CONTENTS INTRODUCTION 1,1 Do's and Don'ts in a Chemistry Laboratory 1.2 Basic Laboratory Equipment's 1.3 Heating Services BASIC LABORATORY TECHNIQUES 2.1 Acquaintance with Analytical Balance (Chemical Balance) PURIFICATION AND CRITERIA OF PURITY 3.1 Purification of sample of potash alum or Copper sulphate and Benzoic acid by crystallization 3.2 Determination of melting point (m.p.) of a solid organic compound 3.3 Determination of boiling point (b.p.) of a liquid organic compound CHEMICAL EQUILIBRIUM. 4.1 To study the shift in equilibrium in the reaction of ferric ions and thiocyanate ions by increasing the concentration of any one these ions 4.2 To study the shift in equilibrium in the reaction between water ligand cobaltion [Co(H,0),]"and chloride CI ions by increasing the concentration of any one of these ions pH & pH CHANGE IN AQUEOUS SOLUTION 5.1 To determine the pH of some fruit juices 5.2 To observe the variation of pH of acid / base on dilution 5.3 To study the variation of pH by common ion effect in case of weak acids and weak bases 5.4 To study the change in pH during the titration of a strong acid with a strong base using universal indicator 5.5:To study the pH of Sodium chloride, Ferric chloride and Sodium carbonate solutions 17 20 21 23 Scanned with CamScannerTITRIMETRIC ANALYSIS 6.1 To determine concentration (strength) of ‘sodium hydroxide solution in terms of gram per litre by titrating against standard (0.1M) oxalic acid solution 6.2 Preparation of standard solution (0.1M) of Sodium carbonate 6.3 To determine the strength of hydrochloric acid in terms of gram per litre by titrating against standard (0.1M) sodium carbonate solution, SYSTEMATIC QUALITATIVE ANALYSIS OF INORGANIC _ SIMPLE SALT 7.1 To detect one cation and one anion in the given salt. 7.2 Model procedure for analysis of simple inorganic salts Viva question for practical examination Scheme of valuation of Ist PUC practical examination 10. List of chemical reagent and preparation of solutions 29 30 32 39 47 51 53 Scanned with CamScanner1. INTRODUCTION Experiment No. 1.1 Do'sand Don'ts ina Chemistry Laboratory lL 2. ‘Wear white coat, shoes & safety glasses while working in the laboratory. Don't touch any chemical with hands and do not taste any;Chemical because some will be corrosive & poisonous. .. Before using any chemical reagent, check & read the label of the reagent bottle carefully. After the use, they are to be stoppered well &replaced to their places. . Don't conduct any experiment with insufficient information. . Avoid using excessive amount of reagents unless itis needed. . Be thorough with the details of experiment & calculations before the start of the any experiment. . Never mix chemicals-unless it is being told to do so otherwise it may lead to serious accidents. . While heating substances in a test tube, see that the open end of the test tube should pointed neither to yourself nor at your neighbour. . Don't smell any gas or chemical directly but smell by wafting them gently towards you. 10. Use concentrated acid in the fuming chamber only. Don't bring them to your place of working on the table. 11. Don't pipette out concentrated acids, bases and phenol solutions. 12. Don't waste water or gas. Close the taps whenever they are not in use. 13. Incase of any mishap, immediately inform the instructor or concerned teacher. 1 Scanned with CamScannerExperiment No. 1.2 Basic LaboratoryEquipment's SL. No. Apparatus Image Uses Test tubes Used to carryout chemical reactions & tests Flasks: a)Conical flask b)Round bottomed flask Used to carryout chemical reactions. Used for conducting titrations. Used for boiling or refluxing the reaction mixture over wire gauze, sand bath or water bath Beakers Used to prepare solutions, solvents to carryout evaporation of precipitation reactions. Condensers Used to condense the vapours into liquid. Water cooled & Air cooled condensers are used for distillation & refluxing. Reagent bottle Used to store chemical solutions Separating funnels Used for the separation of immiscible liquids Measuring cylinders Used to measure the volume of solution Burette Used in titration to add definite volume of solution Scanned with CamScanner~ [Used to draw known 9 | Fipete cesses | /fixcd volume of solution used in titration. Used to separate a solid 10. | Funnels ) from solution during, K Filtration CE) Used for grinding the 1 | Mortar & Pestl ' oS eat Sy chemicals in laboratory 12. | Test tube brushes ir on for cleaning the test ce: . Used to place beaker or 13._ | Wite gauze with conical flask on it during asbestos center heating. 14. | spat Used to transfer chemicals spatula from the containers. Used to keep test tube of 15 | Test tube stand pect . Used for cooling and to LO Oe remove the moisture. a Used to carryout 17 | China dish evaporation of solution. Ss Used to cover the china 18 | Watch glass rim | aio Scanned with CamScannerUsed to place the beaker, china dish etc,, to carry out heating. Are used to carry out 20 ‘| Filter paper filtration and to separate solid from the solution. 19 | Tripod Stand Used to washing the glass 21 | Wash bottle apparatus Used to prepare:standard solutions Standard volumetric 22 flask Experiment No. 1.3 Heating Devices Heating of apparatus in the laboratory is\done by means of spirit lamp, Kerosene Lamp & Gas burner like Bunsen burner. _— Burner tube BUNSEN BURNER tr vent—_| ‘Atr regulator Gas tube ‘Base ‘UDY OF BUNSEN BURNER Parts of Bunsen burner 1. Base: It is a Circular cast iron disc provided with a side tube which acts as inlet for the gas anda nozzle from which gas escapes into the burner tube, Scanned with CamScanner1, Burner Tube: It is a long brass cylindrical tube screwed on the nozzle (or nipple). Near its lower end two air holes are provided for sucking air into the burner tube. 2. Air regulator: This is a metal ring which can be turned around the burner tube to open orclose the air holes thus regulating the entry ofair. Working of Bunsen burner The air holes are closed, gas supply is turned on and the gas is lighted to get a luminous yellow flame. Now the air holes are opened slowly to get a nonluminous blue flame. Types of Bunsen Flame Bunsen burner produce two types of flames namely Luminous flame Nonluminous flame carey) ee 1. It is a yellow coloured long unsteady flame 2. It is produced when air holes are closed 3. Here the gas is partially bunt 4, Relatively it is a low temperature| flame . It is a blue coloured short steady flame It is produced when the air holes are opened . Here the gas is completely burnt . Relatively itis a high temperature flame Ss Scanned with CamScannerParts of Nonluminous Bunsen Flame The nonluminous Bunsen flame consists of three regions 1) A dark inner region of no combustion 2) A greenish middle region of incomplete combustion 3) A faint blue outer region of complete combustion Outer region of complete combustion (Hottest) Middle region of partial combustion (Hot) Inner region of no combustion (Cold) Experiments with Bunsen flame Experiment Observation Inference 1) Introduce a glass tube [Gas bums at the other end | Dark region contains into the inner dark region | with asmall blue flame unburnt gas in slanted position and’ the other end is ignited 2) Splinter test A splinter is’ held across the flame closed to the burner tube & moved up slowly Splinter charred only at the edges touching the flame & charred part widens and finally chars completely. Inner region is cold, middle is hot & outer region is hottest 3)Wire gauze experiment An iron wire mesh is held on the flame closed to the burner tube and moved up A ted hot ring with large gap is formed in the wire gauze. The gap widens & finally vanishes Inner zone is cold, middle is hot & the outer is hottest. slowly. Scanned with CamScanner4) Iron wire experiment | An iron wire is hold over | The wire glows at the two | The tip of the flame ix the flame close to the | points touching the edges | hottest bumer tube and gradually | of the flame. The glowing | | raised. gap enlarges and finally | | | merge together Important precautions for using the Bunsei Check the gas connection for any Icakage of gas. Close the air holes while lighting the Bunsen burner. Open the air regulator slowly to get non-luminous Bunsen flame. No solid substance should be dropped into the burner tube as it blocks the nozzle hole. © Never blow the Bunsen flame to put it off instead it can be put off by stopping the gas supply. © For heating only the tip of the flame must be used because it is hottest flame, 2. Basic laboratory Techniques GLASS WORK Cutting of glass tube & glass rod The glass tube or glass fod to be cut is placed on a piece of asbestos sheet. A deep scratch is made on it using a triangular file. It is held in both the hands such that the points of thumbs are together on either side of the scratch and pressed, so that it breaks up into two pieces the sharp edges are converted into smooth by fire polishing. athe . TA TI as Bending of glass tube The glass tube is held horizontally to the tip of nonluminous Bunsen flame by slowly rotating for uniform heating, When it becomes red hot & sof, itis then removed from the flame and gently bent to desired shape such as U-tube, V-tube & L-shaped tube ete., q Scanned with CamScannerExperiment No. 2.1 Acquaintance with Analytical Balance (Chemical Balance) Achemical balance is used to measure the mass of a substance accurately up to 4 decimal places. It consists of the following parts. @ Base: Base of balance rests on two leveling screws in the front and a Peg at the back. A metallic hollow pillar is fixed at right angle to the base of balance, A metallic rod to the top of which an agate plane is fixed is moving inside the hollow Pillar, Itcan be raised or lower by means ofa knob fitted at the bottom of | balance, @ Metal Scale: A graduated metallic beam with three knife edges and toothed top Surface rests on the agate plane over central knife edge. A pointer fixed Perpendicular to the beam normally oscillates over ivory scale fixed at the bottom of the pillar. Two scale pans are suspended to the metal scale over terminal small knife edges by stirrups containing the agate planes. Two adjusting screws provided at the end of the metallic beam are used to set the pointer to the zero of ivory scale. Aplumb line tied by thread point towards'the vertex point fixed at the foot of the pillar to check the planarity of base of balance & perpendicularity of the pillar. A movable rod called rider carrier can be operated from outside which will help us to place the rider over the toothed surface of balance beam. The whole setup is enclosed ina glass case to guard against the entry of air & dust inside, Note : Chemical balance diagram refer front cover page. Weight box: The weight box ofchemical balance contains © Brass weights coated with nickel for weighing in grams 100, 50,20,20,10, 5,2,2, © Weights for weighing in milligrams 500, 200, 200, 100,50, 20,20, 1 © Rider: Abent aluminum wire weighs about 10mg or 0.01 gm. 10 Scanned with CamScannerPrecautions: © Object to be weighed is kept in left hand side scale pan & weight in right hand side scale pan, @ Weights are always transferred by forceps only. © Hotobjects should not be weighed as they produce expansion of metal scale pans. @ Balance beam should be raised or lowered very gently. @ During weighing, the doors of balance are to be always kept closed: © _ Rider should be always used for fine adjustment and should not be left over on the beam after the use 7 © Add the mass of rider to the net mass if used to right hand side and subtract ifused to lefthand side of the metallic beam. . Calculation of mass of object Massoftheobject = m+rx0.0002 Br he ng m = massonthescale pan r= riderreading Leastcount=0.002g = mass ofrider on small division Mass of rider= 10 mg=0.01 g The mass of rideris spread over 50 small division a Scanned with CamScanner3. PURIFICATION AND CRITERIA OF PURITY Experiment No. 3.1 Aim: Purification of sample of potash alum or Copper sulphate and Benzoic acid by crystallization. Theory:Crystallization is one of the techniques for the purification of an impure compound (Crude material). It involves choosing a single or mixture of solvents, which dissolve the crude material readily when hot saturated solution is obtained. Insoluble impurities are removed by filtering hot solution then cooled slowly to get pure solute crystals, Materials Required:Potash alum or Copper sulphate and Benzoic acid, 250 mL beaker, Glassfunnel, Tripod Stand, Porcelain dish, Glass tod, Sand bath. Procedure: A saturated solution of Potash alum or Copper sulphate in distilled water (50 mL) is Prepared at room temperature. This solution is filtered and the filtrate is taken into a porcelain dish. The dish is heated ona sand bath till nearly 3/4” of the solvent is evaporated. The porcelain dish is covered with watch glass then allowed to cool, when the crystals are formed, the mother liquor is removed by decantation. The crystals are washed with small quantity of alcohol repeatedly and the obtained crystals are dried between the folds of filter paper. Purification of Benzoic acid (using hot distilled water) Similar procedure is followed up to decantation and the Benzoic acid crystals are washed with cold water and dried between the folds of filter paper. Note: Donotuse alcohol to wash benzoic acid crystals because it is soluble. 12 Scanned with CamScannerExperiment No. 3.2 Aim: Determination of melting point (m.p.) of a solid organic compound. Theory: When a substance is heated, Kinetic energy of its molecules increases, the lattice structure of the solid breaks, melts and changes into liquid state. Melting point of a substance is the temperature at which solid state of a substance begins to change into liquid state, when the pressure is one atmosphere. Materials required: Thicle's tube, Thermometer, Capillary tube, Liquid Paraffin, Organic Compound (Naphthalene) |—Thermemeter AY bee Z|« @ Acapillary tube of approximately 8cm in length is taken and one end of the tube is sealed by heating in a Bunsen flame. Procedure: © Fine particles of given organic substance is filled in the capillary tube by dipping the open end into the powder and gently tapped the upper end, so that solid particles are tightly packed in the tube upto nearly cm length. © Thecapillary tube and the thermometer are tied with a thread, so that both the lower ends are at the same level. The thermometer is fitted into a rubber cork which has a groove on its side for the escape of air and vapours. @ About 50 to 60 mL of liquid paraffin is filled into a Thiele's tube, so that it crossed the bent portion of the tube. Thermometer along with capillary tube is 13 Scanned with CamScanner| ich a way that the thermometer bulb and the substance ompletely dipped in the liquid paraffin dipped in liquid paraffin in filled portion of the capillary i © Now the side arm of the Thiele's tube is heated with a low flame and temperature jg noted when the solid starts melting, This temperature is the melting point Of the solid. Result: The melting pointof the given solid organic compounds... Experiment No, 3.3 Aim:Determination of boiling point (b.p.) ofa liquid organic compound. Theory: The boiling point ofa liquid is the temperaturé at which vapour pressure becomes equal to the atmospheric pressure, which the surface ofthe liquid experiences, Materials Required: Thiele's tube (or Kjeldaht's flask), Thermometer (110°C or 360°C), Capillary tube, liquid paraffin and organic liquid. Seale end, Cepllary tube Open end Procedure: © The Thiele's tube is filled with liquid paraffin so that it crosses the bent portion of | the Thiele's tube. One or two drops the given organic liquid is taken in an ignition tube. 14 Scanned with CamScanner© —Theignition tube is tied to the thermometer using a rubber band or a thread such that both the lower ends are at the same level. A capillary tube of approximately 8cm length is taken and sealed at one end by heating ina Bunsen flame. The open end of the capillary tube is dipped in the liquid, present in the ignition tube, ° Now side arm of the Thiele's tube is heated with a low flame until brisk and continuous bubbles start coming out of the capillary tube. The temperature is noted. nC; Result: The boiling point of the given organic compounds ... 4. CHEMICAL EQUILIBRIUM Experiment No. 4.1 Aim: To study the shift in equilibrium in the reaction of ferric ions and thiocyanate ions by increasing the concentration of any one of these ions. Materials Required: Beakers (250 mL), Boiling tubes (5), Burettes (4), Measuring cylinder (100 mL), Ferric chloride, Potassium thiocyanate, Test tube stand. Theory: The equilibrium reaction between ferric chloride and potassium thiocyanate is studied through the change in the intensity of colour of the solution. Fe™ + SCN (qq) === [Fe(SCN)}*aa) Blood red colour The equilibrium constant for the above reaction is written as [Fe(SCN)}*aq) [Fe**] (aq) [SCNTaqy K, is equilibrium constant at constant temperature. Increase in concentration of Ferric (Fe”) ion or thiocyanate (SCN) ion would result in, increase in the concentration of [Fe(SCN)]" ions. In order to keep K, constant, there is a shift in equilibrium in the forward direction, Hence blood red colour intensity of [Fe(SCN)]" increases. 15 Scanned with CamScanner5. pH &pH CHANGE IN AQUEOUS SOLUTION Principle: Water ionizes to a very less extent into H’ and OH ions and equilibrium exist between water molecule and its ions as follows. HO === H+ ON But H" ion exist in the form of H;0*(hydronium ion), the above equilibrium ig written as 2H20 (aq) H30"(aq) + OH ag) Dissociation constant for water is K,, it is expressed as 2 (H30"}aq) [OH"]as Ky = Ke [H20}"(aq) ee THLOF (ag oe Ky 1H30" aq) [OHToaq) Where K,, is ionic product of water and its value is 1 X 10"“mol? dm at 298K In neutral water, [H30*] = [OH] = 107 mol dm? Concentration of these ions can be expressed in the form of pH and pOH as follows pH =-logio[H30*] and pOH =- log)o[OH'] If pH is less than 7, the solution is acidic, if it is more than 7 it is basic and if it is equal to 7, then it is neutral. Experiment No. 5.1 Aim: To determine the pH of some fruit juices. Theory: Fruit juice shows different colours at different pH values. It is due to their structural change, For a universal indicator colour changes with the change of pH value, from a wide range of pH from 1 to 14. : 20 Scanned with CamScannerMaterials required: 100 mL Beakers (4), Test tubes (4), Measuring cylinder, pH universal indicator chart, pH universal indicator solution, fruit juices of lemon, orange, apple and pineapple. Procedure @ —100mL cach of lemon, orange, apple and pineapple juices are prepared in separate beakers. 2 mL each of these juices are mixed with drops of universal indicator in four separate test tubes and shaken well. f © The colour of the juice solutions are matched with the matching colour of standard pH chart. @ — Theabove observation are recorded and arranged them in the increasing order of pH value. Name of Juice |. colonel Acidic/Basic iniversal indicator Pineapple Result: Increasing order of pH value of juices is... Experiment No: 5.2 Aim: To observe the variation of pH of acid/ base on dilution. Theory: Concentration of hydrogen ion decreases on dilution. Hence pH of the solution increases. Materials required:Test tubes (Big size),Measuring cylinder, 0.1M HCl, 0.1M H,SO,, 0.1M NaOHsolution, Universal indicator. 21 Scanned with CamScanner | |Procedure: @ = 2mLof0.1 M HClis taken ina“A” labelled test tube. © = 2mLof0.1 MHCI+18mL of water are taken in “B’ labelled test tube, © = SmLof“B”+20 mL of H,O are taken in““C” labelled test tube. © SmLof*C”+20 mL of H,O are taken in“D” labelled test tube. © 2ml ofeach A, B, Cand D test tube solutions are taken in separate test tubes and shaken well with 2, drops of universal indicator. © = The colour of the solutions are compared with the matching colour of standard pH chart & pH of these solutions are noted & recorded in the following table. © The above procedure is repeated by taking 0,1MH,SO, and 0,1MNaOH Test HCI H,SO, NaOH Tube Colour | pH Colour pH Colour pH A B Cc D Result: © ForHCl solution pH .on dilution. © ForH,SO,olutionpH... «+. ondilution, @ ForNaOH solution pH on dilution 22 , = a ee Scanned with CamScanner