DEPARTMENT OF CHEMISTRY RGIT N71 RAJIV GANDHI Al LZ 4MSTITUTE OF TECHNOLOGY DEPARTMENT OF CHEMISTRY 1/11 SEMESTER ENGINEERING CHEMISTRY LAB (24CHEL 46, /26) LABORATORY MANUAL STUDENT NAME: USN NUMBER: BRANCH BATCH SECTION 1 R ENGINEERING CHEMISTRY LAB (I8CHEL 16/26) PAGE| 1/11 SEMESTE)DEPARTMENT OF CHEMISTRY RGIT ‘Model Procedure for Practical Examination CONTENTS Initial of ‘Name of the experiment Page No. | Marks | 1" PART-A| Potentiometric estimation of FAS using standard | 4 potassium dichromate solution Colorimetric determination of copper. 6 Conductometric estimation of an acid mixture using |g standard NaOH solution. Flame photometric estimation of Sodium and fa : otassium in the given sample of water Determination of pKa value of a weak acid using pH | 5 meter, Determination of viscosity coefficient of a liquid 7 using Ostwald’s viscometer. PART-B Determination of Total Hardness of the given 7 water sample using disodium salt of EDTA Determination of Amount of Calcium oxide in the 18 given cement solution by rapid EDTA method Determination of percentage of Copper in Brass % using standard sodium thiosulphate solution. Determination of Iron in the given sample of Hematite ore solution using potassium Dichromate 2 crystals by external Indicator method Determination of chemical oxygen demand (COD) as of the given industrial waste water sample. ‘Determination of percentage of available chlorine a in the given sample of bleaching powder. VIVA-VOCE 28 41 ENGINEERING CHEMISTRY LAB (18CHEL 16726) PAGE2 1/11 SEMESTER.DEPARTMENT OF CHEMISTRY RAL INSTRUCTIONS TO BE FOLLOWED WHILE CARRYING OUT VOLUMETRIC ANALYSIS. GENE! The working table must be kept clean. 2. Keep all your glass apparatus scrupulously clean. 3. Keep all the reagents in their proper places after the use do not contaminate the reagents. 4. Do not throw the concentrated acids in to the sink, if poured put large amount of water. 5, Do not throw any waste paper in to the sink, 6. Wash all the glass apparatus with tap water and then rinse with distilled water. ‘ 7. Rinse the burette and pipette with small quantity of the solution and then discard the solution. 8. Do not rinse the conical flask with the solution. 9. During burette reading, see that the level of burette solution is at your eye level to avoid the parallax. 10. During transferring of solutions from the pipette in to the conical flask, touch the tip of the pipette to the bottom of the flask gently. Do not blow the last drop from the pipette. 11. During titration, the conical flask must be on a white tile. 12, During titration, the conical flask must be constantly rotated in one hand and in another hand control the burette. ENGINEERING CHEMISTRY LAB (I8CHEL 16/26) PAGE 3 1/11 SEMESTERRoIr DEPARTMENT OF CHEMISTRY EXPERIMENT NO:1 Date: POTENTIOMETRIC TITRATION = To determine the amount of Ferrous Ion present in the given solution using Theory: ‘This is based on the theory of Oxidation-Reduction reactions. The reactions carrieg Out potentiometrically using Platinum—Calomel electrode oes ae pret vee is the ratio of the concentration of the oxidized and reduced forms of o or the reaction, Oxidized form +n electrons +——* reduced Form. one ‘The potential E° is acquired by the indicator electrode at 25°C is given by E=E® +0,0591 /n log [oxd] / [Red]. ‘ Where E° is the standard electrode potential of the redox system. The Potential of the immersed electrode is thus controlled by the ratio of the concentration of the oxidized to that of reduced species present. As the reaction proceeds, the ratio and hence the potential changes more rapidly in the vicinity of the end point of the titration. This may be followed Potentiometrically and a plot of change in potential against volume (from the titration curve) is characterized by a sudden change in the potential at the equivalence point. Apparatus: Potentiometer, 100-ml beaker, micro burette and test tube. Procedure: Transfer 25 cm’ of ferrous Ammonium sulphate solution into a 100ml beaker, Add two test tubes of dilute sulfuric acid. Immerse platinum-calomel electrode into the Solution in the beaker aid connect to a potentiometer. Measure the potential, Fill the burette with potassium dichromate solution. Add 0.Scm’ of the potassium dichromate to the beaker. Stir the solution carefully and measure the potential after 15 sec. Continue the procedure till there is sudden jump in the potential. After the jump note down four more readings. Determine the end point by differential method i.e. by plotting AE / AV against volume of ferrous ammonium sulfate solution and determine the amount of ron in the given solution Equivalence point — Volume of K.Cr0, Result: The amount of FAS present in the given solution ENGINEERING CHEMISTRY LAB (SCHEL len6) PAGE 4 1/11 SEMESTERDEPARTMENT OF CHEMISTRY RGIT Observ: Volume of | E K:Cr,0;_| (mv) AE av AE/AV Nommality of KxCr:0; =0.5 From the graph volume of K,CrO> at equivalence point = X ml. ew Normality of FAS =. (NxV) Keno. = _0.5xX =......(0). 5 3 ‘Vias. 25 Weight of FAS /dm? =N x Equivalent weight of FAS . X392 = Og “ There fore, Weight of FAS / 25 cm>=¢/ 40 ENGINEERING CHEMISTRY LAB (I8CHEL 16/26) PAGES 1/11 SEMESTERRGIr DEPARTMENT OF CHEMISTRY EXPERIMENT NO: Date: . COLORIMETRIC ESTIMATION OF COPPER . : ion using colorimete Aim: — To determine the amount of Cu present in the given solution using col 7 5 tem with th . ek ariation of colour of a syste 7 Theory: Colorimetric analysis is based on ae Se ie aaicastetaenrapilisnaae change in concentration. The colour is usually due e ‘ medium, a portion of the incident light When a monochromatic light falls on a homogeneous nein eer is reflected, a portion is absorbed and the remainder is tr - * For air-glass interfaces use of glass cells about.4% of a incident ray is Teflected and usually Ir is eliminated by the use of control i.e. comparison cel h=Iyth - The transmission ‘T” is defined as the ratio of the intensity of the transmitted to that of the incident light. T=I,/Ip ‘ : The absorbency ‘A’ or optical density ‘D’ is equal to the logarithm of the reciprocal of transmission. Log WT = log I, /1, . , Beer-Lambert’s law is defined as “The radiation absorbed is directly Proportional to the concentration of the solution and the path length”. A=log I, /I = €C1 Where ¢ is known as the molar extinction coefficient, A= absorbency, C = Concentration and ‘I’ is optical path length. A plot of absorbency against volume Bives a Straight line passing through the origin, when € is a constant. For a given substance at a given path length i. A x C. Copper is treated with ammonia to get blue cuprammonium complex, the absorbency of this solution is measured at 620 nm. At this wavelength complex shows maximum absorbency. « Apparatus: Photoelectric colorimeter, 50ml standard flask, micro burette, and test tubes. Procedure: Estimation of amount of Copper. ‘Transfer the given stock solution of copper sulphate into a burette and draw out 2,4,6,8 & 10cm’ of solution into different SOml standard flask. Add 5 ml of ammonia to each flask and dilute up to the mark with ion exchange water. Shake well To the test solution taken Result: The amount of copper present in the given solution = ENGINEERING CHEMISTRY LAB (SCHEL 1620 PAGES 1/11 SEMESTER~ DEPARTMENT OF CHEMISTRY RGIT Observations and calculations. Volume of CuSO« 2 Absorbency 0203 4 00> e Tp 8 0-09 ee pate Test solution OTe (X cm’ = Vol. from graph). 0-07 1000 ml of stock solution contains 4 g of CuSOs Im! of stock solution contains 4/ 1000g i.e. 4mg of CuSOs X ml of stock solution contains = X x 4 mg of CuSOx 249,68 g of CuSO4 contains 63.54 g of Cu ions 249.68 mg of CuSO; contains 63.54 mg of Cu ions 4mg of CuSOz (Iml of stock solution) contains 4 x 63.54 / 249.68=1.017 mg of Cu ions Therefore, X ml of CuSO contains = Xx 1.017mg_ = Zmg of Cu Optical density Vol. of test solution(X ml) Vol. Of CuSO, RING CHEMISTRY LAB (I8CHEL 16/26) PAGE7 1/11 SEMESTERq RGIT DEPARTMENT OF CHEMISTRY EXPERIMENT NO: 3 Date: CONDUCTOMETRIC ESTIMATION OF ACID MIXTURE USING STANDARD NaOH SOLUTION Principle: Conductometric measurements can be used to ascertain:the end point in acid base litration. The conductivity of a solution depends upon the number of ions and 7 mobility of the ions. When an acid is titrated against a base, the conductance of the resultant solution varies for every addition. Consider the system of HCl and NaOH solution, both ie strong electrolytes and are completely dissociated in the solution, The conductivity in the beginning is due to the H’ ions, which have greatest mobility. NaOH +HCI——+ NaCl +H;0. As NaOH, is added the hydrogen ions are removed. ‘The conductivity also decreases and it is minimum at the equivalence point. Now NaOH is added again the conductance increases. This is due to the OH ions, which have the next higher mobility. A graph of conductance against titre values is plotted. A typical conductometric titration curve is shown in the figure. The point of intersection of the two curves gives the end point. Apparatus: Conductivity Bridge, 100m! beaker and micro burette. Procedure: Conductometric titration. Transfer 50 cm’ of the given acid mixture into a 100 cm’ beaker. Place the conductivity cell inside the beaker so that electrode is completely immersed. Fill a micro burette with sodium hydroxide solution. Connect the cell to the conductivity bridge and ‘measure the Specific conductance of given mixture. Add 0.5 cm* of NaOH from the burette and measure conductance of the solution continue finding Specific conductance of the solution after adding 0.5 cm’ of NaOH every time tll there is arise in the Specific conductance, Take a few more reading. Plot é graph of the Specific conductance against the value of NaoHl added Find the neutralization point from the graph and determine the value of NaOH required to neutralize 50 cm’ of HCl and CH;COOH. Let the Volume of NaOH required to be Vi AND ‘V2em*. x Sp.Conductance Vi a Volume of NaOH —> Result: The amount of HCI present in the given solution i The amount of CH;COOH Present in the given solution is = -. ENGINEERING CHEMISTRY LAB (1SCHEL 160) PAGES 1/11 SEMESTERVol Specific Vol Specific of Conductivity in of Conductivity in NaOH ohm cm’! NaQH. ohm’! cm‘! ‘Normality of standard NaOH = 1.0 (Nx V)) of NaOH Nuci= ‘Vaici (50m) x 36.5 Nx(V2-Vi) of NaOH N(CH;COOH) = Vici,coon (50ml) x 60 ENGINEERING CHEMISTRY LAB (I8CHEL 16/26) --g of CH;COOH The amount of HCI = Normality X Equivalent weight of HCl g of HCl. The amount of CH;COOH = = Newscoon X Equivalent weight of CHyCOOH PAGE9 1/11 SEMESTERDEPARTMENT OF CHEMISTRY EXPERIMENT NO: Date: FLAME PHOTOMETRIC ESTIMATION OF SODIUM AND POTASSIUM IN THE GIVEN SAMPLE OF WATER : Principle: Flame photometry is an atomic emission technique used for detection of metals. Ifa solution containing metallic salts is aspirated into a flame, a vapour, which contains metallic atoms, will be formed. The electrons from the metallic atoms are then excited from ground state (E;) to higher energy state (E,) where n=2,3,4... 7, by making use of thermal energy of flame. From higher energy states these electrons will return to the ground state by emitting radiations (E,-E,=hy where n=2,3,4...7), which are the characteristic of each element, Nae Excitation energy? hy (emission) Nacl (s) -> Nacl (g) | ———+Na(g) + Cl (a) Flame photometer correlates the emitted radiations with the concentration of these elements. It is simple and rapid method for the elements that can be easily excited (sodium and other alkali metals) A flame photo meter is consists of the pressure regulator and flow meter for fuel gases an automiser, burner, optical system, photosensitive detector and out put recorder. A filter of the element whose concentration is to be determined, is inserted between the flame and the detector. Propane gas is used as fuel and air or oxygen is used as oxidant. Combination of these two will give a temperature of 1900°C. The whole analysis depends on the flow rate of the fuel, oxidant, the rate of introduction of the sample and droplet size. The sample containing the analyte is aspirated into the flame through automiser. Radiation from resulting flame is collected by the lens and allowed to pass through an optical filter, which Permits only the radiation characteristic of the element under investigation into the photocell. The output from the photocell represents the concentration and nature of the element Procedure for determination of sodium: Transfer 2, 4, 6, 8 and 10cm’ of standard sodium solution into different 50cm’ volumetric flasks from a burette. Make up all the solutions using distilled water. Stopper the flasks and shake well to get uniform concentration, To the given unknown solution also add distilled water and shake well. Switch on the instrument, turn the gas supply on and light the gas at the burner. Adjust the air supply from the compressor to 1lbs/sq inch using pressure regulator knob. Place the sodium filter (589nm) in position. Now dip the capillary tube in a cell containing distilled water. The steam of air atomized as a fine mist draws up the liquid. Regulate the gas supply so that the colour of the'flame completely turns blue. Adjust the flame photometer to zero by means of zero control knobs, Now feed th sodium ion solution and adjust the reading to hundred. Repeat the process to accuracy of the calibration. , : Feed the various sodiunr ion solutions prepared through the flame by spraying with automiser ‘one by one including the unknown solution. Note down the flame photometer reading. Plot a graph of flame photometer readings against concentrations or vollume of the solution to form the calibration curve. Using the curve obtained find out the volume of the un known solution containing sodium ions and calculate the amount of sodium ions in it, F Result e 100 ppm confirm the Amount of sodium present in the given sample of water is ENGINEERING CHEMISTRY LAB (18CHEL 16/26) PAGE 10 1/11 SEMESTERDEPARTMENT OF CHEMISTRY aor Observations and calculation Weight of sodium per ml of the solution= Vol. of NaCI solution | Emission] Concentration pipetted outinmi_| _response__| _of Na in mg 2 10 Unknown, From the graph, the unknown solution contains-~ -mg of sodium. Intensity Volume of unknown Volume of NaC! ENGINEERING CHEMISTRY LAB (18CHEL 16/26) PAGE 11 1/11 SEMESTERRGIT DEPARTMENT OF CHEMISTRY EXPERIMENT NO:5 Date: DETERMINATION OF pKa OF A WEAK ACID USING pH METER Aim: Determination of the pKa value of a weak acid, Theory: During the titration of an acid with a base, the pH of the solution rises gradually at first, then more rapidly. At the equivalence point there is very sharp increase in pH for a very small quantity of an added base. Once passes the equivalence point, the pH increase only slightly on addition of excess base. On plotting the pH Vs Volume we get the fig. 1. The fig.2 suives the first derivative curve ie. ApH / Av Vs. Volume of base. ApH/AV pH | pké Equivalence point Half equivalence point Vol. of the base > Vol. of the base > According to Henderson Hasselbatch equation pH = pKa + logfsalt] / [acid] where Ka is dissociation constant of ‘the given acid. pKa = - log Ka. At half equivalence point {salt} = [acid] and hence, pH= pKa, Thus pH at half equivalence point gives the pKa of weak acid. Apparatus: pH meter,'beaker and pipette. Procedure: Pipette ouit 25 ml of the given weak acid into a beaker. Immerse the glass electrode and calomel electrode assembly into the acid and cofnect the cell to a pH meter Measure the pH of the acid. Fill a burette with the base (NaOH). In the beginning add large increments of (1 ml) the base to the acid. Stir the solution thoroughly and measure the pH of the solution. When the pH begins to show a tendency to increase rapidly, add only small increments (Say 0.Iml) of the base and measure the pH after each addition. Tabulate the reading as given. Plot a graph of pH (ordinates) against the volume of sodium hydroxide added (abscissa). Determine the pH at half equivalence point. This gives the pKa value of the acid, : Result: pKa of the weak acid is ENGINEERING CHEMISTRY LAB (ISCHEL 16720) PAGE 12, 1/11 SEMESTER.DEPARTMENT OF CHEMISTRY Bor Observations & calculations: Volume of pH NaOH ENGINEERING CHEMISTRY LAB (I8CHEL 16/26) PAGE 13, a 1/11 SEMESTERRGIT DEPARTMENT OF CHEMISTRY EXPERIMENT NO: 6 Date: DETERMINATION OF CO-EFFICIENT OF VISCOSITY OF A GIVEN LIQUID. Aim: To determine the viscosity co-efficient ofa given liquid using Ostwald’s viscometer. Theory: Viscosity is a physical property of liquids i.e. property which opposes relative motion of adjacent layers of liquid. The viscosity of liquid measures this internal friction. The viscosity of a liquid is usually measured by observing the rate of flow of the liquid through capillary tube. It is given Pioseuille formula. V=nprd 8 nl Where, V =Volume of liquid, r = radius of the tube, 1 = length of the tube, p is the pressure difference between the two ends of the tube and 1 is the co-efficient of viscosity. The co-efficient of viscosity is defined as force per unit area (dynes-seconds / sq. cm) required to maintain unit velocity gradient (cm/sec) between two parallel layers of liquid situated unit distance apart. Poise is the unit of viscosity. If equal volumes of 2 different liquids are allowed to pass through the same tube under identical conditions then, Te / Tw = td / tydy Where tr, & ty are the time taken by the liquid and waier to travel through a certain distance in the capillary tube dy, & dy are the densities of the liquid and water. , and thy are co-efficient of viscosity, of the liquid and the water. By knowing the value of ms, m1 can be calculated. . Apparatus: Ostwald’s viscometer, pipette and stop clock Procedure: Determination of viscosity co-efficient Clean the viscometer with water, rinse with acetone and dry it. Fix the viscometer vertically to a stand. Bulb should be immersed in water 10 maintain the lab temperature. Using pipette, transfer known volume (say 10ml) of the water into the wider limb, suck it above the upper mark of viscometer. Allow it to flow freely through the capillary, When the level of water just crosses the upper mark, start a stop clock. Stop the clock when the water just crosses the lower mark. Note the time of flow in seconds (t.). Repeat the same for agreeing values. : Pour out the water, rinse the viscometer with acetone and dry i, fix it vertically to the stand and transfer same volume of test liquid into the wider limb. Determine time (t) taken in seconds by the Jiquid to flow through the same distance in the capillary as determined above. Determine the co-efficient of viscosity of the liquid using the above equation. Result: The co-efficient of viscosity of the given liquid is ~ ~-millipoise. ENGINEERING CHEMISTRY LAB (8CHEL 16726) PAGE 14 1/11 SEMESTERDEPARTMENT OF CHEMISTRY RGIT Observations and Calculation: Room Temperature Density of water, dy = g/cm Density of the given liquid dy = g/cm” Viscosity of water, nw millipoise Measurement of time of flow: Flow of time between A & B (in seconds) Liquid (t) Water(tw) Viscosity of liquid, Ty = _ ty dy X nw - ———rmitipoise ty dy ENGINEERING CHEMISTRY LAB (18CHEL 16/26) PAGE 15 1/11 SEMESTERDEPARTMENT OF CHEMISTRY Ror EXPERIMENT NO: 1 Date: DETERMINATION OF TOTAL HARDNESS OF A SAMPLE OF WATER USING DISODIUM SALT OF EDTA Aim: — To estimate the total hardness of the given water sample using Na;EDTA. Theory: EDTA titration (an example of complexation titration) depends upon the precise determination of the end point. Hardness of the water is due to the presence of calcium and magnesium salts in water. NasEDTA titration may be used for metal ions that do not react (or react unsatisfactorily) with a metal indicator, Structure of EDTA is as follows. HOOC - gee GHe-COOH N-CH2-CH2-N ' 1 HOOC - CH) CH3-COOH During the course of the titration the following reaction takes place: M-—EBT + pA ——. M-EDTA * EBT Metal Indicator. Metll EDTA (Blue colour) (Wine red colour) During the titration’ the free metal ions complexes with EDTA until the metal is displaced from the complex (M- In) to leave the free indicator. The indicator colour is affected by the pH of the solution, Thus Eriochrome Black - T (Hs-In) exhibits the following acid base behavior, which during the titration changes from wine red to blue in the pH range 4-7: Apparatus: Burette, Conical Flask, Standard flask, Pipette and test tube. Procedure: Part~A: Preparation of standard solution of disodium salt of EDTA. Weigh out approximately 4.5 g of disodium salt of EDTA crystals, transfer it to the 250 cm’ standard flask add 2 cm’ of ammonia, then dissolve it in ion-exchange water, make it up to the mark, shake thoroughly, calculate the molarity. Part-B: Determination of total Hardness of Water sample. Pipette out 25 cm’ of the given water sample into a clean conical flask, add 2 cm’ NH3 ~ NHACI buffer and a pinch of Eriochrome blank:—T indicator. Titrate against EDTA solution till the colour of the conical flask solution changes from wine red to clear blue. Let the volume of EDTA consumed be X cm* : ppm of CaCOs, Result: The total hardness of the given water is sample is ENGINEERING CHEMISTRY LAB (18CHEL 16/26) PAGE 16 1/11 SEMESTERDEPARTMENT OF CHEMISTRY RGIT Observations and Calculations Preparation of standard Na,EDTA: 1, Weight of the bottle + NaEDTA crystals = Wi= 2. Weight of the bottle after transfer 3. Weight of Na,EDTA crystals ( Wi- W2) Mepta= _ Weight ofNaEDTAx4 = Mol. Weight of NasEDTA. 372.24 Determination of total Hardness of water sample. Burette Standard: Na,EDTA Solution. Conical Flask : 25 cm’ of water sample + 2 cm’ of ammonia-ammonium chloride buffer. Indicator End Point Wine red to Blue. rigchrome Black- T. Burette Reading I I UL Final Reading Initial reading Volume of NaxEDTA rundown in cm* Titre Value = x cm* 1000cm* | M gpra= 100g of CaCOs (Mol. mass of CaCO; =100) ‘ Xom'ofZMEDTA= _XxZx100 gofCaCO; = --(a) 1000 x 1 25 cm’ of hard water sample contains a g of CaCOs. Therefore 10° cm’ (1 million cm’) of hard water sample contains = ax 10° -ppm of CaCOs. 28 Thus the total hardness of the given water sample is = - ppm. of CaCOs ENGINEERING CHEMISTRY LAB (18CHEL 16/26) PAGE 17 : 1/11 SEMESTERDEPARTMENT OF CHEMISTRY RG EXPERIMENT NO. 2 Date: i * DETERMINATION OF PERCENTAGE OF CALCIUM OXIDE IN THE GIVEN SAMPLE OF CEMENT,(RAPID Na:EDTA METHOD) AIM: To determine the amount of calcitim oxide present in the given sample of cement solution using Na3EDTA. solution. Theory: Cement contains oxides of calcium, magnesium, silica and small quantities of iron. The indicator used is' Patton and Reeder’s [2-hydroxyl —1- (Ihydroxy-4 sulpho —Ir naphthylazo) ~3- naphthoi¢ acid, abbreviated as HHSNNA]. Its main use is in the direct "titration of calcium, particularly in the presence of magnesium, The interference of ‘magnesium ions is avoided by precipitating them as hydroxides by the addition of 4 N NaOH. And pH of the solution is maintained at 12 - 14 by adding 5 cm? diethylamine. A sharp end point is obtained by adding 5 cm? 1:1 glycerol. The colour changes from wine red to pure blue when calcium ions are titrated with Na,EDTA solution. Apparatus: Burette, Conical flask, Pipetie, Standard flask. Procedure: Part A: Preparation of standard solution of di sodium EDTA solution Weigh out approximately 4.5 g of disodium salt of EDTA crystal, transfer to the 250 em? standard flask add 2 cm’ ammonia then dissolve it in ion exchange water. Make it upto the mark, shake thoroughly and calculate the molarity, Part-B: —_ Estimation of calcium oxide: Pipette out'25 cm’ of the given cement solution into a clean conical flask. Add 5 cm’ of 1:1 glycerol with constant: shaking of the contents of the flask ‘followed by 5 cm? of diethylamine (To adjust the pH of the solution to 12 or slightly higher). Add’ 10 cm? of 4N NaOH. Mix the solution well. Add a pinch of Patton and Reeder’s indicator. Titrate against EDTA solution till the colour changes from wine red to clear blue. (Perform the titration very slowly near the end point). Let the volume consumed be Y cm’, Results: The percentage of calcium oxide in the given cement sample is-- ENGINEERING CHEMISTRY LAB (I8CHEL 16/26) PAGE 18,DEPARTMENT OF CHEMISTRY Observations and Calculations Preparation of standard Na,EDT. 1. Weight of the bottle + Na,EDTA erystals = Wi= Mol. Weight of Na; Estimation of calcium oxide: Burette : Standard Na,EDTA Solution. Conical Flask : 25 cm? of cement solution + 5 cm’ of 1:1 glycerol + Sem’ of Diethylamine +% "tt. of 4 N NaOH Indicator _: Patton and Reeder’s. End Point —_: Wine red to Blue. Burette Reading 1 I I Final Reading Initial reading Volume of Na:EDTA rundown in cm’ 2 Weight of cement = b= 8 1000 cm? of 1 Mepra = 56.08 g CaO (Mol. mass of CaO =56.08) (a) Xm? of ZMEDTA= XxZx 56,08 g of CaO 1000 x 1 ‘Amount of CaO present in 25 cm’ of cement solution =a g ‘Therefore amount of CaO present in 250 cm’ solution = 10 a= —-— Percentage of CaO in the given cement solution= 10. ax 100 b ENGINEERING CHEMISTRY LAB (18CHEL 16/26) Titre Value = x cm? RGIt PAGE 19 1/11 SEMESTERRGIT DEPARTMENT OF CHEMISTRY EXPERIMENT NO: 3 Date: DETERMINATION OF PERCENTAGE OF COPPER IN BRASS USING STANDARD SODIUM THIOSULPHATE SOLUTION AIM: To determine the percentage of copper present in brass alloy using standard sodium thio- sulphate solution. Theory: Brass is an alloy of copper (80%) and Zinc (20%). Dissolving the sample in minimum amount of nitric acid makes a Solution of brass. Excess of nitric acid is removed by boiling with urea. Copper sulphate when dissolved in water undergoes hydrolysis to form cupric hydroxide. . 2CuSO, + 4H230 —— 2Cu (OH) + 2H2SO4 When aqueous solution of ammonia is added to Cu ** hydroxides dissoive giving an intense blue colour due to the formation of copper ammonia complex. Cu (OH) 4+ 4ANHs ——+ [Cu (NH3), °° + 20H" The cuprammonium complex decomposes in the presence of glacial acetic acid and potassium iodide to give pale blue coloured complex and free iodine. ’ 2 [Cu(NH),"* + Ht +4 KI ——+ Cub +h+ 4K! +H The free iodine liberated is, titrated against sodium thiosuphate using starch as indicator. Starch is an absorption‘indicator. The free iodine oxidizes sodium thiosulphate to Na2S4O (sodium tetra thionate) while itself gets reduced to sodium iodide. 2NaS203!"+ lz = ———— NayS,Oe* + 2.Nal Apparatus: Conical flask, Burette and test tube. Procedure: Part-A: Preparation of brass solution. Weigh out approximately 0.12 g of the given brass sample and transfer it into a conical flask. Add quarter test tube of 1:1 nitric acid. Cover the mouth of the flask with a glass funnel and boil tll alloy dissolves and all the brown coloured oxides of nitrogen are completely expelled, Add 10 em* of ion exchange water and 1g of urea, continue the boiling for few more minutes to destroy the excess of nitrous fumes present, and then cool the solution, Part-B: Estimation of copper. To the brass solution add drops of liquor ammonia till the formation of turbidity. Dissolve this in 1 cm’ of acetic acid. Cool it again, then add 10cm’ of 10% KI and immediately titrate the liberated iodine against sodium thiosulphate solution till the pale yellow colour develops. Add lem? of starch and continue the titration till the blue colour disappears leaving behind white Cuprous iodide precipitate. Repeat the same with another brass sample. Result: The percentage of copper present in the given brass sample is - ENGINEERING CHEMISTRY LAB (18CHEL 16/26) PAGE 20 1/11 SEMESTERDEPARTMENT OF CHEMISTRY Observations and Calculations Estimation of copper in brass sample Burette : NazS,03 solution Conical Flask: Brass solution + 1:1 NH,OH dropwise (till slight ppt) + Acetic acid dropwise (till pale blue) + 10cm’ of 10%KI (reddish yellow ppt)- Titrate Indicator : starch (6 drops towards the end point) End Point : Blue to creamy white ppt RGIT Burette reading Weight of Brass Final Reading Initial reading ‘Volume of NazS:0; rundown in cm? Normality of NazS203 = Y = 0.05N lcm of INNaS:03; = | milliequivalent of copper. (One equivalent of Cu = atomic mass of copper = 63.54) Therefore, 1 cm’ of IN NazS203 = 0.06354 g of Cu. X cm of Y N NaS203 =0.06354 x Xx Y gofCu = (ag Therefore, percentage of copper in the given brass sample = ax 100 w ENGINEERING CHEMISTRY LAB (I8CHEL 16/26) PAGE 21 1/11 SEMESTERDEPARTMENT OF CHEMISTRY th RGIT EXPERIMENT NO: 4 Date: DETERMINATION OF IRON IN THE GIVEN SAMPLE OF HAEMATITE ORE SOLUTION USING POTASSIUM DICHROMATE CRYSTALS BY EXTERNAL INDICATOR METHOD Aim: To determine the amount of iron present in haematite ore solution using standard solution of potassium dichromate, , Theory: Tron does not occur free in nature, since the humid atmosphere easily attacks it. lacmatite ore is Fe2O3..2H20. The following reaction takes place when it reacts with HCl Fe,03 +6HCl —> 2FeCl;+3H,0 For the estimation, fertic ions are reduced to the ferrous state. Reduction is carried in the Presence of acidified stannous chloride solution. The complete reduction is ensured by the addition of slight excess of stannous chloride, 2FeCls +SnC——* 2F eC}, +SnCly This solution is then cooled and the excess of stannous chloride is removed by adding a saturated solution of mercuric chloride. SnCh (Excess) +HgCh = ——+ SnCl,+2Hg.Cl, } Fe then reacts with ferricyanide ion to form the blue coloured complex (Ferro-ferricyanide complex), 3Fe" + [Fe(CN)s]* —* [Fes (Fe(CN)s 2] (Blue coloured complex. ) The following reaction occurs when the conical flask solution is titrated against standard potassium dichromate solution, 6Fe** +Cr07*+14H' —__» 6Fe* +2 Cr" + 7H,0. Apparatus: Burette, Conical flask, Standard flask, Pipette and test tube. Procedure: Part-A: Preparation of standard KCrz 0; Solution Weight out approximately 1.25 g of potassium dichromate crystals, transfer it to 250 cm’ standard flask. Dissolve it in ion exchange water, make it upto the mark, Shake thoroughly. Calculate the normality. Part-B: Estimation of Iron. Pipette out 25 cm’ of the haematite solution into a clean conical flask. Add quarter test tube of concentrated HCl. Heat to the boiling, add stannous chloride solution drop wise till the solution becomes colourless, cool under the tap water and to the cold solution add drop wise mercuric chloride solution — a silky white precipitate should be formed. If black precipitate is formed, discard the solution and repeat the experiment. Add two test tubes of distilled water. Titrate against dichromate solution using potassium ferricyanide, KsFe(CN)s as external indicator. On the wax paper place drops of indicator in series. Run down dichromate solution, shake and bring drop of reaction mixture with the help of glass rod in contact with the indicator. Clean the glass rod after every test. Initially the colour will be dark blue, changes to blue, bluish green and finally fails to develop blue colour with the test drop. Repeat the titration for concordant values and calculate the percentage of iron. Result: The percentage iron in the haematite solution is ENGINEERING CHEMISTRY LAB (18CHEL 16/26) PAGE 22 1/11 SEMESTERDEPAl y RTMENT OF CHEMISTRY RGIT Observations and Calculations Preparation of standard K,Cr,0- 1. Weight of the bottle + KxCr:0; crystals = Wi= 2. Weight of the bottle after transfer = W: 3. Weight of KCr2O> crystals. (Wi- W2) = W = Nuoceor = WeightofKxCnO7x4 = Wx4 Eq. wt. of KxCr:07 490s Estimation of percentage of Fe: Burette - — : Standard KxCr.0; Solution. Conical Flask: 25 cm? of Haematite solution + 5 cm’ of Conc.HCl + Heat + SnClz dropwise(till colourless),cool +1 t.t Water.+ 1/2t-t. HgClz (silky whiteppt) Indicator _: Potassium ferricyanide (Extemal) End Point _ : Deep blue to original colour of the indicator. Burette Reading 1 a UL Final Reading Initial reading ‘Volume of K2Cr207 rundown in cm* Titre Value = x cm* Weight of Haematite = lcm? IN K2Cr,07 =I milliequivalent of Fe Jem? IN K3Crs07=0.05585 g of Fe (1 equivalent of Fe = atomic mass of Fe = 55.858) X om? of ZN KzCrO7 = 0.05585xXxZ g of Fe —-(a) Amount of Fe present in 25 cm’ of Haematite solution =a g of Fe Therefore, Amount of Fe present in 250 cm? of Haematite solution = 10 a= --—--—~ Percentage of Fe in the given Haematite solution = 10a x 100 b ENGINEERING CHEMISTRY LAB (I8CHEL 16/26) PAGE 23 1/11 SEMESTERDEPARTMENT OF CHEMISTRY RGIr EXPERIMENT NO: 5 Date: DETERMINATION OF CHEMICAL OXYGEN DEMAND (COD) OF THE GIVEN INDUSTRIAL WASTE WATER SAMPLE Atm: To determine the chemical oxygen demand (COD) of the given wastewater ample. : Theory: The chemical oxygen demand is usually defined as the amount of oxygen used while oxidizing the organic and inorganic matter of a sample with a strong chemical oxidant under acidic condition. This is important for industrial waste studies. The oxidizable constituents of wastewater include straight chain aliphatic compounds, aromatic hydrocarbons, straight chain alcohol, pyridine and other oxidizable materials. Straight chain compounds and acetic acid are oxidized more effectively in silver ions (Silver sulphate) as catalyst. However the silver ions become ineffective in presence of halide ions (present in wastewater) owing to the precipitation of silver halide. This difficulty is overcome by treating the wastewater with mercuric sulphate, because mercuric ions binds the halide ions and makes them unavailable to bind with silver ions. Apparatus: Burette, standard flask, pipette, and conical flask. Procedure: Part-A: preparation of standard FAS (Mohr’s salt) solution, Weigh out approximately 10 g of FAS crystals and transfer to a 250 cm? standard flask with the help of a funnel. Add 2 test tubes of dilute sulfuric acid and shake well to dissolve the crystals. Make up the solution to the mark with water and shake thoroughly. Calculate the normality. Part-B: Determination of COD of wastewater sample: Pipette out 25 cm? of the wastewater sample into a 250 cm? conical flask. Add 10 cm? of standard potassium dichromate solution followed by 30 cm? of dilute sulfuric acid with constant shaking. Add boiling chips to flask. Attach a reflux condenser and reflex the mixture for half an hour. Cool the solution, wash the condenser with ion exchange water and washings are transferred to the flask. Add 2 to 3 drops of Ferroin indicator and titrate against the Mohr’s salt solution. The colour tums bluish green to reddish brown. Blank titration is done at same experimental condition except wastewater sample. Take the difference between blank and back titration. Calculate the COD of the wastewater sample. ; -mg /dm* Result: The COD of wastewater sample is ENGINEERING CHEMISTRY LAB (I8CHEL 16/26) PAGE 24 1/11 SEMESTERDEPARTMENT OF CHEMISTRY RGIT Observation and Calculation Preparation of standard FAS: 1. Weight of the bottle + FAS crystals = Wi= 2. Weight of the bottle after transfer 3. Weight of FAS crystals =W= N ras = __Weightof FAS x4. = Eq. wt. of FAS. Estimation of COD: Burette : Standard FAS Solution. Conical Flask : 25 om’ of wastewater + 10 cm’ of 1:1 H2SO4+ 10cm’ of KxCr,O7 Indicator: Ferroin (2 to 3 drops). End Point: Bluish green to reddish brown. Burette,Reading I IL Fa Final Reading Initial reading Volume of FAS rundown in cm* ‘The blank titration value X= 25 em’ Titre Value = Y cm? 1 cm’ 1 N FAS solution = Imilli equivalent of oxygen = 8 mg of oxygen (X-Y) em’ of Z N FAS solution = 8 x (X-Y) x Z ~-(a)mg of oxygen i.e. 25 em? wastewater sample contains a mg of oxygen For 1000 cm’ of wastewater sample contains = a x 1000 ---(b)mg of oxygen 25 Therefore the COD of wastewater sample = ~--(b) mg of oxygen per dm? ENGINEERING CHEMISTRY LAB (I8CHEL 1626) PAGE 25 1/11 SEMESTERDEPARTMENT OF CHEMISTRY Retr EXPERIMENT NO: 6 Date: Estimation of percentage of available chlorine inthe given sample of bleaching powder AIM: Estimation of percentage of available chlorine in the given sample of bleaching powder THEORY: ENGINEERING CHEMISTRY LAB (18CHEL 1626) PAGE 26 1/11 SEMESTERDEPARTMENT OF CHEMISTRY RGIT Observation and calculation: ENGINEERING CHEMISTRY LAB (I8CHEL 16/26) PAGE 27 1/11 SEMESTERDEPARTMENT OF CHEMISTRY : RGIT VIVA-VOCE QUESTION: GENERAL: - What is the standard solution? . Define Normality, Molilty & Molarity, |. What is meant my titration? |. What is an indicator? Explain the different types of indicator with examples. Define equivalent weight and molecular weight. .._ Define end point, Neutralization & equivalence point. - What is meant by oxidation and reduction reaction? Give exainples. . What is meant by redox reaction? Give example What is a buffer? What are the different types of buffer? Give examples. |. Define pH, pOH? - What is the pH range of acid, base and neutral solution? . Define acid and base. Give example. . What is meant by weak acid & strong acid? Give examples - What are ligands and coordination compounds? Give examples PART- A Potentiometric estimation of FAS using standard potassjum dichromate solution? 1, What are Potentiometric titrations? The determination. of the equivalence point of red-ox titrations on the basis of potential measurements is called a potentiometric titration. 2. What is its principle? The principle involved in Potentiometric titration is the measurement of the emf between two electrodes, an indicator electrode and a reference electrode. In these titrations, measurements of emf are made while the titration is in progress. The equivalence point of the reaction is revealed, by a sudden change in potential, in the plot of emf readings against the volume of titrant.. 3. What are the electrodes used in the titrations? The indicator electrode used is the platinum electrode (acts as an anode) arid the reference electrode used is the calomel electrode (acts as a cathode). 4. What is determining factor in the oxidation and reduction reaction? The determining factor is the ratio of the concentrations of the oxidized and reduced formsie., Fe’* <—» Fe +e 5. What is an indicator electrode? The electrode whose potential is dependent upon the concentration of the ion to be determined is termed as the indicator electrode. 6. What is the reaction that occurs between FAS and KCr,0;? a) Acidified potassium dichromate oxidises ferrous sulphate to ferric sulphate and itself gets reduced to'chromic sulphate. GFeSOx + 7H2SOs + KzCr07 > 3Fex(SO4)s + K2SOx + Crx($O4)3 +7H0 ENGINEERING CHEMISTRY LAB (I8CHEL 16/26) PAGE 28 1/11 SEMESTERDEPARTMENT OF CHEMISTRY RGIT 7. Explain the change in the Potentiometric curve? The initial change in potential is due to change in conc. of log[Fe**{Fe*'], at the equivalence point is due to logiFe"/[Cr’*] and after the equivalence point it is due to change in cone. of log(Cr*)/{Cr'"] 8, What are the advantages of Potentiometric titrations? i) Turbid, fluorescent, opaque or coloured solutions can be titrated. ii) Mixture of solutions or very dilute solutions can be titrated. iii) The results are more accurate because the actual end point is determined graphically. 9. What are the other methods of determining the concentration of FAS? Titrimetric method- internal indicator, external indicator Colorimetric determination of copper. 1. What is-colorimetry? Chemical analysis through measurements of absorption of light radiation in the visible region of the spectrum (400-760 nm) with respect to a known concentration of the substance is known as colorimetry. 2. What forms the basis for Colorimetric determination? The variation of colour of a system with change in concentration of some component forms the basis for the Colorimetric determination. 3. What are filters and why they are used? The filters consist of either thin films of gelatin containing different dyes or coloured glass. The filters are used in colorimeters for isolating (selecting) any desired spectral region. 4, What is photoelectric colorimeter? It is an electrical instrument, which measures the amount of light absorbed using a photocell. 5, What are wavelength, frequency and wave number? The distance between any two successive peaks or troughs of waves is called wavelength. It is represented by 2. Frequency is the number of waves passing through a point per second, and is represented byy. ‘Wave number is the reciprocal of wavelength. It is represented by n. 6, State Beer’s law and Lambert’s law? Beer's law-The intensity of a beam of monochromatic light decreases exponentially as the concentration of the absorbing substance increases arithmetically. Lambert's law-When a monochromatic light passes through a transparent medium, the rate of decrease in intensity of light is proportional to the thickness of the medium, 7. State Beer - Lambert's law? “The amount of light absorbed is directly proportional to the concentration and path length of the solution. AxC 1 ERING CHEMISTRY LAB (I8CHEL 16/26) PAGE 29 1/11 SEMESTERDEPARTMENT OF CHEMISTRY Rat 8. What is calibration curve? It is the plot of optical density (absorbance) against concentration o solutions obeying Beer’s law, this is a straight line. f known solutions. For 9, What is meant by transmittance, absorbance? ’ Itis the ratio of amount of light transmitted (It) to the total amount of light absorbed (10) Wl, =T Reciprocal of transmittance, Iy/h is called absorbance or optical density A = log Iy/ly= log I/T = -log T ‘ 10. Why ammonia is added and what is the complex formed? ‘Ammonia is added to get cuprammonium sulphate, [Cu(NH3).JSO« a dark blue complex. Same amount of ‘ammonia is added to nullify the absorbance due to any coloring impurities present in ammonia. : 11. What is blank solution? ‘A blank solution is identical in all respects to the test solition except for the absence of test solute. 12. Why the estimation:of Cu is done at 620 nm wavelength? The estimation of copper is carried at 620 nm wavelength because; the complex shows a ‘maximum absorbance at 620 nm, 13, Can different Nessler’s tubes be used during optical density measurements? . Different Nessler’s tubes cannot be used during optical density measurements of solutions, because absorbance depends on the path length of the solution. 14, What are the types of Colorimetric analysis? (1)Colorimeter (2) Spectrophotometer. Conductometric Estimation of HCI and CHsCOOH in a given acid mixture using standard NaOH solution. 1, What is conductance? The reciprocal of resistance is called the conductance 2. What is unit of conductance? ‘The unit of conductivity is ohm" m" or Sm. 3, What is conductivity? The reciprocal of resistivity is called conductivity. 4, State ohm’s law? ‘Ohm’s law states that the current, I (ampere), flowing in a conductor is directly proportional to the applied electromotive force, E (Volt) and inversely proportional to the resistance R (ohm) of the conductor. I= E/R 5. Explain different types of conductivities? ‘A solution may have the following conductivities. Specific conductivity- it is the conductivity of a solution between lem? area and kept 1 cm apart. k=C (Va), If]=1cmanda=1 cm’, then ENGINEERING CHEMISTRY LAB (I8CHEL 16726) PAGDEPARTMENT OF CHEMISTRY RGIT Equivalent conductivity- itis the conductivity of the solution, which contains 1g equivalent of solute, when placed between two electrodes kept | cm apart. M=KV 2, =K x 1000 /C V = Volume containing 1 gram equivalent of solute. C= Concentration of solution. K = Proportionality constant Molar conductivity-It is the conductivity of a solution, which contains 1g molecular weight of a substance, when placed between two electrodes of 1 cm apart. H=KV, 6. Which type of conductivity is measured during conductometric titration? The specific conductivity is measured. The unit is ohm'cm™ ‘What is the principle involved in the conductometric titrations? | ‘ The principle underlying conductometric titration is the replacement of ions of a particular conductance by ions of different conductance during the titration. What is a cell? ; A device, which produces an electromotive force and delivers an electric current as the result of a chemical reaction, is known as a cell, 9. What factors determine the conductance of a solution? Two factors determining the conductance of a solution are i) Mobility of ions - higher the mobility, higher is the conductance and ii) Number of ions - more the number of ions in solution, more is the conductance. 10. What is conductivity cell? ‘ It consists of two Platinum electrodes of one square centimeter area, kept one centimeter apart and measures the conductance of the solution. 11. What is a neutralization point? The point at which acid is completely reacted by a base or vice versa is called Neutralization point. 12, In the titration of acid (HCI) with a strong base (NaOH), the conductance first decreases, then rises, Why? Upon adding. a strong base to an strong acid, the conductance falls due to the replacement of highly mobile H" ions of the strong acid (HCI) by less mobile Na* ions of the base. The conductance then rises as excess of alkali is introduced, due to high mobile OH ions. . 14. What are the advantages of conductometric titrations over visual titrations? i) The method is accurate in dilute as well as more concentrated solutions. ii) It.can also be employed with coloured solutions iii) Very weak acids such as H3BOs, phenol, which aqua solutions, can be titrated conductometrically. iv) Mixture of acids can be titrated more accurately. cannot be titrated potentiometrically in ENGINEERING CHEMISTRY LAB (18CHEL 16726) PAGE 31 1/11 SEMESTERDEPARTMENT OF CHEMISTRY RGIT 15. What are the applications of conductometric titrations? i, To determine the solubility product of sparingly soluble substances. ii, To determine the equivalence conductance of weak electrolyte. iii, To determine the strength of mixture of acid. iv. To determine the degree of dissociation v. To determine the ionie product of water vi. In precipitation titration. FLAME PHOTOMETRY 1. What is flame photometry? 2.Explain the principle involved in flame photometry. 3. Explain the sequence of reaction, when a metal is aspirated in the flame. 4.Give the relation between emited radiation and concentration 5.What are filters? what is the frequency in which sodium is analyzed. 6.How stock solutions ate prepared. 7 what is the colour obsérved, when sodium is present in the solution and why? Determination of pKa value of a,weak acid using pH meter. 1, What is pKa of a weak acid? pKa is a modem method of expressing the strength of weak acids and is mathematically expressed as pKa = - logl0 Ka Where Ka is the dissociation constant of the weak acid 2. What is meant by pH of a solution? pH of a solution is the negative logarithm to the base 10 of hydrogen ion concentration. PH =- logl0[H"] 3. What is the modern definition of pH (IUPAC)? The difference in pH between two solutions S (a standard) and X (an unknown) at the same temperature with the same reference electrode and with hydrogen electrodes at the same hydrogen pressure and is given by: pH(X) -pH(S) = Ex-Es /2.3026RT/F / Exis e.m.f. of the cell in unknown solution, and Es is e.m.f of the cell in standard solution. 4, What are the electrodes used during the experiment? Glass electrode (working electrode) and calomel electrode (reference electrode), 5. Why the glass electrode is used as an ion selective electrode? The glass electrode is called an ion selective electrode because, it is able to respond to certain specific ions (H'ions) and develop a potential while ignoring the other ions in 2 solution. 6. How are pH and pKa related? Why pKa is measured at half equivalence point? Henderson-Hasselbalch equation, pH = pKa + log!0 [salt] /[acid] At half equivalence point [salt] = [acid]. Therefore, pH at half equivalence gives the pKa of the weak acid. ENGINEERING CHEMISTRY LAB (I8CHEL 16/26) PAGE 32 1/11 SEMESTERRGIT DEPARTMENT OF CHEMISTRY 7, Why pH increases suddenly after the equivalence point? ‘AL the equivalence point, the base has neutralized all the weak acid. Afterwards the concentration of hydréxyl ions increases resulting in the sudden increase of pH. 8. Define degree of dissociation. Itis the measure of extent of a dissociation of weak electrolyte. 9. Explain Ostwald’s dilution law. K = Ca? where K is dissociation constant, C is concentration and o is degree of dissociation. Determination of viscosity coefficient of a liquid using Ostwald’s viscometer. 1. What is viscosity? Viscosity arises due to internal friction between moving layers of molecules. A moving layer exerts a drag or friction on its nearest moving layer backward, This property of a liquid by which it retards or opposes motion between the layer is called viscosity. 2. What is viscosity co-efficient of a liquid? The viscosity co-efficient of a liquid is defined as the tangential force per unit area required to maintain a unit velocity gradient between any two successive layers of a liquid situated unit distance apart. 3. What is the SI unit of viscosity co-efficient? The viscosity co-efficient is expressed as Pascal second (Ps) IPs = 1 kg ms 4, What is-density ofa liquid and specific gravity? How they are related? The density of a liquid is the mass of its unit volume. Specific gravity or the relative density is the weight of a given liquid divided by the weight of an equal volume of water at the same temperature. Density of liquid = Specific gravity of the liquid X Density of water at that temperature. 5. What are the factors that affect the viscosity of a liquid? i) Increase in molecular weight results in an increase in viscosity. ii), Branched chain compounds have higher viscosity than those involving straight chain compounds. fii) The polar compounds are more viscous than the non-polar ones, The presence of hydrogen bonds causes the viscosity to increase, iv). The viscosity of liquids increases by the presence’ of lyophilic colloids and suspended impurities. 'y). Temperature has marked influence on the viscosity of a liquid (about 2% per degree). 6. Define Poiseuille Law? The law based on the viscous flow of liquids through capillary tubes is Poiseuille law. It is expressed as. y= mpr't/ 8V1 1 = Viscosity co-efficient, p = hydrostatic pressure, r= radius of the tube, t is the time of flow, V is the volume of the liquid, | is length of the capillary 7. How does viscosity vary with temperature? The viscosity of a liquid usually decreases with the rise of temperature. ENGINEERING CHEMISTRY LAB (18CHEL 16/26) PAGE 33 1/11 SEMESTERRGIT DEPARTMENT OF CHEMISTRY 8. Why should the viscometer be dry before the measurement is done? The viscometer should be dried to avoid the formation of emulsion, which changes the rate of flow of the liquid. 9. Why acetone is used for cleaning viscometer? Acetone is a volatile organic liquid. To dry the viscometer quickly, it is rinsed with acetone 10. Why viscosity measured at constant temperature? 4 Because, the physical constants like density and viscosity of a liquid vary with temperature. 11. What is the name of the Viscometer? Name the type of viscosity measured? Ostwald’s viscometer. Relative Viscosity. 12. Why equal amount of water and liquid is taken in the viscometer? To maintain same hydrostatic pressure. 13, How is viscosity ofa liquid related to its mobility? Viscosity of a liquid is inversely proportional to its mobility. 14, What is fluidity of a liquid? Fluidity of a liquid is the reciprocal of viscosity co-efficient. It is a measure of the ease with which the liquid flows, Fluidity, @= 1/1, 7 = the viscosity co-efficient. PART-B Determination of Total Hardness of the given water sample. 1, What is hard water? Hard waters are generally considered to be those waters that require considerable amounts of soap to produce foam and lather and that also produce scale in hot water pipes, heaters, boilers, etc. 2. What are the different types of hardness of water. ? Temporary hardness is due to bicarbonates of Ca & Mg and Permanent hardness is due to sulfates & chlorides of Ca & Mg. 3. How are the water classified based on the degree of hardness. ? Soft water- 0-75 mg / It Moderately hard water 75- 100 mg / It Hard water 150- 300 mg /It Very hard water > 300 mg/lt 4, How is hardness of water caused? Hardness of water is caused by divalent metallic cations in association with anions such as HCO;,, $O,"; CI’, SiO", etc. The principal hardness causing cations are calcium and magnesium. 5. How is temporary hardness removed? The temporary hardness of water can be removed by boiling water during which bicarbonates decompose to give carbonates. How do we express the total hardness of water? Itis expressed as parts per million of calcium carbonates.’ 7, What is EDTA.” ENGINEERING CHEMISTRY LAB (I8CHEL 16/26) PAGE 34DEPARTMENT OF CHEMISTRY EDTA is Ethylene diamine tetra acetic acid. 8 ENGINEERING CHEMISTRY LAB (I8CHEL 16726) RGIT Write the structural formula of EDTA. ? HOOC CH: Gf Coon N—CH—CH-N HOOC—CH, CH>—COOH Why is di sodium salt of EDTA is preferred to EDTA. ? EDTA is sparingly soluble in water. Therefore, its disodium salt is preferred. Why is NH; solution added while preparing EDTA solution? Ammonia solution is added during the preparation of EDTA solution to increase the rate of dissolution of the salt. Why is NHs - NH,CI buffer added? Ammonia-ammonium chloride buffer is added to maintain a.pH of 10, the desired pH for the titration. Why is the indicatot EBT shows wine red colour at the beginning and blue colour attheend.? When a small amount of Eriochrome Black T, which is blue in colour, is added to hard water with a pH of about 10.0, it combines with a few of the calcium and magnesium ions to form a complex which is wine red in colour as shown in the equation, M” +EBT > (M-EBT) (Wine red complex) During: the titration with EDTA, all free hardness ions are-complexes according to the equation. : M-EBT + EDTA > (M-EDTA) (stable complex) + EBT (Blue colour) This action frees the Eriochrome Black T indicator from the complex. (M-EBT), and the wine red colour changes to a blue colour showing the end point of the titration. How do you prepare 0.01M EDTA solutions? ‘Ww/lt = Molecular wt X Normality = 372 X 0.01'=3.72 gin 1 lt How EDTA reacts with Metal ions? Write the reaction. And also give the complex structure, M-EBT+EDTA> M-EDTA + EBT (wine red) (stable complex ) (blue) . O— OC—CH, : PAGE 35 ; 1/11 SEMESTERDEPARTMENT OF CHEMISTRY RGIT 15. Write the structure of EBT? N10 rs NO 16. Why are the titrations involving EDTA carried out slowly towards the end point? The titrations involving EDTA are carried out slowly towards the end point, because the rate of formation of the metal complex of EDTA is very slow. on 17. What is the application of hardness data in environmental engineering practice? 1D Hardness of water is an important consideration in determining the suitability of water for domestic and industrial uses 1) Determination of hardness serves as a basic for routine control of softening processes. Determination of Amount of Calcium oxi in the given cement solution 1. What are the constituents of Portland cement? ? Oxides of Calcium, Magnesium, Iron, Aluminium and Silicon are the constituents of cement, 2. What is the percentage of CaO in cement? Calcium oxide (60 %) is a prime constituent of ‘cement, 3. What is the role of glycerol? Glycerol is added to get the sharp end point. . Why diethylamine is added? Diethylamine is added to maintain a PH of about 12.5 5. What is the function of sodium hydroxide? Itis added to mask the Mg ** ions by forming Mg(OH): Precipitate and will not allow to interfere during the complex formation of Ca with indicator. 6. What is the indicator ised. Write its structure? OH HO COOH Se ss Patton-Reeders is the indicator used. 7. Why EBT indicator cannot be used in this experiment. ? 5 CHEMISTRY T 1/11 SEMESTERDEPARTMENT OF CHEMISTRY RGIT Eriochrome Black T indicator cannot be used in this experiment, because it forms a very weak complex with calcium ions in the pH range 12-14. So Patton and Reeder’s indicator is used in the determination of CaO in cement solution. Determination of percentage of copper in Brass using standard sodium thiosulphate solution. 1, What is brass? And what are its constituents? Brass is an alloy of copper (50-90%) and Zinc (20-40%). It also contains small quantities of tin, lead and iron, How brass solution is prepared? Brass solution is prepared by dissolving the brass foils in 1:1 nitric acid and heating it to expel the oxides of nitrogen fumes, then one test tube of water and a pinch of Urea is added to destroy excess of nitric acid. Thus brass solution is prepared. - Explain the role of nitric acid while preparing the brass solution? [tacts as an oxidizing agent, it converts metallic Cu° to ionic Cu2* and dissolves it 4, What is the purpose of adding Urea? Urea is added to destroy excess of nitric acid . What happens when water is added to the brass solution? Write the reaction? Copper hydroxide is formed, Cu* + 20H” >Cu(OH)2 6. Why ammonium hydroxide is added to the brass solution? Write the reaction, Ammonium hydroxide is added to neutralize the mineral acid. A dense blue coloured cuprammonium complex is formed with the excess of ammonia solution. Cu (OH), +'4NH; > [Cu (NH;), 2 +20H" Why is acetic acid added? Acetic acid is added to neutralize the excess of ammonium hydroxide and to make the solution slightly acidic. 8. Why KI is added to the brass solution, though Cu in brass is determined. Write its reaction, Cupric ions do not react with sodium thiosulphate solution. However, cupric ions oxidize potassium iodide and iodine is liberated. The amount of iodine liberated is equal to the amount of cupric ions present in the solution. 2Cu +4KI> Cwh +h+4K" 9. How is liberated iodine reacts with sodium thio sulphate? Todine reacts with sodium thiosulphate to form sodium iodide and sodium tetra thionate, which are colorless products. 2Na2$203 + Iz > NazSsOc + 2Nal 10, What is the indicator used and write its structure? Starch is the indicator used. (CH.OH HOH i on ou | : Hon : ENGINEERING CHEMISTRY LAB (18CHEL 16/26) PAGE 37 1/11 SEMESTERRoIr DEPARTMENT OF CHEMISTRY ic ii 1? 11. Why starch indicator is added towards the end point If the intensity of iodine is more, the indicator, starch forms a stable water insoluble starch-iodide complex when reacted with iodine. As a result, the volume of sodium thiosulphate consumed will be less than expected. 12. What is white precipitate produced at the end point? ‘The white precipitate produced at the end point is cuprous iodide. Determination of Iron in the given sample of Haematite ore solution.(external Indicator method) 1. Name few ores of iron. . Magnetite (Fe;O,), Haematite (Fe 03), Iron pyrite (FeS), Syderite (FeCO3). 2. What are the main constituents of Haematite of ore? Hematite is an important ore of iron containing mainly ferric oxide. 3. What is role of conc. HCI and stannous chloride? Write the reaction? It dissolves oxides of Fe to Chlorides of Fe and provides acidic medium, Stannous chloride is added to reduce the ferric ion to ferrous ion and slight excess is added to ensure complete reduction, : 2FeCl; + SnClz > 2FeCl; + SnCly, 4. Why HgCl, is added. Write the reaction? Meteuric chloride is added to remove the excess stannous chloride, Mercurie chloride reacts wih stannous chloride, get itself reduced to form a silky white precipitate of mercurte chloride. i SnCk + 2HgCh > HeCl, + snc, . What is the indicator used and write its formula? Potassium ferricyanide, (K3Fe(CN).) is used as an extemal indicator, 7. Why the indicator K3[Fe(CN)s] cannot be used as an intemal indicat ” Potassium ferricyanide cannot be used as an internal indicator tie aera. Pecause possum ferricyanide combines ireversbly with ferrous ies fe deep blue fore fericyanide complex (Tumbul’s blue). These ferrous ions involern in complex formation are not available for reaction with potassium dichromate, Marcon the end point cannot be detected, as there is no colour change. % ee 3Fe" + 2K3 (Fe(CN)s) > Fex(Fe(CN),)p + 6K" 8. Why is color of the indicator drop remains same at the end point? ENGINEERING CHEMISTRY LAB (I8CHEL 16726) PAGE 38 1/11 SEMESTER