practice school Module-1 1.CONDENSATION Defination: Condensation is the change of the physical state of mater from the gas phase into the liquid phase and is the reverse of vapourization. It can be defined as the change in state of water vapour to liquid water when in contact with liquid or solid surface or cloud condensation nuclei with in the atmosphere Principle: ‘The explanation of condensation ean be found in the kinetic molecuar theory of gases.As the heat is removed from a gas the molecules of the gas move slowly and as a result, the intermolecular forces are strong enough to pull the molecules together to form droplets of liquid. Similarly reducing the volume of gas Le, compression reduce the average distance between the molecules and thus favour to the intermolecular forces tending to pull them together condensation is efficient heat transfer process. General diagram of condensatio1 FIGLA ‘Types of condensation: ~ Film condensation: A thin film of liquid forms upon condensation of vapour on a cold surface that is wetted by the condensate, The liquid film flows downwards as result of gravity ~ Dropwise condensation: On surfaces that are not well wetted vapour may condense in the form of droplets. Nips, Department of Pharmaceutical chemistry :practice school Module-1 1.1 PREPARATION OF ACETANILIDE FROM ANILINE Principle: Acetanilide preparation invovles replacemet of active hydrogens of amino group by acetyl group with the help of acetylating agent in the presence of acetic acid gives N- acetylated aniline ‘The lone pair of electrons of nitrogen will attack the positive carbon of acetic anhydride. In next step the proton and acetate group were removed. REACTION: NH; : NHCOCH, occn,): a + CH,COOH Aniline Acetanilide Procedure: > Place acetic anhydride (10ml) 10Smillimoles and glacial acetic acid (10ml):170ml to the flask containing ina aniline (10m!) 110millimoles > Surill the flask to disslove the content completely > Attach condensor to the flask ( to dissolve the contents ) and boil and heat it gently for 10mins > Pour the hot liquid into a beaker containing cold water 20ml with stirring, > Collect the crystallized acetanilide by titration under suetion and wash with water. > Dry and re crystallize the product from hot water > The melting range of pure acetanilide is 113-115° Uses: > Antipyretic > Inolden days acetanilide used for treating headache , menstrual cramps , analgesic. Nips, Department of Pharmaceutical chemistrypractice school Module-1 FIG-1.2 Experimental setup for prepartion of Acetanilide Report: FIG1.3 pure form of acetanilide Nips, Department of Pharmaceutical chemistrypractice school Module-1 1.2. PREPARATION OF BENZOIC ACID FROM BENZAMIDE Principle: When primary prides are hydrolysed with dilute sodium hydroxide solution. The corresponding salt of acid and ammonia are formed. The alkaline solution when acidified with concentrated HCL liberates free acid which is removed by filteration Reaction: ° ° NH, __4 .NaQH OH +NH3 HCI benzamide benzoic acid Procedure: Place Igrm of Benzamide into 15ml of 10% sodium hydroxide solution and contained in a 100ml flask fitted with reflex condensor and boil the mixture gentely for 30mins during with ammonia freely evolves. Cool in the solution in ice cold water and cone.Hel slowly until the mixture becomes strongly acidic benzoic acid is immedaitely formed .Allow the solution at pump wash the precipitate with cold water and dry. Recrystallize the benzoic from hot water. Benzoic acid is obtained as colourless crystals with melting point of 121°c and almost insoluble in cold water. Uses: > Antimicrobial preservative > Antifungal tablet and Capsule lubricant. ~ In combination with salicyclic acid used in Whitefield’s ointment. Category > Aromatic carboxylic acid class Nips, Department of Pharmaceutical chemistrypractice school Module-1 FIG1.3 Experimental setup for preparation of Benzoic acid Report: FIG1.4 Pure form of Benzoi Nips, Department of Pharmaceutical chemistrypractice school Module-1 2.DISTILLATION Defination : Distillation involves the process of conversion of a liquid into vapour that is subsequently condensed back to liquid form Ex: Genarally its simplest example ie, when steam from a kettle becomes deposited as drops of distilled water on cold surface. Principle: Distillation refer to the selective boiling and subsequent condensation of component in a liquid mixture It is a separation technique that can be used to either increase the concentration of a particular component in the mixture or to obtain ( almost ) pure compounds from the mixture . The process of distillation exploits the difference in the boiling point of the components in the liquid mixture by forcing one of them into a gaseous state Note: Distillation is not chemical reaction Types of Distillation © Simple Distil tion = Simple distillation is used for pure liquids or for mixture of liquids having different boiling points © Fractional Distillation: Fractional distillation is used for mixtures with similar boiling point . A column is required Ex: vigreum column © Steam Distillation: Steam distillation is used for heat sensitive components They are not water miscible. © Vaccum Distillation: Used for liqiuds with high boiling point > 150°e. . ion: It involves limited melting in ligiud mixture and condensation of vapour. . Distillation: A method of separating mixture base on differences in their volatlites in aboiling liquid mixture Nips, Department of Pharmaceutical chemistry 7practice school Module-1 ations: Appl > Salt water is turned into fresh water through distillation > Alcoholic beverages are made through distillation > Its used to separate liquids from non — volatile solids as in the separation of aleoholie liquors from fermented materials > It is used for the separation of to or more liquids having different boiling points as in the separation of gasoline , kerosene and lubricating oils from crude oil Formula: % Efiiciancy of distillation = (practical yield practicalyield + Theoritcalyield )*100 2.1 SIMPLE DISTILLATION: Procedure : v Collect the apparatus used for distillation and assemble them. v ‘Take the liquid mixture of ethanol 30 ml and water approximately ,which is tobe distilled and filled into the flask upto 1/3 of its volume > Heat the apparatus to the temperature not more than 110 °c ( if the round bottom flask is kept without water bath ). ¥ Add small pieces of porecelain or bumping pumice stone before distillation ,avoids bumping v ‘The liquid start vapourizes , distilled and the vapours are circulated through the jacket of the condenser and condensed > Distillate is collected in a collector / receiver v Finally measure the volume of distilled liquid and caluculate the percentage efficiency of distillation Applications: > It is used for preparation of distilled water and water for injection > Used for preparation of volatile and aroma ie waters, > Used for separation of volatile liquids from non-volatile liquids Nips, Department of Pharmaceutical chemistrypractice school Module-1 thermometer tiation Nas cooling water amp —— Liebig condenser saltwater x condensed water é cold water in — Bunsen receiving flak tbumer stile water clamp stand FIG2.1 Experimental setup for simple Di 2.2 STEAM DISTILLATION : Procedure : > Collect the apparatus used for steam distillation > On laboratory scale , the distillation apparatus of steam generator fitted with rubber cork having two holes v ‘Through one hole along safety tube is passed which , it excessive pressure is generated inside the steam generator Escape of steam from the safety tube indicates that the steam can is almost dry vv The steam generator contains water v Through other hole ,a bent tube is passed which carries the steam to bottom of flask v The steam generator contains water and the round bottom flask contains lemon peels and water the liquid in both the steam generator and flask are heated simultaneously > Then ,the liquid begins to boil when some of the two vapour pressures equal to atmospheric pressure > collected in receiver, the distillate which froms oil like substance v The vapours are allowed to pass through the condenser and condensed liquids are collected in receiver the distillate which forms oil like substances Nips, Department of Pharmaceutical chemistrypractice school Module-1 Applications: > tis used in the isolation of essential oils , water purification and alocoholic beverages production FIG2.2 Experimental setup for Steam di Nips, Department of Pharmaceutical chemistrypractice school Module-1 3.EVAPORATION Defination:- The change of liquid into a vapour at a temperature below its boiling point. Evaporation takes place at the surface of a liquid where molecules with a highest kinetic energy are able to escape, When this The happens, the average kinetic energy lowered, and its temperature decreases. Ex: he evaporation of dew from the grass every morning happens more quickly in the sunny parts of yard Note:-The kinetic energy of the molecule is directly proportional to temperature. Principle Evaporation is a surface phenomenon involving the escape of the surface molecules of a liquid as a ‘vapour into the atmosphere at temperature below the boiling point of the liquid. The liquid particles on the top have higher thermal energy as compared to the particles that are trapped inside the bulk, thus the heat available in the surrounding is enough to allow them to break free from liquid state by over coming the forces of attraction and escape as a gaseous particles. Little energy is needed by the particles to change their state, Volatile liquids have higher rate of evaporation as compared to non-volatile liquids as their particles required very low thermal energy to escape as vapours. Applications:- © Evaporation is regularly used in the food processing, chemical kraft papers and pharmaceutical industries to produce liquid concentrations. © Evaporation is used in the preparation of common salt. © Evaporation is used in the manufacture of drugs containing antibioties, enzymes, hormones and many other substances. © Evaporation used in the manufacture of food products and also demineralised water. © In our daily life evaporation is used in drying of clothes. ‘Types of Evaporaters: ‘© Steam jacketed or evaporating pan Nips, Department of Pharmaceutical chemistry =practice school Module-1 ‘Horizontal tube evaporator Vertical tube evaporator. © Climbing film evaporator «Falling film evaporator. Note: Evaporation causes cooling Eg: Aerosol of microscopic water droplets suspended in the air above a cup of hot tea © proplets of water vapour in a pan, © Rain Evaporating after falling on a hot pavement road, Procedure: © Evaporation by using hot air oven. © Evaporation by direct flame. © Evaporation by air dryer. Evaporation by using hot air oven: © Take a clean and dry beaker and a working hot plate. @ Add 30m of ethanol in to the beaker and place it on the hot plate and switch in the hotplate © After few mins due to the evaporation the droplets of ethanol will form on the inside surface of beaker and watch glass. FIG3.1 Nips, Department of Pharmaceutical chemistry apractice school Module-1 4.RECRYSTALLIZATION Defination: Reorystallization is a technique used to purify chemicals by dissolving both impurities and a compound in an appropriate solvent,either the desired compound Impurities can be removed from the solution,leaving the other behind. Principle: The principle behind the re crystallization is that the amount of solute that can be dissolved by a solvent increases with temperature In re crystallization a solution is created by dissolving a solute in a solvent at or near its boiling point.Re crystallization works only when the proper solvent is used Procedure: Add boiling solvent to a beaker containing the impure compound Heat the beaker and keep adding solvent until the solute is completely dissolved. > Cool the solution: The solution is cooled in open air first,and then cooled in an ice bath slow cooling often leads to purer crystals crystals should form at the bottom of the beaker. > Obti the crystals from solute: The purer crystals precipitated from the solute are desirable part of the mixture, and so they must be removed from the solvent The process used for isolating the crystals that remain in the beaker still is called vaccum filtration If for some reason there are no crystals visible.a gravity filtration can performed. Activated carbon is added to the solution the mixture is boiled,and the funnel system is used to transfer the new mixture to a new beaker of boiling solvent filter paper is used in the funnel to remove excess carbon After this mixture cools slowly there should be large erystals present. Nips, Department of Pharmaceutical chemistrypractice school Module-1 > Dry the crystals: ‘The crystals are dried by leaving them in the aspirator and then by removing them to a glass dish to wait a while longer The purity of a crystals can be tested by performing a melting point determination. Figure 1 t FIGA.L 4.1 Recrystallization of acetanilide from water Procedure: > Weigh 4gm of acetanilide into a 200m! conical flask > Add 80m! of water and heat nearly to the boiling point on electric hot plate > The acetanilide will appear to melt and form an oil in the solution. > Add small portion of hot water , while stirring the mixture and boiling gently until solild has dissolved. > If the solution is not colorless, allow to cool slightly, add 0.1g of decolourising earbon and continoue boiling for few mins to remove the coloured impurities > Filter the boiling solution and collect the filterate in a 250ml conical flask .cover the flask with clock glass and cool rapily with swrilling allow to stand for 30mins to complete separation of fluid Nips, Department of Pharmaceutical chemistry 3practice school Module-1 > Filter with solution through a buchner funnel, wash the crystals twice with cold water. > Weigh the yeild of recrystallized material and determine the melting point. FIGS.2 Vaccum filteration appartus Result: FIG4.3 Pure form of Acetanilide Nips, Department of Pharmaceutical chemistry apractice school Module-1 4.2 Recrystallization of sulphanilic acid from water Procedure: Weigh Sem of crude sulphanilic acid and do as in the procedure of acetanilide from water. ‘Add 0.2gm of decolourizing carbon to the solutionand continoue the boiling for several minutes. Filter the cold solution at water pump, wash with a cold water, Dry and weigh the yeild of recrystallized product. Result: FIG4.4 Pure form of sulphanilic acid Nips, Department of Pharmaceutical chemistrypractice school Module-1 5.SOXHLATION Defination:- Soxhlation is defined an extraction by means of soxhlet extractor. i¢, A soxhlet extraction is a piece of laboratory equipment which was originally helps in the extraction of lipid from the solid material and other molecules from the solid material Principle:- Soxhlate extractor is also known as fat extractor, The fat extractor uses the solvent reflux and siphon principle (surface tension pulls the steam of liquid into separate droplets inside of a sealed air filled chamber) . To continuously extract the solid matter by pure solvent. TYPES OF SOXHLATOR: 1, Kimex soxhlet type extractors 2. Gregar extractor 3. Giant extraction soxhlet extractor. 4, Soxhlet extraction body 5. Micto soxhlet extraction apparatus, 6. PYREX accelerated one-step extractor. 7. Standard glass microfiber extractor thimbles. Applications: © Food testing © Biofuels ‘© Enivornmental analysis of solids,sludge and wastes © Ibis the most useful apparatus for solid, liquid extraction in various fields ‘© Extraction of oil from various materials, ‘© Ithas been used widely fr extracting valuable bio active compounds from various natural sources. General procedure: ‘© Solid matrix is placed in sox thimble, solvent is heated under reflux. ‘* Condensation and extraction with fresh solvent solute are transferred from the extraction chamber into reservior. © Continuous repetition of the extraction. ‘© Exhaustive extraction is complete. Nips, Department of Pharmaceutical chemistry apractice school Module-1 FIGS.1 Soxhelt Extractor Apparatus Nips, Department of Pharmaceutical chemistry