10 Project–B 1. Purification and Characteristics of Chemical Substances 3.1 To determine the melting point of organic substance. 3.2 To determine the boiling point of organic substance. 3.3 To obtain Pure Substances by Crystallization Process. (Alum, Copper Sulphate, Benzoic acid) 11 3.1 Determination of the Melting Point of Oragnic Substances Melting Point : The specific temperature of any solid substance at which it melts completly is called its melting point. The pure organic compound always melt at specific temperature, it can be test by its melting point. The melting point becomes less by the presence of impurities. 4. Now place the close end of capillary on table and slowly strike capillary tube or slowly by pen, coin etc. So that the powder comes lower to the close end. Repeat the above procedure 3-4 times so that the capillary tube is filled with powder upto 3-4 mm in height and there Capillary tube fine powdar plate to push to strike Fig 3.1 (A) To close the mouth of capillery tube. (C) (R) Objective : To determine the melting point of organic substance. (acetamide). Apparatus : Beaker or Round bottom flask, tripod stand, thermometer, spirit lamp or bunsen burner, capillary tube, conc. H 2SO4 etc. Procedure : (A) To, fill the capillary tube with given substance : 1. Generally the melting point can be determined with the help of capillary tube. For this take a capillary tube of 5-6 cm long and of about 1mm of diameter. Close one end of the capillary tube by melting it over the flame of burner. 2. 3. Take the some organic compound an a plat and make a powdered substance by grinding. To fill this powder into capillary, push this powder in it, So that some powder will enter into the capillary. will be no portion remain empty (no air is present). (B) To find the melting point of substance: Thermometer Capillary tube burner Fig 3.2 To find the melting point. 12 1. Adjust the apparatus according to the Result : The melting point of given figure. 3:2 Fill the 1/2 of beaker or Round substance is 80°C. bottom flask with water and put it on the Procedure : 1. The open end of capillary tube should tripod stand. be placed on the upper side of liquid of Note : When you have to find the melting point beaker. of the organic substance which is having 2. Take the liquid of that quantity which lower than 1000C melting point then take is sufficient to deep the bulb of the water into beaker, but for the substance thermometer and the bottom end of the of having melting point more than 100°C capillary. If you take more water then it take oil or conc. H 2SO4 in beaker. 2. will take more heat to heat it. Wet the capillary tube with the liquid of 3. Stir the liquid of beaker continuously, beaker and attached it with thermometer in But after 60° – 65° C or before the such a way that the solid substance of close melting point of the substance, repeat end of capillary always remains near to the the stirring process. bulb of thermometer. Tie the capillary tube Table : Find the melting point of some organic substance Substance Phenol Benzophenol Nephthol Melting point in 0C. 42.0 46.0 54.0 Substance Acetamide Oxalic acid Benzoic Melting point in 0C. 82.0 101.0 122.4 Nephthelein 80.0 Urea 132.0 with the thermometer by the thread. 3. 4. 4. The liquid of the beaker should be Burn the beaker slowly in uniform way by Gansparant and heat the substance upto the burner and stirr the liquid. melting point slowly. Now note temperature at which the solid 5. If the solid substance is attached to the substance of capillary tube becomes in the outside wall of capillary tube then form of transparent liquid after melting. This remove it with the help of filter paper. is the melting point of solid. 6. Place the thermometer vertically into the Observation : The given substance is beaker and place the eye at the point of completely melts at t°C (80°). mercury, while taking the reading. 3.2 Determination of Boiling Point of Organic Boiling Point : When the liquid in heated its temp is known as the boiling point of liquid than its vapour slowly increases and after than there will be a pressure will be equal to the atmospheric pressure. stage when the whole water will boil than the temperature remains constant. This temperature 13 [A] Boiling point tube method : Objective : To determine the boiling point of the given organic substance (acetic acid). Apparatus : Boiling tube of having two holes, thermometer, burner, organic liquid whose boiling point has to be determined, the pieces of porcelein, tripod stand, sand bath. Procedure : 1 When the liquid is present in large quantity, take a boiling tube of hard glass. Take a organic liquid of about 20-25 ml into it whose boiling point has to determined. 2. Pour some 3-4 pieces of porcelein into the liquid of the tube so that the liquid should not bump during burning. 3. Place one of the thermometer into the hole of flask and fix the discharging tube into the other hole and fit the cork on the boiling tube. 4. Fix the boiling tube into the clamp of the stand according to figure, place the bulb of the thermometer at 1 cm high from the liquid. Now to heat the boiling tube, heat the sand bath by burner. 5. See the level of mercury of the thermometer of testtube. The temperature of thermometer increases slowly. After sometime the liquid of the boiling tube starts boiling and liquid Vapour comes out from the discharge tube. At that stage, temperature of thermometer becomes constant. Note down the reading. This will be the boiling point of liquid. Observation : The boiling point of given liquid (acetic acid) is 110°C Precautions : according to the experiment 3.1 (B) Capillary tube Method : Objective : To determine the boiling point of organic liquid by capillary tube method. Apparatus : Beaker, burning tube, small boiling tube, Capillary tube, tripod stand, Stirrer, water, oil of conc. H 2SO 4 if you want to heat more than or ignition stirrer, stand, burner wire gauze 100°C. Procedure : 1. When the quantity of liquid is very less than use above method. Take burning Thermometer vapour of liquid boiling hide liquid Sand bath Fig 3.3 To find the boiling pt. of liquid. 2. 3. tube or small boiling tube and fill it with 2ml. organic liquid. Tie the burning tube with the thermometer by thread or rubber ring. Place the beaker on net wire of tripod stand after filling it 1/2 with the oil conc H 2SO4 according to the figure and put the thermometer in perpendicular form with the help of clamp of stand. Thermometer stirrer Capillary tube liquid Bubbles Substance Fig 3.4 To find the boiling point with the help of capillary tube method 14 4. The capillary tube of about 6cm long whose bottom edge is placed on the burning tube. Now heat the liquid slowly and stirrer the liquid carefully. When the bubbles from the bottom edge of capillary coms out then note the temperature of thermometer. It is the boiling point of liquid. Observation : The reading of thermometer is t°C. Result : The boiling point of given organic substance in t°C. Precaution : 1. The thermometer should be placed perpendicular in the beaker. 2. Burning tube should be placed with the thermometer and the thread is kept on the liquid of beaker. 3. Stir the liquid of beaker with the help of stirrer. 4. If the temperature of given organic liquid is less than 100°C than take the water into the beaker. 5. 3.3 To Obtain Pure Substance by Crystallization Process Crystallization : When you cool the hot and saturated solution of substance,it crystalizes, this process is called crystallization. Process of making crystal : There are following terms include in the process of crystallization. 1. To prepare solution : Take some distilled water in beaker put some impure substance in it gradually and continously stir it with the help of glass rod. Try to dissolve the solid by heating the beaker slowly. When some solid is left at the bottom then stop stirring and put some solid in it. 2. glass rod Solution Wire gauze Filtering : Filter the obtain solution and Fig 3.6 To heat the solution. glass rod beaker solution Fig 3.5 Mixing with glass rod. transfer it into the cup of porcelein with the help of filter paper . Fold the filter paper and fit it into the funnel. Take a circular part of filter paper and fold it from the bottom. 15 according to the figure. Open the folded Paper in such a way that 3 largers are in one side and one large is on the other side. In this situation the funnel shape is same as the cone. Put it into the funnel and pour some drops of water in it and mix it. So that the filter paper stick with the wall of the funnel. Now in this way the filtering process is completed. 3. Concentration of saturated solution upto Crystallization point : Now heat this cup by putting it on the sand bath. After every minute take some solution on the glass rod, blow on it or move it in the air. When layers of solid are forms on the glasses rod, stop to heat it. The solution is concentrated , upto the crystallization point. Now put the cup open in the air or put it on the beaker that filled with cold water. So that the solution becomes cold. Filterate Fig 3.7 To fold the filter paper and keeping the funnel. Filtering process in shown with the help of filter paper and funnel and the transformation of solution into the cup of funnel shaped as shown in the figure. To evaporate the solution. Soild residue air blowing To make the layer solid Fig 3.9 To test the crystallisation. Funnel 4. Porceline bowl funnel end filterate Fig 3.8 To filter the solution and transfor. To purify the mother solution and dry the crystals : When the crystallization is completed then carefully purify the mother solution and press, the crystals between the pieces of filter paper to dry it. 16 filter paper Crystals crystal mother solution Cold water Experiment – 1 Objective : To determine the pure substance (CuSO4 ) from the impure sample with the help of crystallization Principle : Filter the impure CuSO4 solution in presence of dilute sulphuric acid and dissolve less quantity of water in it. Now Vapourise the solution upto crystallization point. After cooling the solution, blue crystal of CuSO 4 .5H2O are separated out. 4. When the crystallization is complete then remove the mother solution by decantation. Carefully wash the crystals of CuSO4 into the alcohol. Dry the crystals by pressing them between filter paper. 5. Measure the dry and pure crystals of copper sulphate Result : Apparatus : Beaker, China dish, rod, funnel, sand bath. 1. found Crystals = gm 2. Colour = Substance : Impure copper sulphate. 3. Shape = Method – 1. Grind the impure CuSO 4 properly. Take 6-7 gm impure CuSO4 into the beaker and add less quantity of water in it. Add some drops of dilute H2SO 4 into the solution so that the hydrolysis of CuSO 4 is not possible, filter the solution and take it on the china dish. 2. 3. Blue Precaution : 1. Wash the impure CuSO4 in the presence of less quantity of water. 2. Don’t heat the solution for a long time otherwise you will get a different substance in place of crystal. 3. Put the china dish on the sand bath and start to heat it. Stop heating till we get the crystallization point. Use dilute H 2SO4 during preparation of CuSO 4 solution otherwise there is possibility of hydrolysis of CuSO 4 . 4. Now put the china dish on the beaker for cooling it. After sometime the crystals are formed. Slowly cool the conc. solution so that the big crystal will form. If you cool it then the crystal will become very small. 5. Put the crystal between the filter paper. 17 Experiment – 2 Objective : To obtain the pure substance by impure sample of alum with the help of crystallization method. Principle : Filter the impure sample of alum in presence of dilute sulphuric acid and dissolve less quantity of water in it. Now vapourize the solution upto the crystallization point. After cooling the solution, the crystals of pure sample are separated. Apparatus : Beaker, China dish, glass rod, funnel, sand bath, filter paper, impure sample of alum. Method – 1. Grind the impure alum properly, take 67 gm. impure alum in the beaker and dissolved in less quantity of water and. Add some drops of dilute H 2SO4 in the solution so that the water reduction of alum is not possible, filter the solution 2. 3. 4. 5. and take it into the china dish. Put the china dish on the sand bath and start to heat it ,stop heating when you get the crystallization point. Now put the china dish on the beaker full of water and cool it. After sometime the crystal are formed. When the crystallization is completed than filter the mother solution to remove it carefully wash the crystals of alum into the alcohal, dry the crystals by pressing them between filter paper. Measure the dry and pure crystals of alum. Result : 1. Crystals found .................gm 2. Colour = Colourless............... 3. Shape = octahedral .......................... Precaution : ● Wash the impure alum in the presence of less quantity of water. ● Don’t heat the solution for a long time otherwise you will get a specific substance in stead of crystal.. ● Use dilute H 2SO4 during preparation of solution of alum. otherwise there is possibility of water reduction of alum. ● Slowly cool the conc. solution so that the big crystal formed. ● Put the crystal between the filter paper for pressing. Practice exercise Q.1 Describe the melting point of a substance? Q.2 What is the importance of melting point of a substance? Q.3 What is the effect of impurities on melting point of any substance? Q.4 To know the melting point of any substance, how do we select the medium of heating? Q.5 To while determining the melting point of any substance, Why upper and of the capillary tube is kept on the substance? 18 Q.6 Define the boiling point of liquid? Q.7 What is the definition of boiling point? Q.8 What is the difference between melting point and freezing point of substance? Q.9 What is the reason to cut the pieces of porcelin , during the determination of boiling point? Q.10 How does the boiling point of liquid change by external pressure? Q.11 When the capillary tube is used during the determination of boiling point of liquid? Q.12 What is a crystal ? Q.13 Why oil or sulphuric acid is added in impure copper sulphate during the process of Crystallization? Q.14 What do you mean by saturated solution? Q.15 What do you understand by crysallisation point? Q.16 Write down the formula of potash alum? Q.17 What is the shape of crystal of alum? Q.18 Explain crystal water? (water of crystallization)
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