Chapter 4 I UNIT OPERATIONS # LEARNING OBJECTIVES ¢ After completing the chapter, students will be able to: * Understand various unit operations such as size reduction, size separation, drying, filtration, mixing, extraction used in pharmaceutical industries. * Explain the processing equipments for various unit ‘operations. Describe various factors affecting the unit operations. Discuss the need for various unit operations. . INTRODUCTION Unit operations are those operations wherein no chemical reactions are involved. Unit Operations involve a physical change or chemical transformation such as Size reduction, Size Separation, Mixing, Filtration, Drying, Evaporation, Crystallization, Distillation and. other Feactions, All these unit operations can lead to the unit process, Unit operation is a primary activity where physical forces are involved. The unit process “Involves chemical or biological process as precipitation, electrolysis, biodegradation, etc. Thus, the unit operation is primary process used to facilitate the unit process that is a secondary process. SIZE REDUCTION Size refers to physical dimension of an object. Reduction refers to the method of decreasing the size. Size reduction is usually employed in pharmaceutical industries. Size reduction or Comminution or Grinding or Pulverization may be defined as, “a unit ‘Operation to reducing size of bigger particles into smaller Particles using some forces’. external Objectives of Size Reduction: 1. To increase the surface area of a substance in order to increase maximum contact of solid particle with dissolution medium resulting in faster absorption of the drug. 2. Break a material into very small particles in order to separate the two constituents. _ 3. Achieve intimate mixing. He _ To improve the handling characteristics. To reduce the bulk of material. (4.1)Pharmaceutics (F. Y. D. Pharm. a unit Operations To improve the extraction process of the crude drugs. To improve the stability of the various dosage forms as emulsion, the uniformity of color and improves suspension etc. 8. In tablet formulation, size reduction maintains the functioning of lubricants. 9. To increase the rate of drying. 10. To dispose solid wastes easily. Mechanism of Size Reduction: Size reduction of particles follows four basi Compression and Cutting. Fig, 4.1 illustrates the mechanism of size reduction. * Impact: Occurs when material is more or less stationary and is hit by an object moving at high speed or when the moving particle strike a stationary phase. Attrition; When the moving particle is compressed between the edges of two tangentially moving hard surfaces or against a hard surface resulting in shear forces which break the particles. Compression: Breaking of partic ccc ing: Material is cut by means of sharp blade. ° Us T ° ic mechanisms viZ., Impact, Attrition, le by crushing with the application of pressure. ‘cours when material is more or less. stationary and is hit by an object moving ‘speed of when the moving particle this Skea stationary phase 7 vin verte Ms Moving Hsin hard phase ae inane va paces cant between the : etna tere or opal shad Pressure by P y ‘rte resulting in shea forces which hard surface i et break the parties. Bila of particle Breaking of particle by crushing with the ‘pplication of pressure. (Nutcracker) ee Fig. 4.1: Mechanism of size reduction Affecting Size Reduction: 1. Hardness of material: Hardness of material is directly proporti Sar ies po to size reduction. Harder the material, it is more difficult to reduce m a of id . SK‘Pharmaceutics (F. Y. D. Pharm.) 43 Unit Operations 2. Toughness: The drugs containing high moisture or fiber are the tough drugs. Toughness of material is directly proportional to size reduction. The tough the drug, it is more difficult to reduce the size. To reduce the size of the soft and tough material is more difficult than to reduce the size of hard and brittle material. Example Of tough material includes rubber, green twig etc. 3. Abrasiveness: It is a property of hard material and can cause the contamination of the final product if suitable mill is not used. During grinding of abrasive material, metal of the mill may worn and contaminate the final product. 4. Stickiness: Stickiness of material is directly proportional to size reduction. More sticky is the material, it is more difficult to reduce the size of such material. 5. Softening Temperature: Many mills generate the heat during their operation and Fesults in softening of material (stearic acid etc.), which may further cause stickiness and pose difficulty in size reduction, 6. Moisture Content: It influences many properties of a material such as hardness, _ toughness or stickiness that affects the size reduction process. Ideally for dry Grinding the moisture content should be less than 5 % and for wet grinding it should be more than 50%. as A mill is @ tool that breaks solid materials into smaller matter by grinding, crushing or Cutting, Various mills used in pharmaceutical industries include Hammer mill, Ball mil, Fluid energy mill, Colloidal mill, Edge runner mill, End runner mill and disintegrator. {] Hammer Mill - Principle: ‘Hammer mills works on principle of Impact. Impact occurs when the high speed rotating hammers hit the more or less stationary material. This impact results the material to break or _ shattered into smaller pieces. shown in Fig. 4.2, the hammer mill consists of strong metal casing usually made of stainless steel, enclosing a central shaft. ' The hammers (3-4 in number), made up of rectangular steel bars, are mounted with Stary union (swivel joints) on to the central shaft. 'e upper part or center of the casing is fitted with feed hopper. 1 lower part of the casing is fixed with screen through which material can escape the receiver, when sufficiently size reduced. The screen can be replaced as per the d of particle size required. # aPharmaceutics (F.Y.D.Pharm) Hammers (Rectangular steo! bars) Product Fig. 4.2: Hammer mill * Material is fed into grinding chamber of mill through the feed hopper, usually b gravity. * The shaft is rotated at high speed (5000-10000 RPM) and centrifugal forces cause the hammers to swing out radially. The material is crushed or shattered by a combination of repeated hammer impa __ /shocks, collisions with the grinding chamber wall, and particle-on-particle impact. | Perforated metal screens that cover the outlet opening of the mill retain coarse _| terial for further grinding, while materials of the desired / proper size can pass arough, resulting in finished products. action and can grind number of different types of material. due to high speed of rotor operation that ma} bile) materials or drugs containing gums, fats 0! ? feed is not controlled, resulting in decreasedPharmaceutics (F. Y. D. Pharm a5. Unit Operations Applications: 1, To produce intermediate grade of powder. 2. In pharmaceutical industries for the process of wet or dry granulations to produce compressed tablets. Used for milling pharmaceutical raw materials, herbal medicine, and sugar. 4. Used in powdering of barks, leaves, and roots of medicinal plants except sticky materials. 5. Applied in the milling of Active Pharmaceutical Ingredient (API), excipients etc. [i Ball Milt Principle: The ball mill works on the principle of impact and attrition. The particle receives impact from the moving balls and attrition occurs due to the sliding motion of the balls over each ‘other. Construction: Ball mill consist of hollow cylinder made up of metal/porcelain/rubber. The cylinder having diameter of 1-3 m is mounted onto the metal casing in such a way that it can be rotated on its horizontal-longitudinal axis. The cylinder contains balls made up of metals, porcelain or some time pebbles are used as shown in Fig. 4.3. Balls diameter varies from 75-150 mm and occupy 30-50% of mill volume. is Material tobe Cylinder with metallic size reduced _casing (1-3 m diameter) Fs Horizontal longitudinal axis : Mi at (75-150 mm diameter) oq ai oa Fig. 4.3: Ball mill forking: * Material is fed into the cylinder of the mill. The amount of the material should neither be large as it may exert cushioning effect nor be very less which may lead to loss of efficiency and abrasion. * The cylinder is rotated on its axis with rotational frequency of 0.5 s™*.