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Size Separation

Chapter 2 discusses size separation techniques, primarily focusing on sieving, which is used to classify particles based on size, shape, and density. It outlines the importance of size separation in pharmaceutical applications, including quality control and optimization of processes, and details the standards for powders as prescribed by the Indian Pharmacopeia. The chapter also covers the construction and types of sieves, as well as various modes of motion that enhance the efficiency of size separation.

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Size Separation

Chapter 2 discusses size separation techniques, primarily focusing on sieving, which is used to classify particles based on size, shape, and density. It outlines the importance of size separation in pharmaceutical applications, including quality control and optimization of processes, and details the standards for powders as prescribed by the Indian Pharmacopeia. The chapter also covers the construction and types of sieves, as well as various modes of motion that enhance the efficiency of size separation.

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rithiya.stu2019
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Chapter 2 Size Separation or ro rere pec err rrnger arc rai Official Standards for Powders { | Sieves . | Modes of Motion in Size Separation | Sieve Analysis — Testing of Powder | Equipment for Size Separation | Setting Behaviour of Solids — Methods i t Elutriation Methods \ Selection of Size Separation Equipment ¥ Size separation is a unit operation that involves the separation of mixture of various sizes of particles into two or more portions by mear of screening surfaces. Size separation is also known as sieving, sifting, classifying or screer ing. This technique is based on physical differences between the particle such as size, shape and density. Size reduction of a solid material never gives particles of same size but gives particles of varying sizes, i.e., distributes in different sizes These materials must be subjected to a separation technique to obtai narrow size ranges. As far as possible size separation is included as a: integral part of the size reduction process. When particle size distribu tion is to be controlled for the official specifications, size separatic assumes greater importance and has to be handled independent of th size reduction. Screening is a method of separating particles according to size alone: Particles can be separated into individual sizes using sieves. The fine portion consists of a more uniform size. The material that remains o1' the given screening surface is known as oversize or plus material. Thi’ material passing through the screening surface is known as undersize oi minus material. 36 Ch-2 SIZE SEPARATION : 37 * Applications Size separation of solids has important applications. 1. As a method to determine particle size and size distribution, which [Link] in the production of tablets and capsules. 2. As a quality control tool for the analysis of raw materials such as griseofulvin and aspirin. 3. To test the efficiency of a size reduction equipment ¢ Or process. 4. To optimise the process conditions such as method of agitation, time of screening, feed rate etc. 5. To recover valuable products or byproducts. 6. To prevent environmental pollution. The testing of a powder and equipment used for classifying has been discussed in the chapter. Mainly this chapter is purported to provide adequate support to the size reduction process discussed earlier. > OFFICIAL STANDARDS FOR POWDERS In general, powders are vaguely described as coarse and fine pow- ders. However, it is essential to identify with some guiding specifications. Indian Pharmacopeeia has prescribed standards for powders for phar- maceutical purposes. Accordingly, degree of coarseness or fineness is expressed with reference to the nominal aperture size of sieve through which powder is able to pass. The relevant grades of powders and sieve number along with nominal aperture size are shown in Table 2-1. The IP 1996 specifies five grades of powder. TABLE 2-1 # Grades of Powders and Sieve Number alongwith Nominal Aperture Size as per IP ‘ Sieve through: Nominal ‘Sieve through Nominal Grade of : which all | mesh ; which 40% ‘| mesh Particles : aperture: particles + aperture must pass is * pass iz 38 PHARMACBUTICAL ENGINEERING + UNIT OPEKATIONS Coarse powder : A powder, all the particles of which pass through sieve with nominal mesh aperture of 1,70 mm (No, 10 sieve) and + more than 40,0 per cent through a sieve with nominal mesh aperture 355 um (No. 44 sieve) is called coarse powder. In a similar way, other definitions can be written for the contents , the Table 2-1. When fineness of a powder is described by means of number, it is an indication that all the particles of the powder shall pa through the sieve of which the nominal mesh aperture in pun, is equal that number. Normally, for compound powders, fine powders are preferred, whi moderately coarse powder is used for the preparation of tinctures. Coar powder without fines is employed in percolation process, The above mentioned terminology has applications in the productic of galanicals. A few examples are given in the Table 2-2. The pharmacoposia has prescribed upper and lower limits for tl three coarse grades of powder. For two fine grades, the pharmacope has prescribed only the upper limit. TABLE 2-2 Some Examples of Crude Drugs and Nature of Powder Required Ashoka coarse . Nux vomica j seeds } moderately coarse Rauwolfia roots i moderately coarse Ergot | sclerotia | moderately sine Ipecac root f fine Ephedra stem fine # SIEVES Sieves are the simplest and sieving is the most frequently use method for size separation. Construction Sieves for pharmaceutical testing are constructed from wire clot with square meshes, woven from wire of brass, bronze, stainless steel ( any suitable materials, Sieves should not be coated or plated. Thet must be no reaction between the material of the sieve and the substan¢ to be sieved. Ch-2 SIZE SEPARATION 39 se Types of sieves The prin-ary considerations for sieves are given to the size and shape of aperture opening. Square meshes are arranged as per the specifica- tions. Sieves commonly used in pharmaceutical processing include: > Woven wire sieves » Bolting cloth sieves . > Closely spaced bars (screens) > Punched plates Woven wire sieves : Wire woven sieves are general-purpose sieves and widely used in the pharmacy practice. The types of woven wire sieves are: > Plain weave » Twilled weave The nature of sieve surfaces is shown in Figure 2-1. For fine sieving, metal wire woven sieves are used. Common examples are hand sieves. These are included in roller mill, ball mill etc., during milling. In case of coarse sieves, the wire is generally given a double crimp to preserve the alignment of the wire. . ; ee EB (a) Plain weave sieve _—_(b) Twilled weave sieve Figure 2-1. The nature of sieve surfaces. Bolting cloth sieves : Silk, nylon and cotton are generally woven from twisted multi-strand fibres. Nylon cloths are generally designated by their micrometer opening and available in different grades. These are used for the separation of fine powders. Hum-mer screen uses this type of screen. Bar screens : Bar screens are generally used in handling large and heavy pieces of materials. The bars are fixed in parallel position and held by cross bars and spacers. Bars which taper in thickness from one end to the other are recommended, because they tend to avoid blinding. Grizzlies use these types of screens. Punched plates (Perforated screens) : These are used for coarse sizing. The screens are prepared by using a metal sheet of varying 40 PHARMACEUTICAL ENGINEERING : UNIT OPERATIONS. thickness with perforated holes. The holes may be round, oval, squan or rectangular (Figure 2-2). These types of screens are used in a hamme mill. A plate with a large number of holes and a small amount of residua metal will have a large capacity, but will wear rapidly and vice versa. I general, for openings much over 25 millimetres in diameter, a plate will round perforations is preferred over a wire screen. The applications 0 Screen configurations are given in Table 2-3. Figure 2-2. The configurations of punched plates or perforated screens. TABLE 2-3 Applications of Various Mill Screen Configurations of Perforated Screens Perforation shape: Recommended use : Round holes | Fibrous materials Clogs more quickly; lower i } hole size is limited, because i } of structural strength. f fe dae Herringbone { Amorphous and | Slightly coarse powder than screen (slots) } Crystalline materials | ° equal-diameter round f {perforations Cross-slots | Amorphous materials |. Same. grind size [Link] equal ; and slurries with | ‘sized round pérforation; finer slot size, attainable than } coarse particles | round perforations... i . Herringbone design : Herringbone design consists of a series of slotted holes repeated across the surface of the screen. These are made at an angle of 45 degrees to the length of the screen. It is preferred for &y-2 SIZB SEPARATION 41 Xinding crystalline materials and for continuous operation. If the width '£ the slot is equal to the diameter of a round hole, it grinds the particles ‘@arser than the round hole. This design should not be used for fibrous Materials, as it is possible for fibres to align themselves along the slots aad pass through with inadequate size reduction. Cross-slot screens : In this type, openings are at right angles to the rath travelled by milling mechanism. These are used for milling slurries, rat not used for fine grinding in hammer mills as it clogs readily. Standards of Sieves, Dimensions and Notations Common standards used for sieves are: (a) Tyler standard sieve series (in USA) (b) US standard sieve series (in USA) (c) British standard sieve series (in UK) (d) German DIN (Deutsche Industrienormein) (in Germany and Europe) (©) IP standard sieve series (in India) (f) International test sieve series (ISO) (World wide) Tyler and US standards can be interchangeable, since the difference >etween the two standards is less than the allowable tolerance in weay- ing of the screens. These are also known as test sieves. Sieves used for pharmacopceial testing must match with the following specifications: 1. Number of sieve : Sieve number indicates the number of meshes per linear length of 25.4 millimetres. 2. Nominal size of aperture : Nominal size of aperture indicates the distance between the two adjacent wires. It represents the side of a square aperture. IP 1996 gives the nominal mesh aperture size for majority of sieves in mm or in pm. 3. Nominal diameter of the wire : Wire mesh sieves are made from the wire having the specified diameter in order to give a suitable aperture size and sufficient strength to avoid distortion of the sieve. 4. Approximate percentage sieving area : This standard expresses the area of the mesh as a percentage of the total area of the sieve. It depends on the size of the wire used for any particular sieve. Generally, the sieving area is kept within the range of 35 to 40 per cent in order to give suitable strength to the sieve. 5. Aperture tolerance average size : Some variation in the aper- ture size is unavoidable. This variation is expressed as a percentage and is known as the aperture tolerance average. In 42 PHARMACEUTICAL ENGINEERING : UNIT OPERATK fact, it is a limit given by pharmacopceia within which a pa lar dimension or average aperture size can be allowed to and still be acceptable for the purpose for which it is used. mvshes cannot be woven with the same accuracy as ¢ meshes. Hence, the aperture tolerance average is lowe coarse sieves than the fine sieves. According to IP 1996, a sieve must conform to the specifica given in Table 2-4, TABLE 24 Standards for Sere Seer ee Approximate Approximate _ Nominal mesh’ Toleranc Sl. sieve percentage aperture size average no. number sieving area aperture si . (mm) (+ mm) 1 4 55 4.0 0.13 2 6 TT 2.8 0.09 3 8 48 2.0 i 0.07 4 to 46 7 0.06 5 12 41 14 0.05 6 16 - 1.0 0.03 7 - ~ ym ym 8 22 37 710 25 § 2s 36 600 : 21 10 30 38 500 i u 36 36 425 : 15 R 44 38 355 j 13 i 4 37 230 | 13. 9) 4 85 35 180 - 16) 15 100 36 150 _ 94 (6.6) 16 120 34 125 Meee ac) 17 150 36 106 74 62) 18 170 35 90 | 66 (46) 19 200 . 36 ; 75 » 6.1 (41) 20 240 34 i 63 | 53.67) 21 300 35 53 / 484) a : a i 48 G.1) Note : Figures j in the ‘brac ets, refer to close tolerance and those with brackets refer to full tolerance. Ch-2. SIZE SEPARATION 43 Comparison of Ideal and Actual Screens An ideal screen would sharply separates the feed mixture in such a way [Link] smallest particle in the oversize would be just larger than the largest particle in the undersize. Such an ideal separation defines a cut diameter, Dp. that makes the point of separation between the fractions. Usually, Dp is chosen to be equal to the mesh opening of the screen. An actual screen is the one, which does not give perfect separation about the cut, diameter. In an actual screen, the overlap between the smallest particle in oversize and the largest particle in undersize is more pronounced, when Particles: 7 > are needle like, fibrous. > tend to aggregate. > tend to strike the screen surface endwise and pass through. > tend to strike the screen sidewise and retained. Commercial screens usually give poor separations than testing screens of the same mesh opening when operated on the same mixture. -* MODES OF MOTION IN SIZE SEPARATION Screening is a method of separating particles according to size alone. The basic technique involved is passing the particles through a series of sieves of uniform size. In this, the particles drop through the openings due to gravity. Coarse particles can drop easily through large openings, but it is difficult to screen the fine powders. This process can be hastened by inducing some type (mode) of motion (movement) to the particles. Size separation is + ysically assisted by three methods. 1. Agitation 2. Brushing 3. Centrifugal force These modes of shaking help to shake the material so that sieving will be quick and entire sieving area can be utilised. Agitation Method Sieves are agitated in a number of ways. Some of them are discussed below. Oscillation : The sieve is mounted in 2 frame that oscillates back and forth, i.e., reciprocal motion (Figure 2-3). It is a simple method, but 44 PHARMACEUTICAL ENGINEERING : UNIT OPERATION, the material may roll on the surface of the sieve. The motion is paral to the plane of the sieve. The sieves can be slightly inclined. 7 reciprocating motion is induced by means of an ordinary eccentric or rotating shaft. ott > eee vibrator Mechanically (b) Electrically ibrated vibrated Figure 2-3, Figure 2-4. Oscillatory motion of screen. Vibrating motion of screens. Vibration : The sieve is vibrated at high speed by means of eccentric device (Figure 2-4) either electrically or mechanically. Ray vibration is imparted to the particles that helps the powder to pi through the sieve. Electrically vibrated screens are particularly useful the chemical industry. Example is hum-mer screen. They handle lig fine and dry materials successfully. Inducing vibrations also preve blinding of meshes. Gyration : In this method, a system is made so that sieve is tubber mounting and connected to an eccentric flywheel (Figure 2- This gives a rotary movement of small amplitude to the sieve, which tum gives spinning motion to the particles that helps to pass th through the sieve. > : ZO i ~ Eccentric Eccentric Gyratons yrsta 2 in ration in Gyration at one end horizontal plane vertical plane aand shaking at other end Figure 2-5, Gyratory motions of screens or sieves. Gyratory screens are box like equipment, either round or square, wi a series of screen cloths nested atop one another (Figure 2-5). Mo Ch-2 SIZE SEPARATION 45 gyratory screens have auxiliary vibrations caused by balls bouncing against the lower surface of the screen. Agitation methods are not continuous methods. However, these can be made continuous by inclination of the sieves. Separate outlets are made for undersize and oversize particles. Normally, all the three modes of agitation are used simultaneously for an efficient size separation. Rotex screen works on this principle. Advantages : (1) Agitation methods are inexpensive. (2) Simple and rapid, Disadvantages: (1) Agitation methods have lower limit of the particle size. (2) If the powder is not dried, apertures become clogged with parti- cles leading to improper sieving. (3) During agitation, attrition (particles colliding with each other) occurs causing size reduction. - Brushing Method In this case, a brush is used to move the particles on the surface of the sieve and to keep the meshes clear. The brush is rotated in the middle in the case of a circular sieve, but spiral brush is rotated on the longitudinal axis in case of horizontal cylindrical sieve. One example is brush sifter (Figure 2-6). This is used for size separation of greasy or sticky powders such as waxes and soaps. Figure 2-6. Brush sifter. 4 Centrifugal Method In this method, a high-speed rotor is fixed inside a vertical cylindri- cal sieve, so that on rotation the particles are thrown outwards by centrifugal force. The currents of air can be generated by means of a jet 46 PHARMACEUTICAL ENGINEERING : UNIT OPERATIONS. of air into the equipment, which heips in separating the particles. A fe examples of equipment that work on this principle are cyclone separat and air separator. Advantages: (1) Centrifugal methods are extremely useful in cases where con ventional sieving tends to block the sieves. (2) Extremely useful for fine powder, because sieves have the limi tation of mesh size. SIEVE ANALYSIS—TESTING OF POWDER The milled material is subjected to size separation in order to obtait the powder of desired size or size distribution. Size distribution analysis is important in different areas as mentioned below. » Quality control tool for the analysis of raw materials. » Testing the efficiency of a size reduction equipment or process. > Optimising the process conditions such as method of agitation, time of screening, etc. > Selecting the sieve system for commercial equipment. Errors can arise if the sieves are overloaded or if insufficient time is allowed for the particles to pass through. 2 Sieve Shaker Machine aia Principle : The powdered drug is separated according to its particle L 7 siz using a number of sieves in a nest. These are subjected to different Jypes of agitation, so that size separation is rapid. Construction : Standard sieves of different mesh numbers are avail- able commercially as per the specifications of IP and USP. These sieves are fixed in a mechanical shaker apparatus (Figure 2-7). Working : Sieves are arranged in a nest with the coarsest at the top. A sample (50 g) of the powder is placed on the top sieve (Figure 2-7). This sieve set is fixed to the mechanical shaker apparatus and shaken for a certain period of time (20 minutes). The powder retained on each sieve is weighed. Practical considerations : Care should be taken in order to get reproducible results. The type of motion influences sieving; vibratory motion is most efficient, followed by side-tap motion, bottom-pat motion, rotary motion with tap and finally rotary motion. The type of motion and intensity of the shaker are fixed and standardized. Shakers are commercially available. 7 2 SIZE SEPARATION 47 Figure 2-7. Laboratory sieve shaker machine. Other factors are weight of the sample and duration of shaking. eves produced by photo-etching and electro-forming techniques are ed to get a better estimate of the size distribution analysis with a lower nit of estimation of particle diameter 50 pm. Advantages : It is inexpensive, simple and rapid with reproducible sults. Disadvantages : (1) Lower limit of particle size is 50 pm. (2) If powder is not dry, apertures get clogged with particles, leading to improper sieving. (3) During shaking, attrition (particles colliding with each other) occurs causing size reduction of particles. This leads to error in estimation. Variants : Electromagnetic sieve shaker—It is useful for analysing owders under controlled conditions. Sonic sifter — This apparatus tilises sonic oscillations. A mechanical pulse action is used to reduce linding and agglomeration in the sub-sieve sizes. \spine Airjet Sieve Principle : In the Alpine airjet sieve, sieving action involves the pplication of a jet of air on one side of the sieve und suction on the 48 PHARMACEUTICAL ENGINEERING : UNIT OPERATIc other side. The material is maintained in a fluidised state on the sg, by a stream of air. Vacuum is applied below the screen, so tha undersized powder is sucked through the sieve. Construction : The construction of a Alpine airjet sieve is shoy, Figure 2-8. It consists of a metal housing into which the sieve me fitted. Sieve cover is placed in such a way that an air-tight se obtained. A slit is provided such that its upper edge is in level witt upper edge of the housing. Provision is made to pass airjet beloy, slit. Suction line is provided below the sieve, which can be contr with the help of a manometer. Sieve cover (air tight) Coarse powder Sieve mesh ae Current of air directed Fines through rotating slit Vacuum i. r connection Connection inle Hes to manometer Figure 2-8. Alpine airjet sieve. Working : A small amount of powder (about 10 g) is spread on sieve. The cover is placed in position. The slit is set into rotation sending a jet of air from below. The powder is fluidised in the upv jet of air. The suction is adjusted until the manometer reads at 27 kPa. The vacuum (in the interior of housing) sucks the undersi powder through the sieve. The material is recovered. Sieving is continued for two minutes and the residual powdet weighed. This powder is transferred to the next sized mesh with a ! brush. This process is continued until all fractions are collected from sample, by changing the sieve meshes as well as magnitude of the sucti Uses : Alpine sieve method is used for the analysis of powder for size distribution. This method is particularly useful in cases wh conventional sieving tends to block the sieves below about 80 pm. (h-2 SIZE SEPARATION 49 Advantages : (1) In Alpine airjet sieve, fluidisation of powder pre- vents blocking of the mesh. (2) It is a rapid method once the mesh is placed and gives reproduc- ible results. (3) It is very useful for fine powders. Disadvantages : (1) The capacity of Alpine airjet sieve is limited. Therefore, it is not useful for large-scale separations. (2) This method is tedious, because each time only one particle size powder is obtained. Data Presentation Frequently a powder is assigned by a mesh number of the screen through which it passes or on which it retaines. ‘It is expressed in terms of arithmetic or geometric mean of the two sieves, i.e., a powder passing through a 36 mesh and retained on 44 mesh sieve is assigned an arithmetic mean diameter of (425 + 355)/2 or 390 pm. This is reported as undersize. Data Analysis The weight of sample retained on each sieve is considered for the analysis. The data are analysed for normal, log-normal, cumulative percent frequency distribution and probability curves. Along with these, different mathematical expressions are also used such as average particle diameter, geometric mean weight diameter etc. For further analysis refer the book, “Textbook of Physical Pharmaceutics” by C.V.S. Subrahmanyam, Vallabh Prakashan, Delhi. EQUIPMENT FOR SIZE SEPARATION A wide variety of equipment have -been developed differing in the scale of operation, ruggedness, method of movement of material and material of construction. The modes of size separation are discussed earlier. Some factors to be considered are: (@) wear of the sieves (b) blinding (©) machine noise General Classification of Screening Equipment The screening or sieving machines may be divided into different classes. (1) Grizzles : For coarse materials above 50 mm — large lumps. 50 PHARMACEUTICAL ENGINEERING : UNIT OPERATIONS-I (2) Revolving screens : Separations above 13 mm — trommels. (3) Shaking screens : Separation from 13 mm down wards to fines. (4) Vibrating screens : Coarse size (13 mm) to fines. (5) Oscillating screens : Fine mesh size. (6) Fluidised systems : For very fine powders. Some important equipment are described below. * Shaking Screen Principle : Particles of different sizes are separated by passing them through a sieve, which oscillates to and fro continuously. sks nl rotating shaft biscaiee Figure 2-9. Shaking screen in inclined position. ) Construction : The construction of a shaking screen is shown in Figure 2-9. Shaking screen consists of metal frame to which a screen is fixed at the bottom. The screen cloth may be riveted directly or fitted using a removable bolted frame. The metal frame can be arranged horizontally or in inclined position. “It is suspended by means of hanger rods, so that it can move freely. The side of the metal frame is connected to an ordinary eccentric on a rotating shaft. The entire frame | can experience reciprocating motion. Working : The screen is allowed to shake in a reciprocating motion. ‘The feed (material to be screened) is introduced on to the screen from a side. Therefore, fine particles get screened off initially. The remaining material moves forward during the motion of the frame and gets sepa- rated. Thus, the desired size particles can be obtained from the material. The advantages of shaker screen are that it requires low head-room and low power requirement. The disadvantages are that shaker screen requires high cost of maintenance of screens and supporting structures. Its capacity is low. Ch-2 SIZE SEPARATION 51 Variants : The above screen system may be vibrated to keep the particles moving and to prevent blinding. It is used when large capacity and high efficiency is desired. Rotex Screen 7 Principle : Rotex screen works on oscillating agitation (back and forth) by means of an eccentric mechanism. Further, vibrations are caused by balls bouncing against the lower surface of the screen cloth. This rapid motion helps the particles to roll on the surface of the screen and separate out. Construction : The construction of a Rotex screen is shown in Figure 2-10. The screen is slightly inclined at 5 degrees. A coarser supporting screen is placed below a coarse screen (Figure 2-10a). Between the screens, wooden blocks are placed at different intervals. Between the wooden blocks, a number of rubber balls are placed. This ‘wo-sieve system represents one unit. Several such units are arranged in he desending order, i.e., sieve of larger size at the top and smaller one at the bottom (Figure 2-10b). Screen of certain size = FS Wooden — ber | Single Block EOg Ln Ot paper seen sentinting screen (Coarser than above screen) (a) Unit sieve system Feed Coarsest screen: POST rang Eccentric bearing o> Parner pane 221) Sliding bearing > Wooden blocks Rubber balls Fine Coarse (b) Assembly size size Figure 2-10. Rotex screen. If more number of sieve sizes are desired, n screens are arranged in a imilar manner to obtain (n + 1) fractions. This assembly is supported 52 PHARMACEUTICAL ENGINEERING : UNIT OPERATIOQ, on sliding contacts at the lower end. The upper end of screen syste; connected to an eccentric pin on a flywheel. . Working : The screen system is allowed to agitate with the hel eccentric. The shaking motion of the screen causes balls to fly bety the screens. As they strike the inclined sides of the wooden blocks, balls deflect upward and strike the underside of the screening cloth thus prevent the blocking of the mesh (Figure 2-10a). The fee, introduced at the elevated end of the screen. The material pa through the upper screen and reaches the next screen. This pro continues until all the material is separated into fractions. The fract are collected separately at the outlet point. Uses : Rotex screen is used for handling a variety of chemi usually dry materials. Granular matrices and powdered foods are size separated by Rotex screen. Therefore, these are used extensivel standard equipment in many chemical and processing plants for hanc fine separations. * Cyclone Separator Principle : In cyclone separator, centrifugal force is used to sep the solids from fluids. The separation process depends not only on particle size, but also on the den- sity of particles. Depending on the fluid velocity, the cyclone separator can be used to separate ‘Tangential all types of particles. It is also "| possible to allow fine particles to be carried by the fluid. Construction : The cons- truction of a cyclone separator is shown in Figure 2-11. It consists of a short vertical, cylindrical ves- sel with a conical base. The upper sole part of the vessel is fitted with a ads tangential inlet. The outlet (solid Figure outlet) is arranged at the base. HHL. Cyelone separate Fluid outlet is provided at the centre of the top portion, which ext¢ inwardly into the separator. Such an arrangement prevents the air sh circuiting directly from the inlet to the outlet of the fluid. Working : The solids to be separated are suspended in a stream gas (usually air). Such a feed is introduced tangentially at a very ! velocity, so that rotary movement takes place within the vessel. Flu outl ‘h-2_ SIZE SEPARATION 53 When large particles (high amount) of material is to be hanc Applications : Powder is deliberately suspended in fluid to ot separation of the particles. Dust particles are removed from stream and gases to eliminate contamination. Solids are removed f liquid waste by this method. Disadvantages : It is a batch process. Discrete particle fract cannot be collected, as sample may contain particles of different d eters. Free Settling Free settling implies that particles settle independently, without interference of other particles in the fluid. Free settling is achieved, when the concentration of particles’ i and the volume of fluid is high. The effect of the walls is negli The particles settle under the influence of gravity. As the particle m down, the fluid offers a greater frictional resistance, When the resi force is exactly equal to the force of gravity, a condition is reache which the acceleration of particle becomes zero. From this time wards, the settling of particle follows a constant velocity. 1 conditions are similar to the laminar flow. This velocity is ¢ terminal settling velocity. This velocity can be obtained from St equation. For describing the flow pattern of the fluids, Reynolds nw is also utilised. The Stokes equation is given below. _ P@s=98 = 18) h-2 SIZE SEPARATION 59 here U = Terminal settling velocity, m3/s D = Diameter of the particles, m? Ps = Density of the particle, kg/m} p = Density of fluid, kg/m? Acceleration due to gravity, m/s” 1) = Viscosity of the medium, Pa.s As per equation (1), terminal settling velocity for different flow atterns can be described as follows. > Laminar region - terminal elo is equal to square of the particle diameter, + Turbulent region - terminal velocity is almost proportional to the particle diameter. Whatever is the condition, the settling velocity is so slow and the ize of particle is so small that it is impracticable to produce size eparation. However, sedimentation usually involves settling velocities elow the critical value. Hydraulic classification process may involve articles of one material, but of different sizes, two or more materials of lifferent specific gravities, but of same size. iindered Settling Hindered settling implies that light particles are pushed by heavier articles, on account of particle-particle collisions. When the concentration of solids is high, particles are close to each yther and collide continuously. Stokes law is not applicable in this case. Che settling velocities are lower in the hindered settling due to variety of easons. > There is an appreciable displacement of fluid opposite to the direction of motion of solid particle, due to high concentration of solids, » The available effective cross section of liquid is restricted. For hindered settling, settling velocities are predicted for the concen- tration of uniform svheres. When the size distribution of particles is wide, particles are irregular in shape of when flocculation of fine parti- cles is observed, it is more difficult to predict settling velocities. Settling — Clarifiers and Thickeners In a suspension, if the solids remain as an individual particle of a few micrometers (< 5.0 mm in diameter), the gravity settling rate will be very low due to Brownian motion. In fine suspensions, the particles may form agglomerates and these settle at reasonable rates. Agglomera- 60 PHARMACEUTICAL ENGINEERING : UNIT OPERAT; tion can be promoted by adding flocculating agents, namely ions, mers (ionic and nonionic), alumina, sodium silicate etc. Fy flocculated suspensions are used as dosage forms. These prepar, are known as thickeners. The settling behaviour of the floc so} different from that of denser solids. Flocs : The material to be settled is in the form of flocs (aggre; Further, aggregates have high porosities and retain considerable a of water within them. The flocs are assumed to’ be uniform in siz shape, so that they settle at uniform velocities under conditio hindered settling in the initial stages. The flocs upon settling compressed to a certain extent by subsequent settling of flocs. sedimentation of flocs is hindered by the other solids to a certain e The sedimentation behaviour can be studied using glass cy (Figure 2-16). Several stages in the settling of flocculated susper are described below, using the stage ‘b’ tube. » Initially the dispersion is uniform (Tube ‘a’ of Figure 2-1¢ > After sometime, a layer of clear water is observed at the t portion of tube b). > Coarse particles settle at first to the bottom. It is represent zone D. > The next settled solids form a transition zone, i.e., zone C. » The boundary between the layers C and D is usually ot (not visible) and is marked by vertical channels through ' ‘water is escaping from the lower layer which is under com sion. > There upon a zone of partly thickened material above. » Then a zone of B of the material at original concentration. pitg: iid me = Me () © Figure 2-16. Typical slurry settling tests-Batch process — Thickeners b-2 SIZE SEPARATION 61 As settling continues, the clear zone increases and the zone B de- eases (Tube d). Subsequently zone B disappears (Tube e). The zone gets compressed on the accumulation of solids above. This results in Sappearance of transition zone (Tube e). This further compresses the me D. Compression breaks the floc structures, the void liquid gets spelled to the zone above. After a particular stage. sedimentation stops. Slurries vary in their settling rates and the relative heights of differ- \t Zones, during settling. The experimental studies of settling rate for fferent initial heights and concentrations are needed for the design of e thickner. lassification Methods Classification methods of a powder are the particle separation meth- ls based on the principle of settling rate of particles into different 2ctions of narrow particle size range. Classification method is not a size separation method as obtained ing sieves. Even the mixture contains materials of different densities, d sizes, classification is possible into coarser fraction containing heavier mmponents and finer fraction richer in lighter component. If separation ces place based on differential densities, devices are known as sorting ussification. The principle involved is sink-and-float or differential ttling. Differential settling methods utilise the differences in terminal Jocities that can exist between substances of different densities. ‘The construction of hydraulic classifier is shown in Figure 2-17. In 's type, the sorting columns have same diameter, but water streams are tered at different velocities from the bottom of each column. The size the particles of each vessel is increased, partly because the amount of uid to be handled increases and partly to reduce in stages the surface locity of fluid flowing from one vessel to another vessel. Slimes nN Figure 2-17, Hydraulic classifier. 62 PHARMACEUTICAL ENGINEERING ; UNIT OPERA} Applications : Hydraulic classifiers (fluid classifier) are useful lower size ranges. Sedimentation tests are applied to light ka order to limit the coarseness of the powder. Light kaolin must co; fine particles. Further, therapeutic activity depends on the ads properties, which are related to surface area. Similarly, chalk i subjected to wet-grinding followed by sedimentation or elutriatio water. Disadvantages : Classification methods do not give accuratel; products as screens do. These methods are used to convert dilute of fine particles into a clarified liquid or a concentrated susp These are simple methods and applicable only for batch pro Discreet particle fractions cannot be collected. Double Cone Classifier Principle : The particles in the powder are separated by reg the hydraulic water supply and the height of inner cone by hand Construction : The construction of a double cone classifier is in Figure 2- 18. It consists of two cones of different sizes plac inside the other. Both cones are pointed downwards. Provision i at the bottom for the entry of water. In the upper top portion, fe is arranged. A mixing port is introduced at the centre of the insid Working : The feed of powder is introduced into the inne Water is introduced through the cone and moves upward directiot mixing port is allowed to rotate. The feed is forced towai periphery of outer cone. (centrifugal effect). Such a mechanism Hand land wheel Feed Over flow fines Inner cone Coarse particles Figure 2-18, Double cone classifier. (Ch-2 SIZE SEPARATION 63 the effective interaction of particles and water. The particles under settling impact the uprising water stream. The fine particles are carried upward and escape through the peripheral lounder. The coarse particles settle into the chamber and drawn off at different intervals. Uses : Wet and dry sizing can be done using the double cone Classifier. Corrosive and abrasive materials can also be handled. Advantages : The cost of installation is cheap. Operation of the equipment is easy. Disadvantage : The solubility of solid in the fluids must be low. } ELUTRIATION METHODS Elutriation is a method of separation of particles in a powder based on the low density of fine particles and high density of the coarse particles using fluid flow. Elutiation and sedimentation are different in one respect (Fig. 2-19). In case of sedimentation, particles move in the direction of gravitational force, while in elutriation, some particles move against the gravitational force. The arrows are vectors, showing direction and magnitude of particle movement. In sedimentation, fluid is stationary and particles settle based on the particle velocity. In elutriation, fluid flows in opposite direction of the settling movement. The upward velocity of fluid is less than the settling velocity of the particles. Hence, time is an important factor. In practice, particles can be seen to rise with the fluid and then to move outwards to the tube-wall, where the velocity is lower and these start to fall. Figure 2-19. Comparison of (a) sedimentation and (b) elutriation. 4 PHARMACEUTICAL ENGINEERING : UNIT OPERATI{ Uses : Elutriation technique is applicable to insoluble solids sux kaolin or chalk, which are subjected to wet grinding followed by | mentation or elutriation. Advantages : Elutriation process is a continuous process. Separ of size fraction is quick as compared to other methods. The apparat more compact than that are used in sedimentation methods. Depen on the number of fractions required, the same number of tube different area of cross-section can be connected. Disadvantages : The suspension (or solids) should be diluted, w may not be desirable in certain cases. Static Tank Method The construction of elutriating tank is shown in Figure 2-20. The powder or paste made by levigation is kept in an elutriating tank. mixed with a large quantity of water. The solid particles are distrib uniformly in the liquid during stirring. Then the particles are allowe settle. Depending on the density, the solid particles may either s down or remain suspended in water. Samples are withdrawn at diffe heights through the outlets. The powders are dried and thus various fractions are collected. Fo VD) very fine partictes FO) sedium sized particles SR) coarse particles Figure 2-20, Elutriating tank — Static method. Single Separation With Mobile Liquid In this elutriating process, the particles are suspended in a movi fluid, generally water. The apparatus consists of a vertical column glass tube (or cylinder) with an inlet near the bottom for introducing | suspension (Figure 2-21). An outlet is provided at the top for | overflow of fluid of fine particles. Ch-2 SIZE SEPARATION 65 => Fluid and fine r particles Suspension -> of solids ' Coarse particles Figure 2-21. Elutriation — Simple separation. The feed is introduced from the bottom. The movement of particles is as follows. Generally, fluid is allowed to flow upward direction, while particles move downwards due to gravitational force, depending, on the experimental conditions. > If the upward velocity of the fluid is less than the settling velocity of the particles, sedimentation occurs. » Conversely, if the settling velocity of the particle is less than the upward fluid velocity, particle moves upwards with the fluid flow. Thus, the fluid flow (velocity) contributes significantly for the sepa- ration of particles. Therefore, in elutriation, powder is divided into different size fractions. A single column will give single separation into two fractions. : . ” Separation as Multiple Fractions Several vertical liquid columns may be arranged in series (Figure 2-22). Each subsequent tbe must have an increasing area of cross section. In such a case, each column will give the separation of only two fractions. The velocity of the fluid decreases in successive tubes, as the area of cross section increases. Thus, several fractions are separated, collected and dried. °* SELECTION OF SIZE SEPARATION EQUIPMENT Selection of specific size separation is the pharmacopoeial require- ment. The most efficient method should be selected based on the particle properties, 66 PHARMACEUTICAL ENGINEERING : UNIT OPERATIOQ » If particles are already present in suspension as obtained | colloidal mill (water) or fluid energy mill (air), then separz can be achieved by elutriation and cyclone separation. In t cases, separation is the most important, because oversize n tial is returned to the mill. + As many pharmaceutical solids are water soluble, separ. must be restricted to the use of air (cyclone separator o1 separator) or sieve methods. Over flow with very fine particles Suspension of solids Coarse Medium size Fine particles particles particles Figure 2-22. Elutriation — Multiple fraction separation The final choice of the equipment depends on the feed mat nature of finished product, facilities available and costs in term: procurement and maintenance. Glossary of Symbols p =Density of fluid, kg/m3 1 = Viscosity of the siedium, Pas . Ps =Density of the particle, kg/m? D =Diameter of the particles, m? g =Acceleration due to gravity, m/s? U =Terminal settling velocity, m/s QUESTION BANK Each question carries one mark Note : Encircle the alphabet which corresponds to the single best response. 1. Size classification is also known in one of the following terms. A. Size analysis B. Size distribution C. Size reduction D. Size separation n-2 SIZE SEPARATION 67 s 10. 11. Size separation is NOT based on one of the following properties, A. Particle density B. Particle shape C. Particle size D. Particle texture Which one of the screens is used for size separation of big and heavy particles? A. Bar screens B. Bolting cloth sieves C. Punched plate screens D. Woven wire screens Which one of the screens is attached to the size reduction equipment? A. Bar screens B. Cloth sieves C. Herringbone screens D. Woven wire screens . Which one of the following indicates the nominal size of aperture? A. Area of mesh as percentage B. Distance between two adjacent wires C. Number of meshes per linear length D. Wire having specified diameter that gives suitable aperture . During size separation, movement ‘of particles can be enhanced by one of the following modes. A. Agitation B. Attrition C. Gravitation D. Mixing . Brushing method hastens the movement of one of the following materi- als. ‘A. Coarse materials B. Dry materials C. Light materials D. Sticky materials . Flywheel is used to enhance the motion of particles by one of the following modes. A. Brushing mode B. Centrifugal mode C. Gyration mode D. Oscillation mode . Which equipment is used for sieve analysis? A. Alpine airjet sieve B. Cyclone separator C. Rotex screen D. Shaking screen Fluidised state is NOT used in one of the following equipment. A. Air separator B. Alpine sieve C. Cyclone separator D. Rotex screen Which is the disadvantage of the sieve shaker method? A. Attrition B. Capacity limited C.. Expensive equipment D. Tedious . In cyclone separator, the separation depends on: A. Density and shape B, Shape and surface area C. Size and density D. Surface texture and size . In air separator, centrifugal force for circulation of air is applied by one of the following ways. A. Applying vacuum B. Atomizing air C. Pumping D. Rotating blades ~ 68 20. PHARMACEUTICAL ENGINEERING : UNIT OPERATION . Which is the term used to describe the materials that remains on given screening surface? A Medium size material B. Minus material C. Neutral material D. Plus material . Which one of the following aids in size separation of sieve shi machine? A. Agitation B. Brushing C. Centrifugal force D. Shearing force . Which is the disadvantage of Alpine airjet sieve method? A. Mesh gets blocked B. Method does not give reproducible results C. Not suitable for fine powder D. Method is tedious |. Which are the following forces used in cyclone separator for size sep tion of particles? A. Adhesive forces B. Centrifugal forces C. Cohesive forces D. Shearing forces . A soreen that sharply separates the feed mixture is called: A. Actual screen B. Ideal screen C. Real screen D. Virtual screen . Choose one of the following statements do NOT suit to sieve shaker. A. Apertures get clogged B. Attrition causing size reduction C. Lower limit of particle size is 50 pm D. Method is tedius Choose the equipment in which filtering period and shaking period | alternatively observed. A. Air separation B, Bag filter C. Cyclone filter D. Bortclone Each question carries 2 marks . Name the standards of screens used in pharmaceutical practice, . What are standard sieves? |. Differentiate i¢eal and actual screens. }. List the specifications and standards for sieves, Explain the term blinding of screen. How is it prevented? . What are various grades of coarse powders? Define them. 1. Give the classification of fine powders with definitions. . What are the advantages of expressing sieves by a sieve number over th nominal size of aperture? . Differentiate the terminology, nominal size of aperture and nomio! diameter of the wire. Ch-2 10. 44. 12. 13. 14. 15. 16. SIZE SEPARATION 69 What are the uses of screen analysis? How is it expressed? List the methods of sieve analysis used for testing the powders. Give their relative advantages. What is the difference between sedimentation and elutriation? ‘What is the difference between free settling and hindered settling? State the term ‘elutriation’. Explain its applications and advantages. What is the difference between static and moving liquid methods of elutriation? Compare the methods of sieving and classification in terms of their utility. question carries 5 marks . Explain the working of a cyclone separator and its usefulness. . Describe the method of size separation using the Rotex shaker screen. Explain various grades of powders official in pharmacopeeia. . Give details about the various standards fixed by the pharmacopeeia for sieves. . Describe the specifications of standard sieves as per IP. . Explain the concept of settling behaviour using water with a suitable example. . Explain the behaviour of slurry setting Cd thickeners with a suitable diagram. .. Describe the principle, construction and working of a double cone classi- fier with the help of suitable diagram. . Explain the methods of size separation using water. |. Explain the methods of separation of particles in a powder using air as a Eech LL . Explain the principles of sedimentation of particles using liquid as a medium. . Explain the specific uses and applications of a scrubber. Draw the sketch of the equipment. question carries 10 marks Describe one industrial method for size separation of a powder and its applications.

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