass and air meet and the force acting along the circumference, hence W = 2r , where W is the weight of the drop and 2 r is the circumference of the external wall of the capillary tube. The surface tension of the liquid can therefore be determined from the weight of a single drop and the external radius of the dropping tube. If we have two liquids such that W1 = 2 r 1 and W2 = 2 r 2 then W1/W2 = 1/ 2 Thus the drop weight method can be employed for comparing the surface tension of two different liquids. However, it is easier to count the number of drops formed by equal volumes to two liquids than finding the weight of a single drop. For two different liquids, the weights of equal volumes are proportional to their densities. Let N1 and N2 be the number of drops of liquid produced from the same volume V of the two liquids. Volume of a single drop = V / N1 Weight of a single drop = (V / N1) d1 or 2 r 1 = (V / N1) d1 Similarly for liquid 2 2 r 2 = (V / N2) d2 Where d1 and d2 are the densities of the respective liquids. Dividing these two equations we get 1 / 2 = (N2.d1) / (N1.d2) Procedure: Take a clean and dry Stalagmometer Attach rubber tubing with a screw pinch cock to the upper end of the stalagmometer to control the flow of the liquid and clamp it to a stand. Make marks above and below the bulb with a marker pen if it is not marked. With the help of the rubber tubing, suck distilled water into the stalagmometer till the level rises above the upper mark. __________________________________________________________________________________ SV Group of Institutions 22

Engineering Chemistry Lab Manual (I B.Tech Common to All) Now allow the liquid to flow through the capillary (control the flow rate using the crew pinch cock) and count the number of drops formed (N1) till the liquid level reaches the mark below the bulb. Dilute the given stock soap solution ( 1%) to appropriate dilutions as given below using a burette and determine the number or drops for each of these concentrations. Tabulate the data. Repeat the above procedure for 0.5, 0.1 and 0.05 % of detergent solution also and tabulate it as above. SNo Volume of water + Volume of soap/detergent solution (ml) Concentration of soap/detergent solution Pure water 0.5 % 0.1 % 0.05 % Exp.1 Exp.2 Average (N) Surface tension (dynes/cm)

1 2
3 4

50 + 0 25 + 25 45 + 5 47.5 + 2.5

Calculations: Surface tension of water at 25C = 72 dynes / cm r1 = Surface tension of the reference liquid (i.e., water) r2 = Surface tension of the test liquid r1 = N2.d1 r2 N1.d2

Result : The surface tension of the given liquid = .dynes / cm

Precautions:

Number of drops per minute must be in between 15-20 The lower end of stalagmometer should be free from grease hence wash the stalagmometer first with benzene or NaOH and then with chromic acid. Stalagmometer should be kept in a vertical position.

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Engineering Chemistry Lab Manual

(I B.Tech Common to All)

Experiment-9 IDENTIFICATION OF FUNCTIONAL GROUPS PRESENT IN ORGANIC COMPOUNDS S.No Experiment Observation I PRIMARY TESTS: a) State Solid / Liquid b)Colour Colourless liquid Yellow coloured liquid Colourless solid Brown (or) dark coloured solid (or) liquid c)Odour Pleasant Phenolic Aniline like smell Oil of bitter almond II IGNITION Smoky TEST Non-luminous Charring III Inference Aldehydes, ketones etc., Nitro compound Acids, amides, anilides, carbohydrates, etc., Phenols, aromatic amines etc.,

Nitro compounds Phenols Aromatic amines Nitrobenzene, benzaldhyde Aromatic compound Aliphatic compounds containing low percentage of carbon Compounds such as carbohydrate & its salts get charred on ignition.

SOLUBILITY: Solubility test: One drop of the liquid or small quantity of the solid is dissolved in the following: Experiment Observation Inference a)Ether Insoluble May be carbohydrate/amide/imide/anilide b)Water Soluble, solution is neutral May be carbohydrate to litmus Solution turns blue litmus May be acidic compound red c)Saturated Soluble with effervescence May be Carboxylic acid NaHCO3 and regenerated on solution acidification with dil.HCl Slow effervescence Polyhydric Phenols

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Engineering Chemistry Lab Manual Slow effervescence & solution turns Yellow d)Dilute NaOH No characteristic change solution (changes in the Dissolves readily in the cold are cold & substance is observed & regenerated on adding heated if conc. HCl necessary) Dissolves & solution turns Yellow colour is removed on adding HCl Dissolves readily forming a Yellow or brown solution on boiling Dissolves in cold & solution turns Yellow, Brown & finally dark on shaking Ammonia gas is evolved on boiling Oily drops are formed with aniline like odour on boiling e) Dil. Na2CO3 Soluble with effervescence Soluble without effervescence f) Dil. HCl Soluble and regenerates on adding alkali g) Action of Conc. Blackening with H2SO4: To a small effervescence with the quantity of organic evolution of CO and compound in a dry (or) CO2 & SO2 test tube add conc. Blackening without H2SO4 and note the effervescence change in the code CO and CO2 evolved, and then warm no Blackening gently. IV Test for Un-saturation Experiment a) Action of bromine in CCl4: to 1ml of bromine in CCl4, add drop of the liquid or small quantity of the solid. b)Baeyers Test: Action of dil. KMnO4: Add one drop of the

(I B.Tech Common to All) Nitro phenols Presence of ketones, amines, aromatic nitro compounds Aromatic acids, phenols may be present

Nitro phenols, phenolic aldehydes may be present Carbohydrates may be present Polyhydric phenols may be present

Amides may be present Anilides or Toluidines may be present May be carboxylic acid May be Phenolic Group May be basic compounds like amines Carbohydrates or certain hydroxyl aliphatic acids like Tartaric acid. Polyhydric Phenols like Resorcinol Oxalates (or) Oxalic acid

Observation De-colorisation of bromine without evolution of HBr. No de-colourisation Decolourisation of KMnO4 with Brown ppt.

Inference Un-saturation is present. Saturated compound Unsaturated compound

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Engineering Chemistry Lab Manual liquid or small amount of No decolourisation of the solid to 1 ml of dil KMnO4 KMnO4 c) Br water: 1 ml of Decolurisation Bromine water add a drop of Liquid or small No Decolurisation quantity of solid. S.No Ether H2O NaHCO3 NaOH HCl 1 + + + 2 3 4 5

(I B.Tech Common to All) Saturated compound Unsaturated compound Saturated compound H2SO4

+ + + +

Compound Carboxylic acid Base Hydrocarbon Carbohydrate Neutral Compound

+ + +

+ -

+ -

+ -

+ + -

FUNCTIONAL GROUP ANALYSIS A simple organic compound has one functional group but it may contain two or more functional groups. All these commonly found functional groups have been divided into four groups. The groups correspond to various elements in the organic compounds and are given below. Type Elements present in Organic compound and its functional group compound organic 1. a)C&H Hydrocarbons b) C,H& O Carboxylic acid, phenol and alcohol(-OH),aldehyde, ketone, ether and ester 2. a)C,H&N Amines b)C,H,N& O Amides, nitro compounds & anilides 3. a)Halogens C,H,& X Halogenated hydrocarbons b) Halogens and C,O,AX,O Acid halides,chloral hydrate. 4. C,H,S,O Sulphonic acid ELEMENTAL ANALYSIS C,H and O are considered as basic elements of organic compounds. Other than these three elements, the elements that are most commonly present in organic compounds are nitrogen, sulphur and halogens. The presence of these elements is detected by Lassaignes test. Preparation of sodium fusion extract: Heating procedure for liquids: Gently heat a small piece of freshly cut and dried sodium in an ignition tube in the beginning and then to red hot. Remove the red hot ignition tube from the flame and add one drop of the liquid. Repeat the heating process again until the tube becomes red hot, remove and add another drop of the liquid. Repeat the operation two or three times. Heating procedure for solids: Gently heat a small piece of freshly cut and dried sodium in an ignition tube in the beginning and then to red hot. Remove the red hot ignition tube from the flame and add a few milligrams of solid. Repeat the heating process again until the tube becomes red hot. In the case of solids there is no need to add the compound again. Take 3 to 4 ml of distilled water in a mortar and immerse the red hot ignition tube into water. Grind the ignition tube to pieces with the pestle, filter. Divide the filtrate into three parts and perform the following experiments. __________________________________________________________________________________ SV Group of Institutions 26

Engineering Chemistry Lab Manual Compounds containing: C,H,N,O,S, Halogen (X) + Na NaCN + NaOH + Na2S = NaX Experiment Lassaignes Test:Test for Nitrogen: To one portion of sodium fusion extract add 2 drops of freshly prepared FeSO4 solution. Boil, cool and acidify with dil.H2SO4 with shaking until the solution is clear. Now add few drops of FeCl3 1) TESTS FOR CARBOXYLIC GROUP (-COOH):
S.NO

(I B.Tech Common to All) Observation Bluish / Green Precipitate / colour Prussian blue colour No colour change Inference Nitrogen present Nitrogen absent

1.

EXPERIMENT Add 1 ml of saturated sodium bicarbonate solution to 1 drop of the liquid or small amount of the solid Dissolve one drop of liquid or small amount of solid in 1 ml aqueous alcohol and moisten the blue litmus paper Esterfication: Dissolve one drop of liquid or small amount of solid in 5 ml of methyl/ethyl alcohol and add 2-3 drops of conc. H2SO4 and warm on water bath and pour the content into NaHCO3/Na2CO3 sol. Phenolphthalein Test: Dissolve 0.2 gms of of the compound in water / alcohol. add a drop of phenolphthalein and well diluted NaOH sol. drop wise

OBSERVATION CO2 gas evolved

2.

INFERENCE Carboxylic acid may be present. No CO2 is evolved Carboxylic acid absent. Blue litmus changes Carboxylic acid may to red. be present. No colour change. Carboxylic acid absent Carboxylic acid presence is conformed

3.

Fruity odour

4.

Pink colour is obtained

Carboxylic acid presence is conformed

2) TETS FOR AMINES (-NH2):

S.NO

1.

2.

3.

EXPERIMENT Carbylamine test: add few drops of chloroform to about 0.2 gms of the compound and add 2-3 ml of ethanolic sodium hydroxide / KOH mix well and warm gently. Nitrous acid test: take 0.2 gms of the given compound is 2 ml of dil. HCl and cool. Now add 10% aqueous NaNO2 sol. Diazotization test: dissolve 0.2 gms of the organic compound in 2-3 ml dil HCl cool under tape water now add 2 ml of 2.5 % NaNO2 solution, cool again and add .5 ml of alkaline beta napthol sol.

OBSERVATION A foul smell of isocyanide is observed, by adding conc. HCl smell can be destroyed. A brisk effervescence is appeared. An orange red or a red dye is appeared.

INFERENCE Amine may be present

Amine presence is conformed. Amine presence is conformed.

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Engineering Chemistry Lab Manual

(I B.Tech Common to All)

3) TEST FOR HYDROCARBONS(C&H): EXPERIMENT 1. Sublimation test: to a few 0.2 gms of the compound of 2 ml of the liquid add 3ml of chloroform and shake well. Then transfer a pinch of AlCl3 into a dry test tube and sublime then add chloroform solution to the sublimed AlCl3 such that the chloroform layer touches the AlCl3.
S.NO

OBSERVATION Red colour is appeared Blue or violet colour is appeared. Green colour is appeared.

INFERENCE Mono cyclic hydrocarbon is conformed. Bicyclic hydrocarbon is conformed. Poly hydrocarbon is conformed.

4) TEST FOR CARBOHYDRATES: S.NO EXPERIMENT OBSERVATION 1. Blackening with H2SO4: heat 0.2 gms Immediately charring and of the compound with 1ml of conc. blackening of the H2SO4 . solution is observed. 2. 2, 4 DNP test: To 0.5 gms of Orange ppt. separates. compound in 1 ml of water add 1 ml of 2, 4 DNP reagents. 3. Molisch test: dissolve 0.2 gms of A deep violet coloured is compound in 4 ml of water and add 3-4 formed at the junction of drops of alcoholic Beta- napthol and two layers. add 2 ml of conc. H2SO4 carefully from the sides of the test tube. 5) TEST FOR CARBONYL COMPOUNDS: S.NO EXPERIMENT OBSERVATION 1. 2,4-DNP test: An orange ppt of 2, 4To 2-3 drops of compound add 1 ml of the Dinitro phenyl 2, 4-DNP reagent. Keep it in hot water bath hydrazone is formed. for few minutes. 2. Schiffs test: No purple colour is To 1 ml of the compound add 5 ml of the developed schiffs reagent and heat the mixture on a water bath for 2 minutes. 3. Tollens test: No silver mirror is To 1 ml of the compound add 5 ml of the deposited or no grey tollens reagent and heat the mixture on a colour water bath for 5 minutes. 4. Fehlings test: No red colour ppt is To 1 ml of the compound add 1 ml of formed.

INFERENCE Carbohydrate may be present Carbohydrate may be present Carbohydrate is conformed.

INFERENCE Carbonyl compound is present Aldehyde group is absent Aldehyde group is absent. Aldehyde group is absent.

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Engineering Chemistry Lab Manual Na2CO3 solution and 1 ml of the Fehlings solution A and 1 ml of Fehling solution B. Boil the mixture for 2-3 minutes. 5. Bisulphate test: To 1 ml of the compound add 1 ml of saturated Sodium bisulphate solution.

(I B.Tech Common to All)

White NaHSO3 product is formed.

Ketone is present.

Experiment-10

PREPARATION OF ACETYL SALICYLIC ACID (ASPIRIN)

Aim : Preparation of Acetyl Salicylic Acid (Aspirin) with using salicylic acid. Apparatus: 250 ml Round bottom Flask, 200 ml beaker, Glass rod, Funnel, Dropper, Filter papers, Simple balance with weights

Chemicals Required: Salicylic acid, Acetic Anhydride Acetic acid Conc. Sulphuric Acid (H2SO4) & Distilled-water. Chemical Reaction:

Procedure: 5 gms Salicylic acid and 10 ml Acetic anhydride taken in 200 ml Round Bottom Flask, mix well, and add 1 or 2 ml Concentrated sulphuric acid . Heat it 50-600C on water bath for 15 minutes. Cool and add 100 ml water and filter the precipitate. Recrystallize it with equal volume of alcohol and water. Result: Yield =

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Engineering Chemistry Lab Manual Melting Point =

(I B.Tech Common to All)

Experiment-11

DETERMINE THE RATE CONSTANT OF HYDROLYSIS OF METHYL ACETATE

Aim: To determine the order of reaction and rate constant for the acid catalyzed hydrolysis of methyl acetate. chemicals: Methyl acetate, 0.5N HCL, 0.1NSodiumhydroxide, phenolphthalein indicator, ice. Apparatus: Iodination flask 250ml, Burette, pippete10ml, 250 ml conical flask. Principle: Hydrolysis of methyl acetate is catalysed by HCl. The rate of reaction is followed by titrating the acetic acid formation during hydrolysis by sodium hydroxide at certain intervals of time. Procedure: Fill the burette with 0.1N sodium hydroxide solution and fix to the stand. Take 90ml of 1NHCl into an iodination flask and add 10ml of methyl acetate. Mix thoroughly for 5 to 10 seconds and note time. Immediately pipette out 10ml of the reaction mixture into a clean conical flask containing ice and phenolphthalein indicator. Titrate it against 0.1N sodium hydroxide. Note the volume of sodium hydroxide required for titration as Vo pour the contents out, clean the conical flask and keep it ready for next titration by adding cold water and indicator. After 10 mins of time pipette out another 10ml of the reaction mixture into the conical flask and titrate against sodium hydroxide as before. Note the volume as V10. repeat the titrations at every 10mins of intervals upto 60 mins as V20,V30,V40 ,V50 and V60.heat the reaction mixture on a water bath at 600c for 30 minutes cool and pipette out 10ml of reaction mixture into a conical flask, add phenolphthalein indicator and titrate with sodium hydroxide and note the volume as V Result: the hydrolysis of acetic acid is a pseudo first order reaction the experimental value of K =

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Engineering Chemistry Lab Manual

(I B.Tech Common to All)

S.NO TIME Vol of NaOH Intial 1 2 3 4 5 6 7 Final

V -Vt

Log V -V0 ____V -Vt

K1 = 2.303/t Log V -V0 _______________V -Vt

From the value of the reaction rate constant at two temperatures calcilate the energy of activation for the reaction using the equation: Log K2 = -E [ 1/T2 1/T1] K1 2.303R

E = T1 T2 X 4.567 X Log T2 - T1

K2 K1

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Engineering Chemistry Lab Manual Result: The rate constant of the reaction (k) = ________. The energy of activation (E) =_____________

(I B.Tech Common to All)

Experiment-12

ADSORPTION OF CHARCOAL
AIM: To determine the Adsorption of aqueous acetic acid by Activated Charcoal and to study adsorption isotherm. APPARATUS: Stopper bottles, 20 ML Pipette, Burette, Beakers

CHEMICALS: Powdered activated charcoal, 0.5N Glacial acetic acid and 0.1 N NaOH. PRINCIPLE: Freundlich adsorption isotherm is given by the expression: x = KC 1/n - equation-1 m Where X and m are the amounts of solute (adsorbate) and adsorbent respectively, C is the equilibrium concentration of adsorbate. K is a constant depends on both, the nature of adsorbent as well as of adsorbate. n is another constant and depends only on the nature of adsorbate. Taking log, the equation (1) can be written as log x = log k + 1 log C m n When log X is plotted against log C, it gives a straight line whose slope is 1 and the m n __________________________________________________________________________________ SV Group of Institutions 32

Engineering Chemistry Lab Manual Intercept log k.

(I B.Tech Common to All)

PROCEDURE: Proceed stepwise as follow: 1. Take 50, 40, 30, 20 and 10 ml of 0.5 N acetic acid in stopped bottles and to these add 0, 10, 20, 30 and 40 ml of distilled water respectively and label them. 2. Transfer 1 gm of activated charcoal to each bottle then shake these vigorously for about one hour and allow them to stand for half an hour to attain the room temperature. 3. Filter off charcoal and while filtering discard initial nearly four ml filtrate in each case. 4. Take 5 ml of each filtrate and titrate it against standard solution of 0.1 N NaOH using phenolphthalein as an indicator. 5. Note the reading in each case. OBSERVATIONS: 1 .room temperature =. . . . . . C 2. Amount of charcoal used in bottle = 1g 3. Volume of solution taken for titration each time = 5 ml Bottle No 1 2 3 4 5 Volume of 0.5 N CH3COOH (ml) 50 40 30 20 10 Volume of water added 0 10 20 30 40 Initial normality of the acid (normality) C2 0.50 0.40 0.30 0.20 0.10 Volume of NaOH used, V

Calculate the normality of the acid after adsorption using N1V1 = N2V2. Subtract this value from initial normality of the acid. This will give you the normality of the acid adsorbed. Let it be N. The amount of the acid adsorbed, x = N X 60 gm 1000 m = 1g in all cases Repeat the calculation of remaining solutions and produce your results in tabular form as below: Bottle number Initial normality acid Normality of acid adsorbed Amount of acid adsorbed x x/m log x / m log C

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Engineering Chemistry Lab Manual 1 0.50 2 0.40 3 0.30 4 0.20 5 0.10

(I B.Tech Common to All)

Plot the graph between x/m and log C. The slope is equivalent to 1 / n and the intercept to log k.

RESULT: The trend of the graph is in accordance with Freundlich adsorption isotherm. The values of 1 and k are respectively. and. n PRECAUTIONS: 1. Shake all the solutions properly and uniformly 2. Filter the solution before proceeding for titration and discard the initial small volume of the filtrate. 3. Do not use wet filter paper in filtration as it may dilute the solution.

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