CHIO6BS/CH206BS Exclusively for JNTU (Hyderabad) ENGINEERING CHEMISTRY LABORATORY Chemistry Lab Manual For | Year B.Tech Students As per the JNTU (Hyderabad) Syllabus New Edition 2018-2019 Regulation|- 2018 ab Manual (Observation Note Book Short Procedures Viva - Voce Q&A preparation of Various Reagents} Dr. A. Ravikrishnan Dr. J. Kranthi Kumar Sri Krishna Dr. V. Aparna Hitech Publishing Company Pvt. Ltdpencanarcermene Engineering Chemistry Laboratory Chemistry Lab Manual For | Year B.Tech. Students) As per the JNTU (Hyderabad) Syllabus New Edition - 2018-2018 Regulation - 2018 Dr. A. RAVIKRISHNAN M\Sc., MPhil., M.Ed., Ph.D., MISTE., MILCS HOD / Chemistry ‘Adhiparasakthi Engg. College, Formerly, Melmaruvathur Dr. J. KRANTHI KUMAR, M.Sc., Ph.D., HOD / Chemistry Khammam Institute of Technology & Science Khammam Dr. V. APARNA, M.Sc., Ph.D., Department of Chemistry Nalla Malla Reddy Engineering College Hyderabad Lab Manual Observation Note Book Short Procedures Viva - Voce Q&A Preparation of Various Reagents Sri Krishna op hE, Hitech Publishing Company Pvt.Ltd.CH106BS/CH206BS: Engineering Chemistry Lab (Common to ECE/EIE/ME/IT) Determination of total hardness of water by complexometric method using EDTA. Determination of chloride content of water by Argentometry Estimation of an HCI by Conductometric titrations. Estimation of Acetic acid by Conductomettic titrations Estimation of HCI by Potentiometric titrations. Estimation of Fe?* by Potentiometry using KMnOy Determination of rate constant of acid catalysed hydrolysis of methyl acetate Synthesis of Aspirin and Paracetamol Thin layer chromatography. Calculation of Ry values. eg ortho and para nitro phenols. Determination of acid value of coconut oil Verification of freundlich adsorption isotherm-adsorption of acetic acid on charcoal. Determination of viscosity of castor oil and groundnut oil by using Ostwald’s viscometer. Determination of partition coefficient of acetic acid between n-butanol and water. Determination of surface tension of a given liquid using stalagmometer.vi CONTENTS Determination of total hardness of water by complexometric method using EDTA. 2. [Determination of chloride content of water by Argentometry 6 3. [Estimation of an HCl by Conductometric titrations. 10 4. [Estimation of Acetic acid by Conductometric titrations 4 5. [Estimation of HCI by Potentiometric titrations. 18 © |Bstimation of Fe?* by Potentiometry using KMn0,,24 7. |Determination of rate constant of acid catalysed hydrolysis of methyl acetate | 30 8. [Synthesis of Aspirin and Paracetamol (a) Synthesis of Aspirin 34 (b) Synthesis of Paracetamol 38 9. Thin layer chromatography. Calculation of Ry values. eg ortho and para nitro} 40 phenols. 10. [Determination of acid value of coconut oil 44 LL. | Verification of freundlich adsorption isotherm-adsorption of acetic acid on charcoal.| 46 12, [Determination of viscosity of castor oil and groundnut oil by using Ostwald’s| 50 viscometer. 13. |Determination of partition coefficient of acetic acid between n-butanol and water.| 56 14, |Determination of surface tension of a given liquid using stalagmometer. 60 Short Procedures 63 Preparation of various reagents 66 Viva-Voce Questions and Answers1 Engineering Chemistry Laboratory Structure of Disodium salt of EDTA (Fig-I) HOOCH,C (CH,COO™ Nat N-CH,-CH)-N Na*t“OOCH,C CH,COOH Step I: STANDARDISATION OF EDTA TITRATION - 1 Standard Hard water Vs. EDTA Calculation Volume of standard hard water V, = 20 ml Strength of standard hard water N; = Volume of EDTA Vo= Strength of EDTA N)= According to the law of volumetric analysis ViN] = V2xNo VyxNy ‘I SFEngineering Chemistry Laboratory 2 1, DETERMINATION OF TOTAL HARDNESS OF WATER SAMPLE (EDTA Method) Expt. No. Date: AIM To determine the total hardness, permanent hardness, temporary hardness in the given sample of hard water by EDTA method. A standard hardwater of .. .N and a EDTA solution are provided. PRINCIPLE Disodium salt of Ethylene Diamine Tetra Acetic acid (EDTA) is a well known complexing agent. Its structure is shown in the figure I. Disodium salt of EDTA is used to estimate the various hardness of the given hard water containing Ca®* and Mg”* ions. When EDTA is added to hard water, it reacts with calcium and magnesium ions present in hard water to form stable EDTA metal complexes. From the volume of EDTA consumed the hardness can be calculated. Eriochrome Black - T is used as an indicator. The indicator forms a weak complex with the metal ions present in the hard water and gives wine red colour. 2+ pH=9-10 2+ Ca” + EBT —+| "BHT |eumplee Mg** Indicator Hardwater (Weak) (Wine red colour) When EDTA is added into the hard water, the metal ions form a stable metal complex with EDTA by leaving the indicator. When all the metal ions are taken by EDTA from the indicator metal ion complex, the wine red colour changes into steel blue, which denotes the end point. The metal EDTA complex is stable at pH 8-10. This pH range can be maintained by adding ammoniacal buffer (NH4Cl + NH,OH). Catt pH9-10 Catt a] 7 a4 EBT |complex+ EDTA ———>|“*) Epra |complex + EBT Mg’ (Colourtesg Mg’ (Steel Blue Colou (Stable) (Colourless) From the volume of EDTA, total hardness can be calculated.a) Engineering Chemistry Laboratory Step Il: DETERMINATION OF TOTAL HARDNESS OF HARDWATER SAMPLE TITRATION - Il Hardwater Sample Vs. Std. EDTA Calculation of the total hardness of hard water Volume of EDTA Vi=. Strength of EDTA N=. Volume of the hard water sample V2 =20 ml Strength of hard water sample N=. According to the law of volumetric analysis ViNj =V2* Np VixNi nas Total hardness of hard water sampleEngineering Chemistry Laboratory 4 MATERIALS REQUIRED 1. EDTA solution 2, Standard hand water 3, EBT indicator 4, Buffer solution 5. Burette, pipette, conical flask, 250 ml beaker, 100 ml std. flask 6. Sample hard water PROCEDURE TITRATION - I Standardisation of EDTA Step | The burette is washed well with the distilled water and rinsed with a little amount of the given EDTA solution. It is then filled with the same EDTA solution upto the zero level without air bubbles. Initial reading of the burette is noted. 20ml of standard hard water solution is, pipetted out into a clean conical flask. Sml of ammonia buffer solution and 2 drops of Eriochrome Black - T indicator are added. The solution turns wine red in colour and it is then titrated against EDTA taken in the burette. The change of wine red colour to steel blue colour is the end point. The final reading in the burette is noted. The difference in the burette reading gives the volume of the EDTA solution. The titration is repeated to get concordant values. Step I TITRATION - Il Determination of Total Hardness of Hardwater Sample 20 ml of the given hardwater sample is pipetted out into a clean conical flask. 5 ml of ammonia buffer solution and 2 drops of Eriochrome Black - T indicator are added. The solution turns wine red in colour. This solution is titrated against EDTA solution taken in the burette. The change of wine red colour into steel blue colour is the end point. The titration is repeated to get concordant values. RESULT 1, Amount of total hardness of the given sample of water = ppm.5 Engineering Chemistry Laboratory Step I: STANDARDISATION OF SILVER NITRATE TITRATION - | Standard NaCI Vs AgNO; Calculation of the normality of Silver Nitrate Volume of Sodium Chloride V, = 20 ml Strength of Sodium Chloride Ny Volume of Silver Nitrate Vj = Strength of Silver Nitrate Ny =? According to the law of volumetric analysis VAN = VoNo V,xNy nro Strength of Silver Nitrate =Engineering Chemistry Laboratory 6 2. DETERMINATION OF CHLORIDE CONTENT OF WATER SAMPLE BY ARGENTOMETRIC METHOD [Mohr’s Method] Expt. No. Date: AIM To determine the amount of chloride present in 100 ml of the given water sample, being supplied with standard solution of sodium chloride of strength .. N and an approximately N/20 solution of silver nitrate PRINCIPLE Generally water contains chloride ions (CI”) in the form of NaCl, KCl, CaClp and MgCh. The concentration of chloride ions in water, more than 250 ppm, is not desirable for drinking purpose. The total chloride ions can be determined by argentometric method (Mohr’s Method). In this method CI” ion solution is directly titrated against AgNO, using potassium chromate (KyC104) as an indicator. AgNO3+NaCl ——> AgCll +NaNO3 (in water) (white precipitate) At the end point, when all the CI” ions are removed. The yellow colour of chromate changes into reddish brown due to the following reaction. 2 AgNO3+K C10, ———> AgyCrO,l + 2 KNO3 (Yellow) (Reddish brown precipitate) MATERIALS REQUIRED 1. Std. NaCl solution 2. AgNO3 solution 3. 2% KyCrO4 indicator 4. Burette, pipette, conical flask.z Engineering Chemistry Laboratory Step Il: DETERMINATION OF CHLORIDE IONS TITRATION - Il Water sample Vs. Std. AgNO3 : mace 1. 20 0 2. 20 0 K,CrO4 a! 20 0 Calculation of Normality of the water sample (Chloride ions) Volume of the water sample V; = 20 ml Strength of the water sample (Chloride ions), Ny = Volume of silver nitrate, V= ml Strength of silver nitrate, Ny = According to the law of volumetric analysis VN, =V2Ny _VaxNp 1 Vi Strength of the water sample (Chloride ion) = Calculation of amount of the chloride Amount of the chloride ion present in | __{ Equivalent weight of chloride ion 1 litre (1000 ml) of the water sample | ~ | x Strength of the chloride ion = 35.46 x... NI = . gms <. Amount of the chloride ions presen 100 mi of the given water sample 100 1000 = gms - x 1000 mgs = s+ gms XEngineering Chemistry Laboratory 8 PROCEDURE Step | TITRATION - | Standardisation of Silver nitrate The burette is washed well with distilled water and rinsed with the small amount of AgNO; solution. It is then filled with the same solution upto the zero mark without any air bubbles. The pipette is washed with distilled water and rinsed with the small amount of standard NaC! solution. 20ml of this solution is pipetted out into a clean conical flask. Iml of 2% KC1O} indicator solution is added and titrated against AgNOs solution taken in the burette. The end point is the change of colour from yellow to reddish brown. The titration is repeated for concordant values. Step Il TITRATION II Determination of Chloride ions 20 ml of the given water sample is pipetted out into a clean conical flask and Iml of 2% KyC10, indicator solution is added. It is then titrated against standardised AgNOs solution taken in the burette. The end point is the change of colour from yellow to reddish brown. The titration is repeated for concordent values. RESULT whole of the given water sample (i) Amountof chloride ion present in the ... gms/mgs/ppm (ii), Amount of chloride ion present in the } 100 ml of the given water sample ...gms/mgs/ppm9 Engineering Chemistry Laboratory Step | TABLE - | Titration of Standard NaOH Vs HCI Volume of HCI taken = 20 ml Decreases ul 10 End point 12 ir 3 12 14 13 15 14 16 15 IncreasesEngineering Chemistry Laboratory 10 3. CONDUCTOMETRIC TITRATION OF STRONG ACID WITH STRONG BASE (Determination of HCl) Expt. No. Date: AIM To determine the amount of hydrochloric acid present in 250 ml of the given solution by conductometric titration, You are provided with standard sodium hydroxide solution of ..........N PRINCIPLE Solution of electrolytes conducts electricity due to the presence of ions. The specific conductance of a solution is proportional to the concentration of ions in it. The reaction between HCl and NaOH may be represented as, HCl + NaOH ——*> NaCl + H,O When a solution of hydrochloric acid is titrated with NaOH, the fast moving hydrogen ions are progressively replaced by slow moving sodium ions. As a result conductance of the solution decreases. This decrease in conductance will take place until the end point is reached. Further addition of alkali raises the conductance sharply as there is an excess of hydroxide ions. A graph is drawn between volume of NaOH added and the conductance of solution. The exact end point is intersection of the two curves. MATERIALS REQUIRED (i) Conductivity bridge (i) Conductivity cell (iii) 100 ml beaker (iv) Standard HCI (v) Given NaOH solution (vi) Distilled water (vii) Burette, pipette, glass rod etc.,rr Engineering Chemistry Laboratory Graph: Conductance Vs. Volume of NaOH <1 Equivalent point Conductance (1/R) Volume of NaOH (ml) Step Il Calculation of Strength of HCt Volume of NaOH taken V, = . ml (titre value) Strength of NaOH LN Volume of HCI V2 =20 ml Strength of HCl N2=? According to the law of Volumetric analysis VN; = V2N> Strength of HCI = Zalculation of amount of HCI The amount of HCI present | _ in 1000 ml of the given solution } 8 The amount of HCI present in 250 ml of the given solution } ae gmsEngineering Chemistry Laboratory 12 PROCEDURE TITRATION The burette is washed well with distilled water and rinsed with the standard NaOH Solution. It is then filled with same upto the zero level. 20 ml of the given HCl is pipetted out into a clean 100 ml beaker. The conductivity cell is placed in it and then diluted to 50 ml by adding conductivity water, so that the electrodes are well immersed in the solution. The two terminals of the cell are connected with a conductivity bridge. Now 1 ml of NaOH from the burette is added to the solution, taken in the beaker, stirred for some time and then conductivity is measured. The conductivity is going on decreasing upto the end point. After the end point, further addition of NaOH will increase the conductivity. This process is repeated until atleast five readings are taken after the end point has been reached. Now the graph is plotted by taking volume of NaOH in the X-axis and conductance in the Y-axis. The end point is the intersection of the two curves. From the volume of NaOH, the strength and hence the amount of HCI present in 250 ml of the solution is calculated. RESULT (i) The strength of given HCI solution = aN (ii) The amount of HC! present in 250 ml of the. given solution = . . gms13 - Engineering Chemistry Laboratory Step | TABLE - | Titration of CHzCOOH Vs Std.NaOH Volume of CH;COOH taken = 20 ml Slow increase 10 L ir 10 End point @ 12 i 13 12 14 13 15 14 16 15 Sudden increaseEngineering Chemistry Laboratory 14 4. ESTIMATION OF ACETIC ACID BY CONDUCTOMETRIC TITRATIONS Expt. No. Date: AIM To determine the amount of CH;COOH present in 250 ml of the given solution by conductometric titration. You are provided with standard Sodium hydroxide solution of ... Ny PRINCIPLE Solution of electrolytes conducts electricity due to the presence of ions. The specific conductance of a solution is proportional to the concentration of ions in it. The reaction between CH3COOH and NaOH may be represented as, CH3COOH + NaQH ——> CH3COONa + H,0 When a solution of acetic acid is titrated with NaOH, the fast moving hydrogen ions are progressively replaced by slow moving sodium ions. Initially the conductivity of CH;COOH is low, this is due to the poor dissociation of CH;COOH. As NaOH is added gradually, condutance will be going on slowly increasing. This is due to the formation of highly ionised CH;COONa. A graph is drawn between volume of NaOH added and the conductance of solution. The exact end point is intersection of the two curves. MATERIAL REQUIRED () Conductivity bridge (ii) Conductivity cell (iii) 100 ml beaker (iv) Standard NaOH. (v) Given CH3COOH solution (vi) Distilled water (vii) Burette, pipette, glass rod etc.,15 Engineering Chemistry Laboratory Graph: Conductance Vs. Volume of NaOH g a i Equivalent point g Volume of NaOH (ml) ~~ Step il Calculation of Strength of CH3COOH Volume of CH3;COOH taken V; =20ml Strength of CH3COOH N=? Volume of NaOH V2= ml (titre value) Strength of NaOH wN According to the law of Volumetric analysis VjN, = V2N> V2N2 are Strength of CHyCOOH Calculation of amount of CH;COOH The amount of CH;COOH present 0 in 1000 ml of the given solution { = ©? * « ‘The amount of CH;COOH present in 250 ml of the given solution |=60x.Engineering Chemistry Laboratory 16 PROCEDURE TITRATION The burette is washed well with distilled water and rinsed with the standard NOH solution. It is then filled with same upto the zero level. 20 ml, of the given CH,COOH is pipetted out into a clean 100 ml beaker. The conductivity cell is placed in it and then diluted to 50 ml by adding conductivity water, so that the electrodes are well immersed in the solution. The two terminals of the cell are connected with a conductivity bridge. Now 1 ml of NaOH from the burette is added to the solution, taken in the beaker, stirred for some time and then conductivity is measured. The conductivity is going on slowly increasing upto the end point. After the end point on further addition of NaOH will suddenly increased the conductivity. This process is repeated until atleast five readings are taken after the end point has been reached. Now the graph is plotted by taking volume of NaOH in the X-axis and conductance in the Y-axis. The end point is the intersection of the two curves. From the volume of NaOH, the strength and hence the amount of CH3COOH present in 250 ml of the solution is calculated. RESULT (i) The strength of given CH;COOH solution = . N (ii) The amount of CH;COOH present in 250 ml of the given solution = .. gmsre Engineering Chemistry Laboratory FIGURE | Potentiometric Titration Step | x TABLE - | (Titration - |) ‘i HCI Vs NaOH Volume of HCI Solution =20 mlEngineering Chemistry Laboratory 18 5. ESTIMATION OF HCl BY POTENTIOMETRIC TITRATION Expt. No. Date: AIM To estimate the amount of HCI present in 100 ml of the given solution potentiometrically. A standard solution of NaOH of strength N is provided. PRINCIPLE Potentiometric titrations depend on measurement of emf between reference electrode and an indicator electrode. When a solution of H* ions is titrated with a solution of NaOH} the following redox reaction takes place. HCl + NaOH NaCl + H30 A little change is produced at the begining is due to fraction of H* ions removed. At the end point the emf is suddendy decreased and above the equivalent point there is small change in emf. The cell is set up by connecting this pt electrode with a calomel electrode as shown below. Ha (Pt) acid | solution |] KCI (aq) | calomel electode A graph between emf measured against the volume of NaOH added is drawn and the end point is noted from the graph. MATERIALS REQUIRED 1, Potentiometer 2. Pt electrode 3. Saturated Calomel electrode 4. Standard NaOH solution 5. Given HCI solution 6. Burette and pipette 7. Distilled water PROCEDURE The given HCI solution is transfered into 100 ml standard flask and made upto the zero mark using distilled water. 20 ml of this made up solution is pipetted out into a clean 100 ml beaker. 20 ml of distilled water are added in it. A platinum19 Engineering Chemistry Laboratory Graph 1: Volume of NaOH Graph 2: Volume of NaOH Vs emf Vs. AE/AV AE/AV H Volume of NaOH (ml) —» ‘Volume of NaOH (ml) —> TABLE - Il (Titration - Il) HCI Vs NaOH Solution Volume of HCI Solution =20 mlEngineering Chemistry Laboratory 20 electrode is dipped into the solution. This electrode is then coupled with a saturated calomel electrode and the cell is introduced into potentiometric circuit. TITRATION - | The burette is washed well with water and rinsed with the given NaOH solution. It is then filled with the same upto zero mark and titrated against the HCI solution taken in the connical flask. The addition is carried out by adding std. NaOH solution in portions of 1 ml and the emf of the cell is measured after each addition. The addition of NaOH is continued even after the end point and the range at which end point lies is found out by plotting volume of NaOH added against emf (graph - 1). TITRATION - II Another titration is carried out by adding std. NaOH solution in portions of 0.1 ml near the end point and the emf of the cell is measured after each addition. The addition of NaOH is continued even after the end point for further 1 ml. The accurate end point is determined by plotting AE/AV Vs Volume of NaOH added (graph - 2). From the end point, the strength of HCI solution and hence its amount is calculated. RESULT The amount of HCI present } in 100 ml of the given solution is gms.21 Engineering Chemistry Laboratory Step - I Calculation of strength of HCI solution Volume of HCI solution, V; = 20 ml Strength of HCI solution, Ny =........? Volume of NaOH, V> Strength of NaOH, Np =. N According to the law of volumetric analysis V,Ny = V2N> V2 XN- Ny cee Ni= ~. Strength of HCI solution N; = Calculation of amount of HCI ‘The amount of HCI present in 1000 ml of the solution } nxt’ g/l :. ‘The amount of HCI present 100 in 100 ml of the given ae Mx 26AS pS em gms23 Engineering Chemistry Laboratory FIGURE | Potentiometric Titration Burette «—| KMn0,+— Ferrous solution <—+ TABLE - | (Titration - 1) KMnO, Vs Iron Solution Volume of Ferrous Iron (Fe”*) Solution = 20 mlEngineering Chemistry Laboratory 24 6. ESTIMATION OF Fe?* CONTENT OF THE GIVEN SOLUTION USING POTENTIOMETER Expt. No. Date: AIM To estimate the amount of Iron (ferrous iron (Fe?*)) present in 100 ml of the given solution using potentiometer. A standard solution of Potassium permanganate of strength N is provided. PRINCIPLE Potentiometric titrations depend on measurement of emf between reference electrode and an indicator electrode. When a solution of ferrous iron is titrated with a solution of potassium permanganate, the following redox reaction takes place. 2KMnO, + 3H,SO, => _ K,SO4 + 2MnSOQ, + 3H30 + [0] 2904 F=—= B2804 2 2FeSO4 + HpS04+[0] <=> Fe2(SO4)3 + H,0. = During this titration Fe? * is converted into Fe? *, whose concentration increases At the end point, there will be a sharp change due to sudden removal of all Fe2* ions. The cell is set up by connecting this redox electrode with a calomel electrode as shown below. Hg /Hg,Cly.,, KCI// Fe?* , Fe? * /Pt A graph between emf measured against the volume of KCr)07 added is drawn and the end point is noted from the graph. MATERIALS REQUIRED 1. Potentiometer 2. Pt electrode 3. Saturated Calomel electrode 4. Standard KMnO, solution 5. Given ferrous iron solution 6. Burette and pipette 7. Dil. H)SO, 8. Distilled water25 Engineering Chemistry Laboratory Graph 1: emf Vs Volume of KMn04 Graph 2: AE / AV Vs Volume of KMnO4 AE/AV Volume of KMn0, (ml) —» Volume of KMnO, (ml) —> TABLE - II (Titration - Il) KMnO, Vs (Fe**) Solution Volume of Ferrous Iron Solution =20 mlEngineering Chemistry Laboratory 26 PROCEDURE The given iron (ferrous iron) solution is transfered into 100 ml standard flask and made upto the zero mark using distilled water. 20 ml of this made up solution is pipetted out into a clean 100 ml beaker. About 10 ml of dil HySOq and 20 ml of distilled water are added in it. A platinum electrode is dipped into the solution. This electrode is then coupled with a saturated calomel electrode and the cell is introduced into potentiometric circuit. TITRATION - I The burette is washed well with water and rinsed with the given KMnO, solution. It is then filled with the same upto zero mark and titrated against the ferrous iron solution taken in the connical flask. The addition is carried out by adding std. KMnOg solution in portions of 1 ml and the emf of the cell is measured after each addition. The addition of KMnOg is continued even after the end point and the range at which end point lies is found out by plotting volume of KMnOy added against emf (graph - 1). TITRATION - Il Another titration is carried out by adding std. KMnO, solution in portions of 0.1 ml near the end point and the emf of the cell is measured after each addition. The addition of KMnO, is continued even after the end point for further 1 ml. The accurate end point is determined by plotting AE/AV Vs Volume of KMnO, added (graph - 2). From the end point, the strength of ferrous iron solution and hence its amount is calculated, RESULT . gms, The amount of ferrous iron present in 100 ml of the given solution is27 Calculation of strength of ferrous iron solution Engineering Chemistry Laboratoy Volume of ferrous iron solution, V; = 20 ml Strength of ferrous iron solution, Ny = Volume of KMnO,, V7 = Strength of KMnOg, N3 = N According to the law of volumetric analysis VN = V>N> _V2XNo ‘ 120 : Ni= +. Strength of ferrous iron solution Ny = Calculation of amount of ferrous iron a N x 55.85 The amount of iron (ferrous iron) present in 1000 ml of the solution 1 V/I The amount of iron (ferrous iron) present |- Nx 55.85 x 200. in 100 ml of the given solution rin ams .- gms.29 Engineering Chemistry Laboratry _Engineering Chemistry Laboratory 30 7. DETERMINATION OF RATE CONSTANT OF ACID CATALYSED HYDROLYSIS OF METHYL ACETATE Expt. No. Date: AIM To determine the rate constant of the acid catalysed hydrolysis of methyl acetate. PRINCIPLE The hydrolysis of methyl acetate in water’ occurs according to the following equation. H CHjCOOCH; + Hy0 ——> CH;COOH + CH;0H As the large amount of water is used in the reaction, it is called a pseudo unimolecular reaction, The rate equation is ~ Spake where , C= concentration of methyl acetate at time t t= time k= rate constant The progress of the reaction can be followed by withdrawing known amount of samples and titrating with alkali at various time intervals and at the end of reaction. The rate constant can be calculated by using the following formula. 2.303, Veo Vo = log t Veo Vt K Where, V..= Titre value at infinite time V, = Titre value at time t. Rate constant can also be calculated graphically by plotting log (V..— V,) Vs time31 Engineering Chemistry Laboratry log (V,,- V)) —> 0) 400 900 1400 1900 2400 2800 34003900 4400 . Time (sec) —» Figure: log (Vq—V,) Vs TimeEngineering Chemistry Laboratory 32 MATERIALS REQUIRED 1, Burette 2. Pipette 3. 250 ml conical flask 4. Phenolphthalein indicator 5. 0.5 N HCI 6. Methyl acetate ester 7. Stop watch 8. 0.2 N NaOH PROCEDURE TITRATION 95 ml of 0.5 N HCl is taken in a clean dry 250 ml conical flask and 5 ml of ester (methyl acetate) is pipetted out into the conical flask. 5 ml of the acid-ester mixture is immediately withdrawn into another dry conical flask. The reaction is then arrested by the additien of ice cubes into the conical flask. The stop watch is started when the pipette is half emptied and the time is recorded. The mixture is titrated against 0.2 N NaOH using phenolphthalein as an indicator. The end point is the appearance of permanent pale pink colour. Let, the volume of NaOH consumed = Vo. 5 ml of the same acid-ester mixture is similarly withdrawn after 10, 20, 30, 40, 50, 60 minutes respectively and titrated against the same NaOH using phenolphthalein as an indicator. Let, the volume of NaOH consumed for each time intervals (t) = V;. The remaining reaction mixture is heated in a water bath for about 15 minutes, Then the solution: is cooled and 5 ml of the sample is pipetted out into the conical flask as before and titrated against NaOH. The volume of NaOH consumed = V.. RESULT The Rate constant for the hydrolysis of an ester 1. Calculated value = 2. Graphical value =Preparation of Aspirin “OH o-d-cy oO or , ‘OH Soar C-oH Salicylic acid fe anhydride Acetylslicytic acid (CH,0,) (C4603) (CoH) Engineering Chemistry Laboratory 2 1 * CH,-c-oH Acetic acid (CH,0,)Engineering Chemistry Laboratory 34 8. SYNTHESIS OF ASPIRIN AND PARACETAMOL (a) Synthesis of Aspirin Expt. No. Date: AIM To prepare aspirin by acetylation of salicylic acid APPARATUS Beaker, Conical flask, watch glass, stirring rod, Buchner funnel, filter paper. CHEMICALS Salicylic acid, acetic anhydride, glacial acetic acid, sulphuric acid, ice and distilled - water, PRINCIPLE Aspirin is acetylsalicylic acid, It is a synthetic organic derivative derived from salicylic acid by acetylation in acidic medium, Salicylic acid is a natural product found in the bark of the willow tree and was used by the ancient Greeks and Native Americans, among others, to counter fever and pain. It was first synthesized in 1987 by a German chemist named Felix Hoffman. PROCEDURE 2.0 g (0.015 mole) of salicylic acid is taken in a 125-ml Erlenmeyer flask. 5 ml (0.05 mole) of acetic anhydride, followed by 5 drops of conc. HySOQq is added and swirled the flask gently until the salicylic acid gets dissolved. The flask is heated gently on the steam bath for at least 10 minutes and is allowed to cool to room temperature. The wall of the flask is scratched with a glass rod. If acetylsalicylic acid does not begin to crystallize out, scratch the walls of the flask with a glass rod. The mixture is cooled slightly in an ice bath until crystallization is completed. The product is appeared as a solid mass when crystallization is completed.35. Engineering Chemistry Laboratory Calculation of Amount of Aspirin Formed Weight of weighing bottle = + Weight of weighing bottle Dried product Weight of AspirinEngineering Chemistry Laboratory 36 50 ml of water is added and cooled the mixture in an ice bath. Water is added after the crystal formation was complete. The solution is filtered through a Buchner funnel to remove any insoluble impurities (or) polymers that may have been formed. The beaker and the funnel is washed with 5 to 10 ml of water, The crude product, thus formed, is recrystalised with 1:1 ratio of acetic acid and alcohol. The product is completely dried and weighed. Its melting point (lit mp 135—136°C) and the percentage yield were calculated. RESULT The percentage yield of Aspirin is37 Engineering Chemistry Laboratory Preparation of Paracetamol oO ool HO ° Ho-~C)-n, + we—b-o-t-cn, —— 0 -~(O)-N-C-cn, + H,c- C-0n 4-aminophenol cethanoic anhydride paracetamol ethanoic acid (acetic anhydride) (acetic acid) Calculation of Amount of Paracetamol | Weight of weighing bottle =........ soe QMS “ Dried product gms. Weight of weighing bottle | gms. Weight of ParacetamolEngineering Chemistry Laboratory 38 8. (b) Synthesis of Paracetamol Expt. No. Date: AIM To synthesize analgesic and antipyretic drug paracetamol. APPARATUS Round bottomed flask, measuring jar, glass rod, spatula, funnel, filter paper, water bath, watch glass; CHEMICALS ‘ 4-amino phenol, acetic anhydride, distilled water. PRINCIPLE Paracetamol, also known as acetaminophenol (or) APAP, is a medicine used to treat pain and fever. Paracetamol is made by reacting 4-aminophenol with acetic anhydride, This reaction forms an amide bond and acetic acid as a byproduct. When the reaction is complete the Paracetamol is then isolated and purified. PROCEDURE About I.1 g of p-amino phenol is taken in a round bottomed flask and 30 ml of distilled water and 12 ml of acetic anhydride were added. The reaction mixture is vigorously stirred with a glass rod and heated (warm) on water bath till the solid disappeared. After 10 min the reaction mixture is cooled and filtered the solid material to separate acetyl derivative. The crude product is dried and recrystallized from hot water. The pure product is dried and the melting point (literature 169°C) and percentage yield is calculated. RESULT The yield of pure Paracetamol is Melting point is39 Engineering Chemistry Laboratory aa=a==e |<— Solvent Front + solvent front --- Center of spot Ga §x ii |+— Starting point of spot Calculation of the Ry value: i 1 ——— The distance is measured from the starting point to the center of the spot on the: TLC plate (distance a). The distance is measured from the starting point to the solvent front (distance b) The retention Factor is calculated as:Engineering Chemistry Laboratory 40 9. THIN-LAYER CHROMATOGRAPHY, CALCULATION OF Ry VALUES Expt. No. Date: AIM To determine the Ry values of ortho and para nitro phenols using Thin-Layer Chromatography. APARATUS TLC-Plates, TLC-Chamber CHEMICALS Ortho and para nitro phenols. PRINCIPLE Thin layer chromatography (TLC) is a useful technique for the separation and identification of compounds in mixtures. Thin layer chromatography (TLC) uses the same principles as extraction to accomplish the separation and purification of compounds: that is, the separation of different compounds between two phases based on differences in solubility of compounds in the two phases. In the case of TLC, one phase is a mobile liquid solvent. phase and the other phase is a stationary solid phase with a high surface area. The stationary phase normally consists of a finely divided adsorbent, silica (SiO>) (or) alumina (Al,O3) powder, used in the form of a thin layer (about 0.25 mm thick) on a supporting material. The support is usually a sheet of glass (or) metal foil. The mobile phase consists of a volatile organic solvent (or) mixture of solvents. TLC is used routinely to follow the progress of reactions by monitoring the consumption of starting materials and the appearance of products. Commercial applications of TLC include the analysis of urine for evidence of “doping”, the analysis of drugs to establish purity (or) identity of the components and analysis of foods to determine the presence of contaminants such as pesticides.at Engineering Chemistry Laboratory Retention factors are numbers between zero and one, representing the position of the spot on the TLC plate. The Ry (rate of flow) value is usually constant under fixed conditions such as TLC plate, developing solvent, and temperature. Therefore, each. compound can be identified based on the Ry value along with the shape and color of its spot. The Ry value is usually recorded to the second decimal place. PROCEDURE Thin-layer chromatography is carried out with a glass plate coated with silica gel. When one of the edges of the plate is dipped in a developing solvent, the sample moves along with the solvent. The mobility of samples depends on their properties This method is utilized for checking the purity of a product and the progress of a reaction. ‘ PREPARATION A small amount of a sample is taken with a micro spatula and dissolved in a small amount of an appropriate solvent. The starting line is drawn lightly with a pencil at about 10 mm above from a shorter edge of a silica gel plate. Cross marks are drawn on the line as chromatography starting points. The sample solution is taken with a capillary and spotted lightly on one of the starting points and dried the spot with a dryer if necessary. This operation is repeated a few times to concentrate the sample in the small spot, which should be less than 2 mm in diameter. A new capillary is used when a different sample is taken. DEVELOPMENT The developing solvent is poured into a wide-mouth bottle to about 5 mm in height. The bottle is closed with the cap and waited a little while until the bottle is saturated with the solvent vapour. The cap is opened and hold the upper end of the TLC plate with tweezers. The TLC plate is placed in the bottle so that the bottom of the plate is dipped in the solvent and the top of the plate is leaned against the wall of the bottle. The solvent should be drawn straight upright. The development is finished when the solvent front reaches at about 10 mm below the upper end of the TLC plateEngineering Chemistry Laboratory 42 The TLC plate is taken out and the front line of the developing solvent is immediately marked with a pencil. Waited for some time until the solvent gets evaporated (or) dried the TLC plate with a dryer. A UV lamp is tumed on and the spots where detected with UV ray and the out lines are traced with a pencil. The shape and colour of the spots were recorded and Ry value is calculated at a Rat a= The distance from the starting point to the gravity center of the sample spot. b= The distance from the starting point to the. front of the developing solvent. RESULTS: 1. Ry value of Ortho nitro phenol 2. Ry value of para nitro phenol43 Engineering Chemistry Laboraton Calculation Titration I; Standardization of Potassium Hydroxide Solution: S.No. |. Volume of Burette Reading Concordant Volume Oxalic acid (ml) |" Tnitial Final of KOH (ml) 1. 20 0 2. 20 0 3. 20 0 Calculation Volume of oxalic acid (V;) = 20 ml Normality of oxalic acid (Ny) = Volume of KOH consumed (V;) Normality of KOH consumed (N)) According to the volumetric law Vy Ny = V2 Ny Normality of KOH (WN ) Titration I: Estimation of acid value SNo,| Volume of Burette Reading Concordant Volume “N° | alcohol + oil (gm) |" Tnitial_| Final of KOH (ml) 1 | Sem+50ml 2. | Sem +50 mi 5 gm + 50 ml Calculation Acid value = {Volume of KOH x Normality of KOH x Eq. wt of Lauric acid x 1000) Weight of Oil sample _ Nx 200 x 1000 Acid Value = Note: In coconut oil, free fatty acid is present as Lauric acid, the equivalent weight of lauric acid = 200.Engineering Chemistry Laboratory 44 10. DETERMINATION OF ACID VALUE OF COCONUT OIL Expt. No. Date: AIM To determine the acid value present in given Coconut oil. CHEMICALS Oxalic acid, KOH Solution, Alcohol, Coconut oil, Phenolphthalein indicator and distilled water. APPARATUS Burette, pipette, conical flask, wash bottle, dropper. PRINCIPLE . Acid value indicates the proportion of free fatty acid present in an oil (or) fat and may be defined as “the number of milligrams of caustic potash required to neutralize the acid in 1 gm of the sample.” The normal acid value for most samples lies within 0.5. If any titrable acid other than a fatty acid is present in the sample, it will be an error. A high acid value indicates a stale oil (or) fat stored under improper conditions. PROCEDURE TITRATION - Standardization of KOH 20 mi of 0.1 N oxalic acid solution is pipetted out in a 250 ml conical flask. 1 (or) 2 drops of phenolphthalein indicator is added to this solution. This solution is titrated against KOH taken in a burette. The appearance of pink color is the end point. From the volume of the KOH solution in burette, the normality of KOH is found out. TITRATION - Il: Determination of Acid Value in Coconut oil 5 gm of coconut oil is weighed and transferred it into 250 ml conical flask. 50 ml of neutralized alcohol solution is added to the oil solution. This mixture is heated for 10 minutes by using the heater. After 10 minutes this solution is taken out and 1 (or) 2 drops of phenolphthalein indicator is added. It is then titrated against the KOH solution from the burette. The appearance of pink color is the end point. RESULT The acid value of the given Coconut oil sample was found to be =45. OBSERVATIONS AND CALCULATIONS The observations are tabulated and a graph is plotted. Engineering Chemistry Laboratory NaOH solution Initial. | Equilibrium | Amount Flask’ peauired lconcentration|concentration | adsorbed | x Be lisc No. | for 10 ml) of Acetic | of Acetic EG) | in| 989. | 8 Ce Canes. acid (C;) | acid (C,) ag adsorption. log— 5 |«—>Engineering Chemistry Laboratory 46 11. VERIFICATION OF FREUNDLICH ADSORPTION ISOTHERM-ADSORPTION OF ACETIC ACID ON CHARCOAL Expt. No. Date:] | AIM To verify Freundlich Adsorption Isotherm for adsorption of acetic acid on a given sample of charcoal. APPARATUS Stoppered reagent bottles, buretie, pipette, conicalflask, beakers, funnels, glazed paper (filter paper). CHEMICALS Acetic Acid (0.5M), NaOH (0.1M), Distilled water, phenolphthalein indicator. PRINCIPLE The property of accumulating other substances on the surface of porous solid is called adsorption. At a given temperature, tlc variation in the amount of solute adsorbed with change in concentration of the solution is given by an empirical relation suggested by Freundlich known as Freundlich adsorption isotherm. This is Zac m Where, C stands for the equilibrium concentration of the solute in solution. Taking logarithms of the terms in the Freundlich isotherm we get, log = log K++ 10g. C If we plot a graph between log i Vs log C, a straight line would get. The slope of the line will be equal to 4 and log K can be obtained as the intercept which the straight line makes on the ordinate for a value of log C equal to zero.Engineering Chemistry Laboratory 43 PROCEDURE About 2 gms of finely powdered charcoal is accurately weighed in each of the thoroughly cleaned and dried bottles numbered as 1 to 6. 0.5 M acetic acid solution is prepared for 250 ml by means of a burette and 10, 20, 30, 40, 50 ml of acetic acid solutions and 40, 30, 20, 10 and 0 mi distilled water are added in the bottles 1, 2, 3, 4 and 5 respectively. The unknown solution is taken in the bottle no. 6, The bottles are vigorously shaken and left them at a desired temperature for about half an hour. 0.1 M NaOH solution is prepared for 250 ml and standardised with standard oxalic acid solution using phenolphthalein indicator and the concentration of acid solution is determined. The solution of each bottle is filtered by means of filter paper. The filtrates are collected properly in separate conical flasks numbered with 1, 2, 3, 4 and 5. While filtering about 5 ml of initial filtrate is rejected in each case. 10 ml from each filtrate is pipetted out and titrated against standard NaOH solution. The equilibrium concentration of acid in each bottle is calculated. RESULT:49 Engineering Chemistry Laboratory Ostwald’s viscometer Lower mark Capillary Table - I: Measurement of flow time (to) of distilled water S.No Time of flow of distilled water Mean flow time (éq) sec of distilled waterEngineering Chemistry Laboratory 50 12. DETERMINATION OF VISCOSITY OF CASTOR OIL AND GROUNDNUT OIL BY USING OSTWALD’S VISCOMETER Expt. No. Date: AIM To determine the viscosity of castor oil and groundnut oil by using ostwald viscometer. THEORY Viscosity is one of the most important properties of any lubricating oil. This indicates us about the suitability of the oil for lubricating purpose. A lubricant must reduce friction between sliding parts of any machine. This avoids the direct metal to metal contact. The main criteria of a lubricant are that it should be sufficiently viscous under high temperature and pressure exerted by the machine to adhere to the surface. If the viscosity is low then a thin film of lubricant cannot adhere to the sliding surfaces. In case the viscosity is high there will be excessive friction. The absolute viscosity of fluid oil can be determined by measuring the rate of flow of the oil through a capillary tube kept at a uniform temperature. But in case of lubricating oil specific viscosity is generally determined by measuring the time taken for a given quantity of oil to flow through an orifice (or) jet of standard dimension under standard conditions. Measurement of viscosity of lubricating oil is made with the help of an apparatus called Ostwald’s viscometer. Ostwald’s viscometer is commonly used for determining viscosities of thin lubricating oils. Important Viscosity definitions 1, Relative viscosity (n,) 2. Specific viscosity (nyp) 3. Reduced viscosity (Med) ny eae 4, Intrinsic viscosity (n;) y= lim ApEngineering Chemistry Laboratory Step Ill: Determination of flow time of groundnut oil The viscometer is thoroughly washed and dried. Now the same volume of groundnut oil is introduced into the viscometer and sucked upto the level Ay and the time of flow of groundnut oil from mark A, to Ap is measured. The same is repeated for 3 to 4 times and the mean value is taken. RESULT SLNo. Types of viscosities Castor Oil Ground Oil 1. Relative viscosity (n,) 2. Specific viscosity (Msp) Reduced yiscosity (ec)55 Engineering Chemistry Laboratory OBSERVATIONS AND CALCULATIONS. Pipette Burette Reading (ml) | Volume of i NaOH Cy Layers Taken | Readi reas " (ml) Initial Final ae Leta Aqueous Layer Organic Layer Aqueous Layer (C}): Vol. of aqueous layer x C, = Vol.of NaOH required (V) x strength of NaOH (S) 10 mlx Cy =VxS. (VxS) CTO Organic Layer (C2): Vol. of organic layer x C2 = Vol.of NaOH required (V) x strength of NaOH (S) 10 mlx C)=VxSEngineering Chemistry Laboratory 56 13. DETERMINATION OF PARTITION CO-EFFICIENT OF ACETIC ACID BETWEEN N-BUTANOL AND WATER. Expt. No. | Date: AIM To determine the partition co-efficient of Acetic acid between n-butanol and water. CHEMICAL n-butanol, acetic acid, distilled water, NaOH solution. APPARATUS ‘ Burette, pipette, 100 ml conical flask, 250 ml Stoppered bottle, Wash bottle, Dropper. PRINCIPLE Nernst distribution law states that at constant temperature, when a solute is allowed to distribute between two immiscible solvents in contact with each other, then at equilibrium the ratio of concentration of the solute in two solvent layers is constant. When a solute is shaken in two immiscible liquids, then the solute is found to be distributed between the liquids in a definite manner, if the solute is soluble in each of the solvent. According to distribution law, the distribution co-efficient at a particular temperature is given by Ky=— dacs where, Cy and C3 represent concentration of acetic acid in water and concentration of acetic acid in butyl alcohol respectively, when the solute molecules in each solution phase are in same state of association.Engineering Chemistry Laboratory 58 PROCEDURE A 250 ml stoppered bottle is taken and washed properly with distilled water. This bottle is filled up with 40 ml of n-butanol, 50 mi distilled water and 10 ml of acetic acid. Then it is allowed to shake in a mechanical shaker for about an hour. After shaking, it is kept aside for about 5 minutes so that two layers are separated out clearly. 10 ml of aqueous layer is pipetted out in a 250 mi conical flask. 2-3 drops of phenolphthalein indicator is added and titrated against standard NaOH solution until colour changes from colorless to pink. Similarly 10 ml of organic layer is pipetted out in a 250 ml conical flask. 2-3 drops of phenolphthalein indicator is added and titrated against standard NaOH solution until colour changes from colorless to pink. The experiments are repeated to get concordant values. ” RESULT: Partition Coefficient of Acetic acid between water and n-butanol is Precautions: 1. Stoppered bottle should be thoroughly cleaned and dried. 2. During withdrawing of liquid for titration, one layer must not be contaminated with other layer.59 Engineering Chemistry Laboratoy Figure: Stalagmometer Capillary tube | ll Surface tension AX), acts along the \—~} circumference we Weight of drop Observation and Calculations Number of drops of unknown S.No. | Number of drops of water (n;) liquid (v2) Surface tension of water at 25°C =72 dynes/cm ¥, = surface tension of water (reference liquid) Y= surface tension of unknown liquid. Viva = npdy/nydyEngineering Chemistry Laboratory 60 14. DETERMINATION OF SURFACE TENSION OF A GIVEN LIQUID USING STALAGMOMETER Expt. No. Date: AIM To determirie the surface tension of a given liquid using stalagmometer. APPARATUS Stalagmometer, stand, beakers CHEMICALS Distilled water, test liquid. PRINCIPLE Surface tension is defined as the force in dynes acting on a surface at right angles to any line of unit length (or) per centimeter. Surface tension of a liquid is measured using an apparatus called stalagmometer. The method is based on the principle that the weight of a liquid falling from a capillary tube held vertical is approximately proportional to the surface tension of the liquid. It is more convenient to count the number of drops of the liquid. The weight of equal volumes of two liquids are proportional to their densities. If nj and ny are the same volumes of two liquids then VW/¥2 = M2 dy / ny dy If the surface tension of the one liquid is known then that of the other can be easily calculated from the equation. Generally liquid 2 is a reference which is water, whose data can be obtained from literature. DESCRIPTION OF APPARATUS The apparatus “Stalagmometer”, used to determine the surface tension, is a pipette with a capillary at the lower end, a bulb in the middle. The upper end is provided with one screw pinch cock. It is provided with two marks A and B, A is in the upper end and B is in the lower end. These marks A & B define the volume of a lubricant to be delivered for counting the drops. The rate of flow can be adjusted using screw pinch cock.Engineering Chemistry Laboratory ez PROCEDURE A clean and dried stalagmometer is taken. The stalagmometer is filled with distilled water by sucking it while immersing the lower end into the distilled water. The level of the water is brought to mark A. The pinch cock is opened and adjusted it, so that the rate of flow of liquid is about 12-15 drops per minute and the number of drops formed is counted till the level of the liquid reached the mark B. The time interval is noted in the given table. The experiment is repeated to get two concordant values. The procedure is repeated for unknown liquid to determine the surface tension. PRECAUTIONS 1. The tip of the lower end should not come in contact with hand (or) anything else as it will be contaminated with traces’ of grease, which will alter the size of the drop. 2. 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Hard water. 1 litre 0.01 M_ {1.0 gm of CaCO; + (mol. weight of min. con HCl + 1 CaCO = 100) litre distilled water. 3. |Sample Hard water. 1 litre 0.5 gm of NaHCO; (or) Ca(HCOs) + 1 litre distilled water (or) Tap water. 4. |Buffer solution. 1 litre 70 gms NH,Cl (NH,CI + NH4OH) crystal + 568 ml con NH make up to I litre using distilled water. 5. | Indicator. 100 ml 1 gm of EBT + 100 Eriochrome Black-T ml methanol (or) ethanol.Engineering Chemistry Laboratory ‘Expt. No. 2) Determination of chloride content of water by Argentometry 1. |Std. NaCl. 1 litre 0.01. N [0.584 gms of AR. (mol. wt = 58.44) NaCl + 1 litre dis. water. 2. |Std. AgNO. 1 litre 0.01 N_— [1.698 gms of (mol. wt = 169.87) AgNO + | litre dis, water. 3. |Water sample. 1 litre 0.05 N [2.92 gms of AR NaCl + 1 litre dis. water. 4. |Indicator. 100 ml 2% 2 gms of K,CrO4 KyCrO4 + 100 ml dis. water. Estimation of an HCI by Conductometric titrations. 1. |Std HCL 1 litre O1N 8.9 ml of con (con. HCl = 11.3 N) HCI in 991 ml dis. water. 2. |Std NaOH. 1 litre 01N 4.0 gms of A.R. (mol.wt = 40) NaOH + | litre dis. water. Estimation of Acetic acid by Conductometric titrations 6 ml of con CH3COOH in 994 ml dis. water. CH;COOH (con. CHyCOOH = 17 N) Std NaOH. 1 litre 0.1.N 4.0 gms of A.R. (mol.wt = 40) NaOH + 1 litre dis. water. nvEngineering Chemistry Laboratory 1. |Std NaOH. Estimation of HCI by Potentiometric titrations. 40 gms of 1 litre 0.1.N (Eq.wt = 40) NaOH + 1 litre dis. water. el Estimation of Fe’* by Potentiometry using KMnO, 1. |Std KMnO,. 1 litre O.1N [3.16 gms of (Eq.wt = 31.6) KMnO, + 1 litre dis. water. 2. |Std FAS 1 litre O1N [39.2 gms of (FeSO4 (NH4)2 SO, - 6H20. FAS + 15-20 (Eq.wt = 392) ml HySO, in 1 (or) litre dis. water. Ferrous iron solution 3. [Std. HySO4. 250 ml 25N [17.36 ml of con, HySO4 + 232.6 ml dis. water. Determination of rate constant of acid catalysed hydrolysis of methyl acetate 1. |Std HCI 1 litre 42.5 ml of con.HC! in (con HCI = 11.3 N) 57.5 ml of dis water Std. NaOH Llitre 0.2.N 8.0 gms of A.R. NaOH (mol.wt = 40) + 1 litre dis water Phenolphthalein indicator |100 ml |1% 1 gm of phenolphthalein + 100 ml ethanol.Engineering Chemistry Laboratory vv VIVA - VOCE QUESTIONS & ANSWERS. Determination of Total hardness of water by complexometric method _u: EDTA 1. Define hardness of water. Hardness is the property or characteristics of water, which does not produce lather with soap. 2. Define hard water and soft water. 1, Hard water Water, which does not produce lather with soap solution but produces white precipitate (scum) is called hard water. This is due to the presence of dissolved Ca and Mg. salts. 2€\7H3sCOONa + Catt ——+ (C}7H3sCOO)2 Ca + 2Na* [ hardness ] ‘Sodium soap calcium soap [fener tat | causing | [eter note] ion | 2. Soft water Water, which produces lather readily with soap solution is called soft water. This is due to the absence of Ca and Mg salts. 3. What are the salts responsible for carbonate and non-carbonate hardness of water. Carbonate hardness: Ca(HCO3)> and Mg (HCO3)2 Non-Carbonate hardness: CaCl), CaSO4, MgClp, MgSOy. 4. How is hardness of water expressed. The concentration of hardness producing salts are usually expressed interms of an equivalent amount of CaCO. Significance: Its molecular weight is whole number and it is the most insoluble salt. If the concentration of hardness producing salt is X mgs/lit, then to CaCO3 molecular weight of Amount equivalent } X x molecular weight of CaCO3 hardness producing substanceVv.2 Engineering Chemistry Laboratory 5. How is temporary hardness removed? Give example. It can be removed by (i) boiling the water (ii) adding lime to the water. The above two processes convert the bicarbonates into insoluble carbonates and hydroxides, which can be removed by filtering. Ca(HCO3). eo +H30 + CO. Mg(HCO3)2 + 2Ca(OH); —>Mg(OH)>1 + 2CaCO31 + 2,0. (lime) 6, What are the units of hardness. 1. Parts per million (ppm) 2. Milligrams per litre (mgs/lit) 3. Clarke's degree (Cl) * 4, French degree (°Fr) 7. Draw the structure of EDTA. HOOCH,C. ZROT Nat N-CH)-CH,-N : ne 2 ‘OOCH,C ‘CH,COOH 8. How will you calculate temporary hardness. Temporary hardness of the water sample is calculated by subtracting permanent hardness from total hardness. Temporary hardness = Total hardness - Permanent hardness. 9. What is the colour change when EBT is added to hard water. Write its equation. The indicator forms a weak complex with the metal ions present in the hard water and gives wine red colour. 2+ pH=9~-10 24 ca (+ EBT. ———>| @ 34 EBT |complex Mg** | Indicator Mg? Hard water (Weak) (Wine red colour)Engineering Chemistry Laboratory VvV3 10. What is a buffer solution. Buffer solution is a solution which resists the change in PH by the addition of acid or base i.e., Buffer solution maintains the constant P4 of a solution. 11. What buffer is used in EDTA titration. Why? EDTA make complex with Ca‘t & Mg** ions only at P™ 8 - 10, This range can be maintained by adding ammonia buffer (NH4Cl +NH4OH). 12. Hardness is expressed in terms of CaCO equivalent - comment. The concentration of hardness producing salts are usually expressed interms of an equivalent amount of CaCO3. CaCO3 is chosen as a standard because, (i) Its molecular weight (100) and equivalent weight (50) is a whole number, so the calculations in water analysis can be simplified. (ii) It is the most insoluble salt, that can be precipitated in water treatment. 13. What is the colour change, when EDTA is added to hard water + EBT. Write its equation. When EDTA is added into the hard water, the metal ions form a stable metal complex with EDTA by leaving the indicator. When all the metal ions are taken by EDTA from the indicator metal ion complex, the wine red colour changes into steel blue. ct PHO-10 7 G24 “EBT |complex+ EDTA ——-> | ‘*) EDTA |complex + EBT Mg (Colourless) Mg’ (Steel Blue Colour) (Stable) (Coloutless) Determination of Chloride Content in Water by Argentometric Method 1. What is the form of chloride ions present in water. Chloride ions present as salt in water. Example = NaCl, KCI, CaCl, & MgCl 2, What is the name of the method used in this titration. Mohr’s method 3. Write the reaction between AgNO; and chloride ions present in water. AgNO; + Cl ——>AgCl 1 + NO3 white precipitateVV.4 Engineering Chemistry Laboratory 4. What is the equivalent weight of chloride ion. 35.46. 5. What is the indicator used in the titration. Potassium chromate. 6. What is the colour change in the titration. Colour change form yellow to reddish brown. 7. Write the reaction between AgNO and K,CrOy. 2AgNO3 + KxCrO, ——>Ag,CrO, + 2KNO3, yellow (Reddish brown) 8. What is the standard solution used in the standardisation of AgNO3. Standard NaCl solution. 9. How to calculate the amount of chloride present in 100 ml of the solution from the normality of chloride ion solution. a I . -,. 100 = 35.46 x Normality of CI” ion xo [ 3._Estimation of an HCI by Conductometric Titrations 1, What is meant by strong acid give example. If 100% ionisation occurs in acid, it is strong acid e.g., HCl, HySO,, HNO3 2. Give some examples for strong base. NaOH, KOH, Ca (OH) 3. What is the basic principle of conductometric titration. Solution of electrolytes conducts electricity due to the presence of ions. The specific conductance of a solution is proportional to the concentration of ions in it. 4. What is conductance, mention its unit. The conductance of an electrolyte is the reciprocal of its resistance Unit of conductance: 1 ol Sam = ohm’ (or) mho.Engineering Chemistry Laboratory VV5 5. What is specific conductance, mention its unit. The reciprocal of specific resistance is called specific conductance. (or) It is the conductance of lcm? of a material. ies where p=C Unit of Specific Conductance cm k=———,; ohm x cm’ 1 =——— = ohm! cm (or) mho-em™ ohm xem, 1 6. What is equivalent conductance, mention its unit. It is defined as the conducting power of all the ions produced by dissolving 1 gram equivalent of an electrolyte in the solution. _ 1000 x Neq C where, C=concentration of the solution in gm equivalent weight. Unit of equivalent conductance cm? 1 gm. equivalent x mhocm™ =mho cm? gm - equ! 7. What is molar conductance, mention its unit. It is defined as “the conducting power of all the ions produced by dissolving 1 mole of an electrolyte in a given solution.”Vv6 Engineering Chemistry Laboratory where, C= molar concentration Unit of molar concentration 2 3 om - NaCl + H,0 10. What is the equivalent weights of HCl and NaOH. HCI = 36.45 NaOH = 40 11. Why is conductance decreased during the titration When a solution of hydrochloric acid is titrated with NaOH, the fast moving hydrogen ions are progressively replaced by slow moving sodium ions. As a result conductance of the solution decreases.Engineering Chemistry Laboratory VT 12. Why is conductance increased after the end point. Further addition of alkali raises the conductance sharply as there is an excess of hydroxide ions. 13. How will you calculate the amount of HCI from the solution. Amount of HCI present in 1000 ml of the given solution = 36.45 x Normality 4. Estimation of Acetic Acid by Conductometric Titrations 1. What is meant by strong acid give example. If 100% ionisation occurs in acid, it is strong acid e.g., HCl, HySO4, HNO; 2. Give an examples for week base. NH4OH 3. What is the basic principle of conductometric titration. Solution of electrolytes conducts electricity due to the presence of ions. The specific conductance of a solution is proportional to the concentration of ions in it 4, What is conductance, mention its unit. The conductance of an electrolyte is the reciprocal of its resistance 1 Cc Unit of conductance: ~ ohm G = ohm! (or) mho. 5. What is specific conductance, mention its unit. The reciprocal of specific resistance is called specific conductance. (or) It is the conductance of 1 cm? of a material. x Lf or K=vv8 Engineering Chemistry Laboratory where 2=C Unit of Specific Conductance cm i ohm x cm? =——— = ohm! cm (or) mho-em™ ohm xem 6. What is equivalent conductance, mention its unit. It is defined as the conducting power of all the ions produced by dissolving 1 gram equivalent of an electrolyte in the solution. _ 1000 x Neq Cc where, C= concentration of the solution in gm equivalent weight. Unit of equivalent conductance 1 =mho cm? gm- equ 7. What is molar conductance, mention its unit. It is defined as “the conducting power of all the ions produced by dissolving 1 mole of an electrolyte in a given solution.” 1000K An=—e where, C= molar concentration Unit of molar concentration 1 2. mho - cm? - mole~! 3 em: . Am = 22 x mho « cm mole 8. What is cell constant, mention its unit. It'is the ratio of distance between two electrodes (/) and area of the electrodes (a).Engineering Chemistry Laboratory vg x= als where, /= length in cm; a= area in cm? This cell constant is multiplied with observed conductance (c) or (2) to get specific conductance (Ke) cedxl “Roa Unit of cell constant ee om! cm? 9. Write the reaction between CH;COOH and NaOH. ; CH3COOH + NaOH ——>CH3COONa + H,0 10. What is the equivalent weights of CH;COOH and NaOH. CH,COOH = 40 NaOH = 40 11. Why is conductance increased after the end point. Further addition of alkali raises the conductance sharply as there is formation strong CH3COONa. 12. How will you calculate the amount of CH;COOH from the solution. Amount of CH3COOH present in 1000 ml of the given solution =40x Normality of CH;COOH. 5. Estimation of HCI by Potentiometric Titration ] 1. What is emf. Electromotive force is defined as, "the difference of potential which causes flow of current from one electrode of higher potential to the other electrode of lower potential. Standard reduction Standard reduction EMF =| potential of right hand }~! potential of left side electrode hand side electrode E°ce = Eright — EtenV.v.10 - Engineering Chemistry Laboratory 2. What is the standard solution used in this titration. NaOH 3. What is the name of the instrument used here. Potentiometer 4. What is the basic principle of potentiometric titration. Emf of a cell depends on the concentration of the electrolytes with which the electrodes are in contact. Therefore, the ‘electrode reaction is, M"* +ne™ ———->. As the concentration of M"* changes, the emf of the cell also changes correspondingly, 5. Why does emf increase during the titration. When it is titrated against the standard NaOH) solution, taken in the burette, the emf is going.on decreasing as the concentration of H* decreases due to the following reaction. HCI + NaOH -_——> HO + NaCl 6. What is the name of the indicator electrode used in this titration, Platinum electrode 7. What is the name of the reference electrode used here, write its representation. Calomel electrode; Hg/Hg2Cl, KCI 8. Write the cell representation of the titration. The cell is set up by connecting this redox electrode with a calomel electrode as shown below P\(Hy) / acid // KCleq / calomel electrode 9. What is redox reaction. Redox reaction is a chemical reactions, where oxidation occurs in one half and reduction occurs in another part. 10. Write the nernst equation of a cell. + B=E°— 0.0591 log Zn**} [cu]Engineering Chemistry Laboratory Matt 11. What are the advantages of potentiometric titrations. 1. The necessary apparatus required is cheap and easily available. 2. This method can be used for coloured solution. 3. Fixing up end point is easier when compared to the titrations in which indicators are used to fix up end points. 4. Very dilute solutions can be titrated with accuracy. 5. Several components may be titrated in the same solution. 12. How will you obtain the end point in the titration. The accurate end point is determined by plotting AE/AV Vs Volume of KMnO, added. 13. What is the equivalent weight of HCl. 36.45 14, How will you calculate the amount of HCl. Amount of HCl = 36.45 x N gms/lit 6. Estimation of Iron content (Fe?*) by Potentiometric Titration 1, What is emf. Electromotive force is defined as, "the difference of potential which causes flow of current from one electrode of higher potential to the other electrode of lower potential. Standard reduction Standard reduction | EMF =} potential of right hand || potential of left side electrode hand side electrode | E°cett = Fright ~ E°ten. 2. What is the standard solution used in this titration. KMnOq 3. What is the name of the instrument used here. Potentiometer 4, What is the basic principle of potentiometric titration. Emf of a cell depends on the concentration of the electrolytes with which the electrodes are in contact. Therefore, the electrode reaction is, M"* +ne7 ———>M.v.v.t2 Engineering Chemistry Laboratory As the concentration of M"* changes, the emf of the cell also changes correspondingly. 5. Why does emf increase during the titration. When it is titrated against the standard KMnOg solution, taken in the burette, the emf is going on increasing as the concentration of Fe** increases due to the following reaction, KMnO, Fett 5 Fe 4 0 6. What is the name of the indicator electrode used in this titration, Platinum electrode 7, What is the name of the reference electrode used. here, write its representation. . Calomel electrode; Hg/Hg Cl, KCI 8. Write the cell representation of the titration. The cell is set up by connecting this redox electrode with a calomel electrode as shown below Hg / Hg,Cly,,, KCI// Fe?*, Fe? * / Pt 9. What is redox reaction. Redox reaction is a chemical reactions, where oxidation occurs in one half and reduction occurs in another part. 10. Write the nernst equation of a cell. + E=E°- 2.0591 log 22°11 [cu**] 11. What are the advantages of potentiometric titrations, 1. The necessary apparatus required is cheap and easily available. 2. This method can be used for coloured solution. 3. Fixing up end point is easier when compared to the titrations in which indicators are used to fix up end points. 4, Very dilute solutions can be titrated with accuracy. 5. Several components may be titrated in the same solution.Engineering Chemistry Laboratory vv.13 12. How will you obtain the end point in the titration. The accurate end’ point is determined by plotting AE/AV Vs Volume of KMn0Oy added. 13, What is the equivalent weight of Fe?* ion. 55.85 14, How will you calculate the amount of Fe”* ions. Amount of Fe?* = 55.85 x N gms/lit 7. Determination of Rate constant of acid catalysed hydrolysis of methyl acetate 1, What is rate of reaction It is the measure of the change in concentration of the reactants per unit time. 2. What is first order reaction If the rate of reaction depends on a single reactant it is first order reaction. 3. What is Pseudo first order reaction If the concentration of a reactant is constant it is Pseudo first order reaction. 4, Give the rate equation of the Pseudo first order reaction ah kC 5. Give example and reaction of Pseudo first order reaction. Hydrolysis of methyl acetate in water using an acid # CH,COOCH; + H,O ——> CH,COOH + CH,0H 6. How is rate constant calculated 2.303 1 Veo — Vo == lo} K pi) 1 8 VA, 7. What is the indicator used in ester hydrolysis Phenolphthaleinvv.t4 Engineering Chemistry Laboratory [ 8. Synthesis of Aspirin and Paracetamol 1. What is aspirin Aspirin is a acetylsalicylic acid. 2. What is the main source of aspirin. It is available is the bark of the willow tree. 3. Write the structure of aspirin. ° 1 o-o7 or c-on 1 ° 4. What is the chemical name of paracetamol. cH, Acetaminophenol. 5. Write the structure of paracetamol. u? vo-_-N-c- cH, 6. What type of disease can be cured by paracetamol? Pain and Fever. 7. What is the melting point of paracetamol. 169°C 8. What is the raw materials used for the preparation of aspirin Salicylic acid and Acetic anhydride. 9. Thin Layer Chromatography. Calculation of R; values of Ortho and Para Nitro Phenols 1. What is chromatography It is a technique used for the separation of mixtures. 2. What are the types of chromatography (a) Adsorption chromatography (b) Partition chromatographyEngineering Chemistry Laboratory VivV.A5 3. What is partition chromatography If the mixture is separated by means of partition between a moving phase and stationary phase it is called partition chromatography. 4. Give some examples for stationary phase Finely divided silica and alumina. 5. Give some examples for mobile phase Volatile organic solvents like, benzene, acetone. 6. What is Rr Ry is a retention factor. It is the ratio of distance travelled by the solute and the solvent. 7. How is spot identified. By placing the TLC plate in the iodine chamber (or) exposing it in UV light. - 8. What is eluent Eluent is a type of solvent used to separate a compound from the stationary phase. 10. Deter ation of Acid value of Coconut Oil 1. Define acid value. It is the number of milligrams of KOH required to neutralize the acid present in 1 gm of oil. 2. What is recommended acid value of an oil. Less than 0.5 3. What is the significance of acid value. Suitability of an oil can be found because when acid value of an oil increases with time due to hydrolysis with moisture. 4. Why KOH is used for the titration. Because it is primary standard. 5. How will you prepare N/100 alcoholic KOH solution. 5-6 gms of KOH is dissolved in 1 litre of ethyl alcohol 6. What is the colour change in the titration. Appearance of pink colour.V.V.16 Engineering Chemistry Laboratory 7. What is the main acid present in coconut oil. Laurie Acid. 8. Write the structure of Laurie Acid. C\)H);COOH 11. Verification of Freundlich Adsorption Isotherm-adsorption of Acetic acid on Charcoal 1. Define Adsorption and Adsorbate. (i) Adsorption: The phenomenon of concentration of molecules of a gas or liquid at a solid surface is called adsorption. The adsorption of gas on a solid is sometimes called occlusion (ii) Adsorbate: The substance which is held on the surface of the solid is called adsorbate. : 2. What is sorption? Sorption is the process in which both adsorption and absorption takes place simultaneously. 3. What is chemisorption? Give an example. Chemical adsorption is the one, in which the adsorbed molecules are held on the surface of the adsorbent by chemical bonds (Covalent bond (or) ionic bond). Example: Adsorption of Hy on Ni. 4. What is physical adsorption (or) physisorption. Give an example. Physical adsorption is the one, in which the adsorbed molecules are held on the surface of the adsorbent by weak physical (or) Vander Waal’s forces of attraction. Example: Adsorption of Hp (or) O> on charcoal. 5.. Mention some important characteristics of adsorption. 1. Adsorption on surface of a solid is always spontaneous. 2. Adsorption is always accompanied by‘ evolution of heat. 3. Adsorption is accompanied both by decrease in enthalpy and entropy of the system. 4, Adsorption is a selective process. 6. Explain the function of activated charcoal with example. (i) It adsorbs coloring matter present in sugar solutions.Engineering Chemistry Laboratory VVA7 (ii) It also adsorbs certain acids like CHyCOOH and (COOH), present in water, thereby acid concentration in water decreases. (iii) It also adsorbs out NH3 from the solution of NH4OH and phenolphthalein. 7. What is Freundlich’s adsorption isotherm? The relationship between the magnitude of adsorption (x/m) and pressure (P) can be expressed mathematically by an equation known as Freundlich adsorption isotherm x ==xp™" m 8. Explain the limitations of Freundlich’s adsorption isotherm. 1. 2. Freundlich equation is purely empirical and has no theoretical basis. The equation is valid only upto a certain pressure and invalid at higher pressure. s The constants K and ‘n’ are not temperature independents, they vary with temperature. Freundlich’s adsorption isotherm fails, when the concentration of adsorbate is very high. 9. What is Langmuir adsorption isotherm? How it is mathematically represented? The relation between the amount of gas adsorbed to the pressure of the gas at constant temperature is known as Langmuir Adsorption isotherm. It is represented mathematically as KP. x=K/— 1+KP 12. Determination of Viscosity of castor oil and groundnut oil by the using Ostwald’s visometer 1 How is intermolecular forces related to viscosities? When the liquid molecules have strong intermolecular forces, they have greater viscosities than those liquids having weaker intermolecular forces. 2 What is viscosity. It is the internal resistance to flow. What is the relationship of temperature and viscosity. Viscosity e Temperature.VV.18 Engineering Chemistry Laboratory 4. What are polymers and monomers? Polymers: These are large molecules of higher molecular weight. Monomers: These are small molecules of lower molecular weight. 5. Write the polymerisation reaction of ethylene. nCHy=CHy ——> -¢CHp ~ CHy Jy 6. What is the name of viscometer used in this experiment. Ostwald’s viscometer 7. What is Oligomers. Polymers with low degree of polymerization are oligomers their molecular weight ranges from 500 - 5000. 8. Write the relationships between different viscosities. (i) Relative viscosity (n,) (ii) “Specific viscosity (nyp) (iii) Reduced viscosity (Myeq) (iv) Intrinsic viscosity (nj) Determination of partition coefficient of acetic acid between ‘butanol and water 1. Define partition Coefficient It is ratio of concentrations of a compound in a mixture of two immiscible phases at equilibrium. 2. Mention an important use of measuring partition coefficient. To estimate the distribution of drugs within the body. 3. What is hydrophobic liquid It is water-hate liquid i.e., Insoluble in water. 4. What is hydrophilic liquid It is water-loving liquid i.e., soluble in water.Engineering Chemistry Laboratory vv.19 5. What is molecular formula of n-butanol (CH3-CH)~CH)~CH)-OH. 6. What does n-butanol water partition coefficient mean? n-butanol/water partition coefficient is the ratio of a chemical concentration in the n-butanol phase to its concentration in the aqueous phase of a two-phase n-butanol/water system. 7. What is the formula for calculating distribution co-efficient. GQ KG 14. Determination of surface tension of a given liquid using stalagmometer 1. Define surface tension Surface tension is defined as the force in dynes acting on a surface at right angles to any line of unit length (or) per centimeter. 2, How does surface tension occurs? It is due to the uneven intermolecular forces of the molecules in the surface. 3. What are the factors affecting the surface tension. (i) Nature of the liquid (ii) Surrounding environment (iii) temperature. 4. In what way intermolecular forces affect the surface tension. Liquids having larger attractive intermolecular forces will have a larger surface tension. 5. In a liquid where will be surface tension more. On surface, surface tension will be more. 6. How is weight of an oil is related to densities. Weight <-density. 7. What is the name of the apparatus used to determine the surface tension. Stalagmometer. 8. What is the formula used to find out surface tension. V/¥2= 12d) / my dy