1 PU Lab Manual LABORATORY DISCIPLINE |. The duly completed record should be submitted, once in every week. 2. Description of the experiment should be written on the right hand page and observations, diagrams and calculations on the left hand page of the record. Each experiment should always be commenced on a fresh page Experiment number and date should be written at the left hand page The apparatus issued should be returned in a good condition. - Students will be held responsible for any loss or damage of the apparatus | The students should pay in full the cost of apparatus broken or Tost. 6. 1 8. Keep the working table clean and neat. 9 . Used filter paper should be thrown in the dustbin and not in the wash basin. 10. Before leaving the laboratory, gas and water taps should be closed tightly 11. Use the chemicals, water and gas very economically, 12, The bench reagents should not be displaced from their proper places and they should never be placed on the working table. 13. Never attempt to taste the chemicals. 14, Try to avoid smelling gases or vapours as far as possible, 15. All accidents should be reported immediately to the staff member in charge for necessary first aid. 16.To light the bumer, use only spirit lamp or lighter. 17 Handle organic chemicals very carefully (while heating) as they are highly inflammable. 18, Exercise caution while handling concentrated acids as they are “corrosive”. 19, Do not spoil or erase the labels pasted on the reagent bottles. 20, Do not intermix the reagents; explosion may take place. 21. The rules should be strictly obeyed. 22, Students disobeying the instructions will be viewed seriously. 23. Get the records certified before the preparatory examination.| Air hole: | | N xe Dy [o] ir Regulator SS _— AT) — Side Tube CY | = Base — | Bunsen burner mrcton : Aer Region | liddle Region \ | Inner Region eee Small Blue Region ark Region t Luminous Flame Non Luminous Blue fame Zones of flame of Bunsen burner 2 Vilaya Pre-University College, Tu!Experiment No.1 (A) STUDY OF BUNSEN BURNER ‘Aim: To study various parts of Bunsen burner and the Bunsen flame. Bunsen burner: It is commonly used in the chemistry lab for heating purposes. Its different parts are dismantled and studied, It consists of three parts namely metal base, Burner tube and air regulator. Metal Base: This is provided with side tube and a nozzle from which gas enters the burner tube. Metal base keeps the burner in a stable upright position. Burner Tube: It is cylindrical metallic tube which is provided with two air holes at its lower end. Through these holes air can be admitted into the tube. Air Regulator: It is short metal ring with two holes. It is loosely fitted at the lower end of the burner tube. By rotating the air regulator. air holes could be closed fully or partially. By doing so the supply of air can be regulated. To study how burner works, the three parts are reassembled and connected to the gas tap by means of rubber tubing. Lighting of Bunsen burner: The air holes are closed completely, the gas tap is opened and the burner is lighted. A smoky, yellowish flame is obtained called Luminous flame. This Luminous flame consists of four regions. ‘A small blue region at the base of the flame. . A dark inner region of non combustion containing unburnt gases. . A luminous middle region of incomplete combustion. A pale blue outer region of complete combustion. ‘A luminous flame is made Non-luminous by slowly turning the air regulator until a non- smoky bluish flame is obtained. A Non-luminous flame contains three regions. |. A dark inner region of non combustion containing unburnt gases. 2. A middle region of incomplete combustion. 3. A pale blue outer region of complete combustion. Some simple experiments are carried out with the Bunsen flame and the conclusions are made as follows: 1. ‘The outer region of the Bunsen flame is hotter than the middle region 2. ‘Tip is the hottest part of the flame and should be used for general heating purpose Vijaya Pre-University College, Tumkur 5ee — PU Lab Manuat | —I (B) BASIC LABORATORY TECHNIQUES Aim: To study some of the basic laboratory techniques like cutting glass tube, bending a glass | tube, drawing a glass jet, boring a cork, filtration ete. Glass work: The laboratory apparatus for carrying out reactions, in general is made up of Blass. It is because glass is resistant to the action of most of the chemicals, Generally two types are used for making apparatus for laboratory work. These are soda lime glass and borosilicate glass. Soda lime glass softens readily at about 300- 400° in the burner flame. (For glass work, glass tubes made of soda lime are taken.) |. Cutting and fire polishing of glass tubes: A deep soraich is made on the glass tube Wherever a cut is needed using a triangular file. Its held in both hands in such a way that the points ofthe thumbs are together on either side ofthe scratch. Now the tube is pressed ‘ih the thumbs and pulled with fingers. The tube breaks at the scratch with a sharp edge. The cut ends of the tube must be rounded off or smoothened by fire polishing, The end of the tube is heated in a Bunsen flame. The tube is continuously rotated for uniform heating. ‘The heating is stopped when the edges melt and becomes soft. * Bending a glass tube: The glass tube is held lengthwise in the flame with both hands and heated gently by waving in the blue flame of fish tail burner. Keep the tube rotating in the flame for uniform heating. When the tube becomes hot and soft, take it out of the flame and is bent to the desired angle. - Drawing out the glass tube to form a jet tip: The glass tube is held lengthwise ‘in the flame with both the hands. The tube is rotated about its own axis for uniform heating. When the glass is softened, the tube is removed from the flame and its ends are pulled out quickly and carefully. The narrowed portion of the tube may be at its middle point. From this we can get capillary and jet tips. Vijaya Pre-Universiy College, TumutScratch mark Koop rotating the glass tube Breaking the glass Fire polishing Hotend edb Heating Bending the glass tube Remove the tubing from the flame and after a moment pull the ends apart to get the narrow capillary in the middle. Cut to length and fire-polish the two ends of droppers. Drawing a jet. Jets obtained after cutting and fire polishing Vijaya Pre-University College, Tumkur 5—— |PULab Meng | Experiment No.2 PURIFICATION OF COMPOUNDS, AIM: Puritication of compound prepared by erystallization, THEORY: The compounds prepared are usually impure or erude .In order to remove the impurities in * Compound crystallization is one of the methods for purification. This is done by preparing saturated solution of the compound using a suitable solvent. This solution on cooling gives Pure crystals. PROCEDURE '. A saturated solution of benzoic acid is. prepared by using hot water, (dissolve the compound until it stops dissolving to get a saturated solution) 2. Filter and transfer the Saturated solution into a china dish, Heat on a sand bath till reduced ‘o quarter of the original quantity - Dip a glass rod in the solution and blow air from the mouth, if solid film deposits stop heating, + Cover the porcelain dish with a watch glass and kee P the content of the dish undisturbed for cooling. When the crystals are formed remove the mother liquor by decantation, 6. Wash the crystals with cold water and filter. ~The procedure is repeated several times to get maximum amount of pure substance. Dry the crystals between the folds of filter paper and store in safe dry place. Vijaya Pre-University College, Tumiut "IPU Lab Manual Experiment No.3 DETERMINATION OF MELTING POINT Definition: The temperature at which solid changes to liquid state is called Melting point. Theory: The kinetic energy of the molecules of a substance increases on heating. At a particular temperature, Lattice structure of solid breaks and thus the solid melts and turn to liguid state. Materials required: Apparatus Chemicals 1, Thiele’s tube 1. Liquid paraffin 2. ‘Thermometer 2. Organic compound 3. Capillary tubes 4. Iron stand with clamp PROCEDURE: 1. Take a capillary tube of approximately 8 cm in a length, seal its one end by heating. 2. Organic compound whose Melting point has to be determined is taken in a capillary tube and tied to thermometer in such a way that base of capillary tube and bulb of thermometer are at same level. 3. Apparatus are arranged as shown in the figure. 4. The Thiele’s tube is heated and the temperature at which the solid starts melting is noted. REPORT: The Melting point of given organic compound is found to be ||. thermometer Capillary tube - Solid Liquid paraffin Vijaya Pre-University College, Tumkur 7Experiment Nod ii) DETERMINATION OF BOILING POINT - of the becomes equal to Definition: The temperature at which the vapour pressure of the liquid bee qual tc atmospheric pressure is called Boiling point Materials requi Chemicals Apparatus Organic liquid 1. Thiele’s tube Liquid paraftin. 2. Thermometer Iron stand with clamp Ignition tube (fusion tube) Capillary tube. PROCEDURE: | |-2 drops of Organic liquid is taken in an ignition tube, a capillary tube whose one end 's sealed is inverted and placed in a fusion tube. Apparatus are arranged as shown in the figure. On heating the Thiele’s tube, at a particular temperature, bubbles start coming out briskly and continuously. This temperature is the boiling point of liquid. REPORT: 1. Boiling point of given Organic liquid is 3% Correctior Actual Boiling point = observed B.P + correction Term= _ Thermometer Capillary Substance Ignition tube ia ety gs To : aeExperiment No. 5 PREPARATION OF STANDARD OXALIC ACID SOLUTION AND DETERMINATION OF CONCENTRATION(STRENGTH) OF SODIUM HYDROXIDE USING STANDARD OXALIC ACID SOLUTION A. Preparation of Standard Oxalic acid solution Theory: Oxalic acid is primary standard. Its molecular formula is (COOH).2H20 and molecular mass is 126. If 126g of oxalic acid is present in | liter of solution, it is known as one Molar (1M) solution. For the preparation of 1 liter of 0.1 M oxalic acid solution, 126/10 = 12.6 g of hydrated oxalic acid is required. Therefore for preparing 250 mL. of oxalic acid solution. (12.6g x 250mL)/1000mL = 3.1500g of hydrated oxalic is required Note: Molarity of the solution can be calculated using the formula: Mass of solute x 1000 Molarity = — S00 —______ Gram molecular mass of solutex Volume of solution Procedure: Weigh empty. clean and dry weighing tube (W,) accurately. Place about 3.15002 of a oxalic acid in weighing tube and weigh again (W.). Transfer the oxalic acid crystals into the beaker and dissolve it completely by adding about SOmL of distilled water. Transfer this solution into 250ml. volumetric flask using funnel and glass rod wash the interior of the beaker with distilled water and add the washings to the volumetric flask. Remove the funnel after washing with distilled water. Make up the volume in the volumetric flask to the etched mark. Stopper the flask and shake well for uniform concentration. Calculate the exact molarity of the solution from the amount of oxalic acid dissolved. Result: The molarity of oxalic acid solution prepared = Observation and Calculation: _ Weight of empty weighing tube (W,) = . Weight of empty weighing tube + oxalic acid (W2) Weight of oxalic acid crystals (W> ~ W,) = The molarity of the solution prepared = (W> ~ W,) x 7 - ~ Viaya Pre-University College, Tumkur10 B. Determination of concentration of given sodium hydroxide solution by using standarg oxalic acid solution Apparatus required: pipette, Burette, conical flask Chemicals required: NaOH, H,C,0,, phenolphthalein indicator et. Principle: A known volume of oxalic acid solution is titrated against sodium hydroxide solution by using phenolphthalein as an indicator. Sodium hydroxide is a mono acidic base and oxalic acid is a dibasic acid, The neutralization reaction takes place to form salt and water, 2NaOH + C3H,0, —> NajC,0, + 2H,0 Procedure: A burette is washed with water, rinsed and filled with the given sodium hydroxide Solution. Care is taken to see that there are no air bubbles in the nozzle of the burette. The initial burette reading which corresponds to lower meniscus of the liquid is noted A pipette is washed with water rinsed with given oxalie acid solution and exactly 25mL of the same solution pipette out into clean conical flask. Two drops of phenolphthalein indicator is added the colourless solution is titrated against the sodium hydroxide solution, taken in the bureite by adding in small quantities at a time after each addition mixture is shaken well, The addition of NaOH is stopped when the colourless solution tums pale pink. The final reading of the burette is noted. The titration is repeated to get concordant values. Observations: I. Solution in Burette : NaOH solution Solution in conical flask: 25mL of 0.1 M oxalic acid. . Indicator: Phenolphthalein point: Colourless to pale pink. Tabular column: Trial No. Final burette reading Initial burette reading | Volume of NaOH added in mL | Vilaya Pre-Univesity College, TumkurCalculation: I. Calculation of Molarity: 8, (M.M.)sson = 2 (M2V2Jen.0, Where M; and V; are molarity and volume of NaOH. M, and V; molarity and volume of CoH;0, (@M.Va)eo, ay (acidity of NaOH) Maun ann Mision) = M a» (basicity of oxalic acid) . Concentration (strength) of sodium hydroxide solution in g/L = Molarity x gram molecular mass of NaOH x 402 & Result: 1, Molarity of NaOH solution= 2. Concentration (strength) of NaOH = _ Vijaya Pre-University College, Tumkur "Experiment No. 6 . "ARBONATE PREPARATION OF STANDARD SOLUTION OF SODIUM C HvDROCHLAN DETERMINATION OF CONCENTRATION (STRENGTH) OF Motos ACID USING STANDARD SODIUM CARBONATE SOLU A: Preparation of 0, standard solution of anhydrous sodium carbonate ° te i herefore 10.68 in one Theory: The molecular mass of anhydrous sodium carbonate is 106. Therefore 8 IN one litre gives 0.1M solution. 2.65 in 250 ml gives 0.1M Note: Molarity of the Solution can be calculated using the formula Molarity = __Mass of solutex1000__ Gram molecular mass of solutex Volume of n Procedure: Weigh empty, clean and dry weighing tube (W;) accurately. Place about 2.7¢ of sodium carbonate in weighing tube and weigh again (W,). Transfer the sodium carbonate into the beaker and dissolve it completely by adding about 50mL of distilled water. Transter this Solution into 250mL volumetric flask. Make up the solution exactly to the mark and shake welh for uniform concentration, Result: The molarity of NayCO, solution Prepared= M Observation / Calculation: 1 Weight of empty weighing tube (W,)= _ ~ Weight of empty weighing tube + sodium carbonate (W:) ~ 3. Weight of sodium carbonate (W,-W,)= W,- The molarity of the solution prepared = iu Vijaya Pre-University College, Tun” a1 PU Lab Manual B. Determination of concentration of given Hydrochloric acid solution by using standard Sodium carbonate solution Apparatus required : Pipette, Burette, conical flask Chemicals required : NayCO3, HCI, Methyl orange indicator etc. Principle: A known volume of sodium carbonate solution is titrated against hydrochloric acid solution by using an indicator. Na,COs is a weak base and hydrochloric acid is a strong acid and the neutralization takes place to form salt and water with the liberation of carbon dioxide Na,CO; + 2HC] —> 2NaCl + CO,t + H,0 Procedure: Pipette out exactly 25 mL of sodium carbonate solution into a clean conical flask. Add about two drops of methyl orange indicator. The solution turns yellow. Titrate this solution against hydrochloric acid solution, which is taken in the burette till the yellow colour changes to pinkish red. Note down the burette reading and repeat the titration to get concordant values. Observations : . Solution in Burette: Hydrochloric acid solution | Solution in conical flask: 25ml of 0.1 M sodium carbonate solution . Indicator: 2-3 drops of methyl orange . End point: Yellow to pinkish red Tabular column: Trial No. Final burette reading Initial burette reading Volume of HCI added in mL, Vijaya Pre-University College, TumkurEEE Calculation: I. Calculation of Molarity: ¢ molarity and volume of HC] 8, (M,V cq =42(M,V,), are m Where M, and V) riity and volume of Na,COs N00, Mp and V2 molar ‘a,M.V, Maney = CMa, (ac a, (basicity of HCI) =! M = M a ( acidity of NayCOs) = 2 . Concentration (strength) of HCI solution in g/L. = Molarity x gram molecular mass of HCI = x 36.5 Result: 1. Molarity of HCI solution = M 2. Concentration (strength) of HCI = Vijaya Pre-University College, Tum" ——— TN ee -