(iit) FIRST YEAR EXPERIMENTS DEMONSTKATUN EXPEKI MENTS ___INTRODUCTION TO BASIC LABORATORY. TECHNIQUES $a rr ————_ COMMON LABORATORY APPARATUS Wash Bottle: Wash bottle is a.convenient container for water in the laboratories, It is used for (1) adding small quantities of water (2) for adding water dropwise and (3) for washing precipitates. Wash bottles are of two types: (a) Glass wash bottle: It consists of a flat bottomed flask fitted with a two- holed cork. Through the holes two bent tubes are inserted; one short and the other long. The longer tube is connected to a small jet tube through a rubber tubing. The other end of this tube reaches almost the bottom of the flask. ‘ (6) Polythene wash bottle: It is a polythene bottle with an airtight stopper through which a bent tube is introduced. After filling with water if we press on its sides, water comes out through the bent tube. The bent tube may be connected to a jet tube to get water in the form of a jet. The Standard Flask (Volumetric Flask): This is a flat-bottomed flask with a long narrow neck, provided with a ground glass stopper. The long neck has a mark around it. The capacity of the flask upto this mark is written on the bulb. There are standard flasks of different capacities. Standard flasks are used for preparing standard solutions (solutions of known concentrations) and for making up solutions to a definite volume. . Cylinder: ‘Measuring cylinder is a graduated cylinder made of thick glass with a spout at the top. (Polythene measuring cylinders are also available), It is graduated from bottom to top. The topmost mark indicates the maximum capacity of the cylinder. Measuring cylinders of various capacities = eer A eemuring cylinder is generally used for measurements oft Te Fig 1(a) Glass wash bottle Fig 1(b) Polythene wash bottle Fig.2: Standard MeL Fig. 3: Measurin, 1g cylindertransfer a definite volume of a liquid from one vessel to’another. It consists of a long glass tube with an elongated bulb in the middle, ending in a jet at one end. The upper end has @ mark around it. The capacity of the pipette is marked on the bulb. Pipettes of different capacities are available. Burette: It is a long graduated glass tube with a stop cock and a nozzle at one end. It is graduated in millilitres starting from zero at the top. Each mL is further divided into 10 equal divisions so that each division corresponds to 0.1 mL. Burettes are usually of 50 mL capacity. (vi) Conical flask: It is a special type of flask of convenient size used for carrying out titrations. It has a wide neck, large belly and flat bottom. The wide neck permits the direct fall of the liquid from the burette even when the flask is shaken lightly during titration. The big belly avoids the risk of liquid going up along the sides while shaken. Conical flask of 250 mL capacity is generally used in titrations. Conical flasks are also called titration flasks. The conical flask can be heated if desired. (vii) Test tube: It is a hollow cylindrical vessel of thin glass with one end closed. It is made of special glass which can withstand sudden alterations of temperature. Test tubes are used to carry out general chemical tests. There are test tubes of different sizes. The most common size is 15 cm long and 1.5 cm in diameter. {viii) Beaker: Beaker is a wide mouthed hollow cylindrical glass vessel having a flat bottom. (Beakers made of polythene are also available). There are beakers of different sizes. Beakers are generally used to prepare solutions and to heat liquid. (iv) Pipette: A pipette is used to (i) The Bunsen Burner: Bunsen burner is the commonly used device for providing heat in a chemical laboratory. In most of the laboratories, LPG is used as fuel. The bunsen burner consists of three parts. They are: (1) the base of the burner (2) the burner tube and (3) the air regulator (fig. 68) ee of tae burner has a side tube for admitting the gas. It also contains a barnes ae ae the nozzle through which the gas enters the burner tube. The lols ariete ee is @ metallic tube fixed vertically over the base. It has two a inaiia lee sides for admitting air, The air regulator is a metal ring tube freely, By Pposite sides and it can be rotated over the base of the burner turning it we can regulate the air flow into the burner tube.——— 20 mL | eeniea) Flash eee Fig. 5 Burette ig. a ‘ hottest portion B Burner tube (ricer Base Fig .6(a) Parts of the burner Fig .6(b) The bunsen flameHow to light a burner? Close the air holes completely by rotating the air regulator. Open the gas tap and immediately light the gas with a match stick. The gas burns with a yellow luminous flame. Now adjust the length of the flame by regulating the gas supply. Luminous flame A luminous flame is obtained when the gas is lighted keeping the air holes completely closed. Since the supply of air is not enough, combustion is incomplete and it consists of unburnt carbon particles. Partially luminous flame Partially luminous flame is obtained by opening the air hole partially. It consists of three parts : (1) _ the outer zone of complete combustion (C) (2) the central zone of incomplete combustion (B) and (3) the inner zone of unburnt gases (A) (Fig. 6(b)). The inner zone -has the lowest and the outer zone has the highest temperature. Non-luminous flame Open the air holes gradually so that the flame loses its yellow colour completely and becomes blue. The flame thus obtained is non-luminous. Now the flame contains only two parts: (1) the inner blue zone of unburnt gas and (2) the outer pale blue flame where complete combustion occurs. The hottest region in a non-luminous flame is the region just outside the inner blue zone. This flame is used for strong heating.Principle Potash alum is prepared by dissolving an equimolar mixture of potassium sulphate and hydrated aluminium sulphate in minimum quantity of water containing little sulphuric acid and then subjecting the resulting solution to crystallisation. K2SOs + AlxSO4)318H20 + 6H20 -> — K2SOsAl2(SO4)324H20 174 666 948 Potash alum is obtained as a colourless octahedral crystals. - Requirements. Two 250 ml beakers, china dish, glass rod, funnel, filter Paper, potassium sulphate, aluminium sulphate, dilute sulphuric acid etc. Procedure About 50 ml of water is taken in a 250 ml beaker and add 13.5 g of aluminium sulphate into it. Then added five drops of conc. H2SOs and stirred the contents until the crystals dissolve. To another 250 beaker, 5g of K2SOs is dissolved in 50 ml of water by stirring. The two solutions are mixed in a china dish and heated to crystallisation point by placing the china dish over a sand bath or a water bath. The china dish containing the concentrated solution is placed over the mouth of a beaker containing cold water and is kept aside undisturbed for slow crystallisation. The mother liquor is decanted off and the crystals are washed with a small quantity of ice cold water. Dried the crystals by pressing between the folds of filter papers. Note the colour, shape and yield of crystals obtained. Results: ; - 1. Colour of the crystals s Z 2. Shape of the crystals = 3.Yield =Experiment Exp-tlo:3 1. PREPARKHION OF FERROUS AMMONIUM SULPHATE (MOHR’S SALT) Principle . Mohr’s salt or Ferrous ammonium sulphate is prepared by mixing equimolar solutions of hydrated ferrous sulphate and ammonium: sulphate in water. The resulting solution is evaporated to get light greenish blue crystals of Mohr’s salt separate out which are monoclinic in shape FeSO4.7H20 + (NH4)2SO4 ? FeSO«(NH4)2S04.6H20 +20 Ferrous sulphate ammonium sulphate Ferrous ammonium sulphate 278 132 . 392, Requirements ‘ 250 ml Beakers, funnel, glass rod, china dish, filter paper. dilute sulphuric acid, ethanol, distilled water etc, Procedure Take 14 g of ferrous sulphate and 6.5.g ml of dilute sulphuric acid into it. The addition o: ferrous sulphate, ammonium sulphate ammonium sulphate in a clean beaker. Add about 2-3 f acid is to prevent hydrolysis of ferrous sulphate. Boil about 50 ml of distilled water in another beaker for about five minutes to expel dissolved air. Add this hot water to the contents in the first beaker and stir the mixture with a glass rod to dissolve the salts. Filter the solution and heat the filtrate in achina dish upto the crystallisation point: Cover the china dish with a watch glass and allow it to cool by keeping it in beaker containing water. When the crystallisation is over, decant off carefully the mother liquor. Wash the crystals using ethanol to remove any sulphuric acid sticking to the crystals. Dry the crystals by pressing between the folds of filter paper and note the colour, shape and yield. Results 1. Colour of the crystals = _Light greenish blue 2. Shape of the crystals 3,Yield = Hees :Capillary tube I— Substance Determination of Melting Point 1. DETERMINATION OF MELTING POINT OF A SOLID: Melting point of a solid is the temperature at which the solid converts into the liquid at constant pressure. Procedure : A high boiling liquid like concentrated sulphuric acid (or liquid paraffin an or ‘elycerol) is taken in a Thiele’s tube (or in a 100cm3 round-bottomed flask) to a level above of its side-tube. The apparatus can be fitted with a cork having a slit carrying a thermometer. One end ofa capillary tube (about 4 cm. long) is sealed by melting. The given organic solid is powdered and about half the length of the tube is filled with it. The bulb of the thermometer is moistened ‘with the bath liquid and the capillary tube is attached to it. The thermometer with the tube is then introduced into the liquid and is heated gently with a small flame. When the solid in the capillary tube begins to melt (shrink) the temperature is noted. This is the melting point of the given sub- stance. The experiment is repeated to get a constant value. Result “The melting point ofthe solid = .. AZ. KDetermination of Boiling Point 1. DETERMINATION OF BOILING POINT OF A LIQUID: Boiling point of aliquid is the temperature at which the liquid converts into the vapour at constant pressure. Procedure : The given liquid is taken in a boiling apparatus ie, a hard glass boiling tube with a side-tube. Two or three pieces of porous bits are added to prevent bombing and to enable Steady boiling, The boiling tube is closed with @ cork carrying a thermometer, the bulb of which should reach only upto the level of the side-tube. An adaptor is attached to the side-tube by means fof a cork. A dry test tube (receiver) is kept at the free end of the adaptor. The liquid is heated gently with a small flame to avoid overheating. At the point, the temperature remains constant ‘and the liquid steadily distlls over. This temperature is noted. The experiment is repeated with the liquid collected in the receiver to get a constant value Result The boiling point ofthe liquid =... 42... K