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A Practical Manual of Pharmaceutical Engineering

By: P.S.Sona
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A Practical Manual of Pharmaceutical Engineering provides 50 relevant experiments  covering  almost all the topics of pharmaceutical engineering like heat transfer, mass transfer, flow of fluids, size reduction, size separation, mixing, sedimentation, humidity and air conditioning, drying, filtration, centrifugation, distillation, crystallization, evaporation, packaging materials and corrosion. The designed experiments in the book provide simple demonstrations for the conceptual understanding of pharmaceutical engineering.

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Preface_F

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A PRACTICAL MANUAL OF PHARMACEUTICAL ENGINEERING

Copyright © by Laxmi Publications (P) Ltd.

All rights reserved including those of translation into other languages. In accordance with the Copyright (Amendment) Act, 2012, no part of this publication may be reproduced, stored in a retrieval system, or transmitted in any form or by any means, electronic, mechanical, photocopying, recording or otherwise. Any such act or scanning, uploading, and or electronic sharing of any part of this book without the permission of the publisher constitutes unlawful piracy and theft of the copyright holder’s intellectual property.

If you would like to use material from the book (other than for review purposes), prior written permission must be obtained from the publishers.

Printed and bound in India

Typeset at Shubham Composer

First Edition: 2015

UPE-9744-195-A PRAC MAN PHARMA ENGG-SON

ISBN 978-93-83828-43-2

Price: ` 195.00

Limits of Liability/Disclaimer of Warranty: The publisher and the author make no representation or warranties with respect to the accuracy or completeness of the contents of this work and specifically disclaim all warranties. The advice, strategies, and activities contained herein may not be suitable for every situation. In performing activities adult supervision must be sought. Likewise, common sense and care are essential to the conduct of any and all activities, whether described in this book or otherwise. Neither the publisher nor the author shall be liable or assumes any responsibility for any injuries or damages arising herefrom. The fact that an organization or Website if referred to in this work as a citation and/or a potential source of further information does not mean that the author or the publisher endorses the information the organization or Website may provide or recommendations it may make. Further, readers must be aware that the Internet Websites listed in this work may have changed or disappeared between when this work was written and when it is read.

 

Ch_1_F

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Determination of Radiation Constant of Metal Cylinder

EXPERIMENT

1

1

DETERMINATION OF RADIATION

CONSTANT OF METAL CYLINDER

AIM

To determine the radiation constant of the given metal cylinder.

To demonstrate the cooling pattern during natural cooling of a hot body.

REQUIREMENTS

Metal cylinder

(1)

(made up of any metal for example iron, aluminum, brass, copper of 1 inch diameter, 1.5 inch length which is having drilled hole half way down, so that thermometer would fit nicely).

Hotplate

(1)

Digital thermometer

(1)

Vernier calipers

(1)

Weighing balance

(1)

Weight box

(1)

Tongs

(1)

Hot pad

(1)

PRINCIPLE

Heat transfer process plays an important role in science and engineering. When two objects at different temperature are brought into contact, heat flow occurs from the object having higher temperature to the object having lower temperature. The total heat loss from the body to its surroundings often includes appreciable losses by conduction, convection, and radiation. If the body is not in contact with any surfaces the heat transfer by conduction is neglected. So the heat transfer is mainly by convection and radiation. The present experiment demonstrates the pattern of cooling of a hot body by combined convection and radiation.

 

Ch_2_F

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Determination of Radiation Constant for Painted and Unpainted Metal Cylinders 7

M

hS hS dT

= 1 (T � Tair) + 2 (T4 � Ts4 )

C

C dt

� (Eq: 2.1)

Where,

M = Mass of the body (Kg) dT/dt = Rate of change of temperature (Rate of heat loss) (K/sec) h1 = Heat transfer coefficient for pure convection (W/ m2.K)

S = Surface area of the hot body (m2)

T = Temperature of the metal surface (K)

T air = Temperature of the surroundings (K)

Ts = Temperature of the surroundings (K) h2 = Radiation constant (W/m2.K4

C = Specific heat of the metal (J/kg K)

Substitute all other known parameters in the equation to get the radiation constant.

The present experiment explains the effect of color on the radiation constant and on the cooling pattern.

All warm objects emit electromagnetic radiation. Hotter objects emit more radiation. Objects that emit a lot will quickly cool. Objects that don�t emit as much will stay warm longer. Black will absorb more than white, shiny objects will reflect energy and not absorb it. Color also affects emission. For objects near room temperature, which emit radiation in the far infrared part of the spectrum, most are black�that is, they are good absorbers and good emitters. For instance, human skin, regardless of color, is a very good absorber and emitter of far infrared. No matter what color your skin is, you are black in the infrared. The same is true of fabrics and of painted surfaces. All colors of cloths and all colors of paints are black in the infrared; they absorb and emit quite nicely.

 

Ch_3_F

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12 A Practical Manual of Pharmaceutical Engineering q = mc cpc (Tcb � Tca)

Where, q mc cpc

Tcb

Tca

� (Eq: 3.1)

= Rate of heat transfer

= Mass flow rate of cold water (liter/sec)

= Specific heat of cold water (J/kg)

= Temperature of the leaving cold water (°C)

= Temperature of the entering cold water (°C)

Rate of heat transfer, based on the area of heating surface (tube) can be determined as follows, dq /da = UDT

� (Eq: 3.2)

dq/da = Local flux, DT = Over all local temperature difference (Th � Tc , where Th is the average temperature of the hot fluid, Tc is the average temperature of the cold fluid)

U = Local overall heat transfer coefficient

Since DT can vary considerably from point to point along the tube, the heat flux is proportional to DT. To apply this equation for the total surface area, the equation must be integrated. This can be done with some simple assumption that, the overall coefficient U is a constant, the specific heat of hot and cold fluids are constant, the flow is steady in both parallel or counter current. After integration and proper arrangement the equation becomes, q=

 

Ch_4_F

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16 A Practical Manual of Pharmaceutical Engineering

EXPERIMENT

4

DETERMINATION OF TYPE OF FLOW

BY REYNOLD’S APPARATUS

AIM

To determine the Reynold�s number by Reynold�s apparatus.

To demonstrate the type of flow (laminar, turbulent, or transition zone).

To determine the critical velocity of flow of a liquid.

REQUIREMENTS

Reynold�s apparatus

(1)

Pump

(1)

Water tank

(1)

Colored solution (KMnO4)

PRINCIPLE

Fluid can flow through a pipe in two different ways. At low flow rates the pressure drop in the fluid increases directly with the fluid velocity and at high rates it increases much more rapidly. At low velocity the fluid will travel as layers and there is no mixing of the layers of the fluid. This type of flow is called as laminar flow. At high velocity this pattern of flow is disturbed and there will be a complete mixing of the layers and production of turbulence. This type of flow can be called as turbulent flow.

The distinction between the two flows can be demonstrated with the help of Reynold�s experiment. Reynold�s experiment uses a transparent glass tube with central nozzle for the introduction of colored solution. Water is allowed to pass through the glass tube at low velocity and through the nozzle colored solution is also introduced. At low velocity it is found that the colored solution is traveling as a straight line as there is no mixing of the layers. By slowly increasing the velocity of the flow a particular velocity is reached where the thread of color become wavy and gradually

 

Ch_5_F

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Determination of Flow Rate by Direct Weighing or Measuring

EXPERIMENT

21

5

DETERMINATION OF FLOW RATE BY

DIRECT WEIGHING OR MEASURING

AIM

To determine the flow of fluid by direct weighing or measuring.

REQUIREMENTS

Long tube connected to a water inlet

(1)

Measuring tank

(1)

Measuring cylinder of capacity (1000 ml)

(1)

Weighing balance

(1)

Stop clock

(1)

PRINCIPLE

One of the methods of determination of flow rate is by direct weighing or measuring. In this method no other parameters are considered for calculating the flow rate. The amount (volume) of the liquid coming out from the pipe up to a particular time is determined and from the value, the volume of liquid passing through the pipe per min is calculated. Same way the weight of the liquid collected for different time Interval is determined and the flow rate in weight per min or sec is found out.

PROCEDURE

1.

2.

3.

4.

5.

Arrange a pipe line (straight) of known length.

Attach one end of the pipe line to the water tap with suitable arrangements.

The opposite end of the pipe is fixed into a measuring cylinder.

 

Ch_6_F

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Determination of Pressure Difference during Liquid Flow Using Simple Manometer

EXPERIMENT

DETERMINATION

23

6

PRESSURE

DIFFERENCE DURING LIQUID FLOW

USING SIMPLE MANOMETER

OF

AIM

To determine the pressure difference in a flow of liquid through a pipe with the help of simple Utube manometer.

REQUIREMENTS

Orifices meter or venturi meter assemble

(1)

Pump

(1)

Manometer

(1)

Water

PRINCIPLE

A manometer, when used properly, is a very accurate instrument for the determination of pressure difference during fluid flow. The U-type manometer is a primary standard due to its inherent accuracy and simplicity of operation. The manometer has no moving parts subject to wear, age, or fatigue. U tube Manometer consists of two limbs which are attached to the pipe through which the fluid is flowing. Both the limbs are filled with mercury in equal quantity. If there is no pressure difference both the limbs show same height of the mercury level on the scale. If any pressure difference occurs between the limbs, mercury level in the limb will differs and shows increased or decreased scale readings. The pressure difference can be determined by the equation,

 

Ch_7_F

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26 A Practical Manual of Pharmaceutical Engineering

EXPERIMENT

7

DETERMINATION OF PRESSURE OF

GAS FLOW BY U TUBE MANOMETER

AIM

To determine the pressure of the gas flow using U tube manometer.

REQUIREMENTS

U tube manometer

(1)

Pipe connections

(2)

Gas source

(1)

Acetone

Mercury

PRINCIPLE

Simple U tube Manometer consists of a U shape transparent tube of height 10 mm or more, U tube manometer can measure both positive and negative pressures. One of the limbs of U-tube manometer is longer than the other and is kept open to the atmosphere. This is called as open limb. The other limb is connected to the pressure tapping. The mercury level (bottom of the concave meniscus of the mercury) in each limb is read and the difference is calculated. This is called as deflection. This will be the pressure of the flow of the gas. With the help of conversion factors, the pressure in mm

Hg can be converted into other units (Refer the appendix I & II).

The open-tube manometer is used to measure the pressure of a gas in a container. The pressure of the gas is determined by finding out the h (the difference in mercury levels) in units of torr or mmHg. During the experiment one of the limbs is connected to the gas source and the other limb kept open. The Atmospheric pressure pushes the mercury from one direction, and the gas flow from the container from the other direction. So for the determination of the gas pressure during flow can be determined using the equations,

 

Ch_8_F

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Determination of Pressure of Gas Flow by Inclined Manometer 29

EXPERIMENT

8

DETERMINATION OF PRESSURE

OF GAS FLOW BY INCLINED

MANOMETER

AIM

To determine the pressure of flow of gas by inclined manometer.

To find out the gas pressure at different gas flow rate.

REQUIREMENTS

Inclined manometer

(1)

Pipe connections

(1)

Gas source

(1)

Scale

(1)

Protractor

(1)

PRINCIPLE

Inclined manometer is used to determine small differences in pressure during fluid flow. In this type of manometer, one of the legs is inclined at angle a and the liquid in the limb should move a considerable distance for a small difference in pressure. The inclined manometer or slant manometer is an enlarged leg manometer with its measuring leg inclined to the vertical axis by some angle.

The inclination is done to expand the scale & thereby to increase the sensitivity. Commonly used

Manometric liquids in inclined manometer are:

1. Mercury: It has low freezing point � 38 °F & high boiling point 675 °F but it corrodes many metal & it is poisonous & expensive.

 

Ch_9_F

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32 A Practical Manual of Pharmaceutical Engineering

EXPERIMENT

9

DETERMINATION OF FLOW

OF FLUID—ROTAMETER

AIM

To determine the flow of fluid through a pipe using Rotameter.

REQUIREMENTS

Rotameter

(1)

Pipe connection

(2)

Measuring cylinder

(1)

Water

PRINCIPLE

Rotameter consists of a tapered glass tube with the smallest diameter at the bottom. The tube contains a freely moving Float/plummet which rests on a stop at the base of the tube. When the fluid is flowing, the float rises until its weight is balanced by the up thrust of the fluid and reaches a position of equilibrium, this position then indicates the rate of flow. Floats can be of many shapes, but spheres and ellipsoids being the most common. The float is shaped so that it rotates axially as the fluid passes. Readings are usually taken from the top of the float.

The rotameter�s operation is based on the variable area principle: Fluid flow raises the float in a tapered tube, increasing the area for passage of the fluid. The greater the flow, the higher the float is raised. The height of the float is directly proportional to the flow rate. With liquids, the float is raised by a combination of the buoyancy of the liquid and the velocity head of the fluid. With gases, buoyancy is negligible, and the float responds to the velocity head alone.

 

Ch_10_F

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Determination of Frictional Pressure Loss during Fluid Flow through a Pipe

EXPERIMENT

35

10

DETERMINATION OF FRICTIONAL

PRESSURE LOSS DURING FLUID

FLOW THROUGH A PIPE

AIM

To determine the pressure loss due to friction during the flow through a pipe.

To determine the relative roughness of the pipe using the Moody�s diagram.

To determine the fanning frictional Factor.

REQUIREMENTS

Long PVC pipe connected to a tap/long PVC pipe connected to a pump with regulating valve (1)

Collecting tank (measuring tank)

(1)

Stop clock

(1)

Long scale

(1)

Vernier calipers

(1)

PRINCIPLE

As the Fluid flows through a pipe from a point A to B the pressure decreases due to frictional loss between the flowing liquid and the pipe. The extent of pressure loss designated in feet depends on many factors. These factors include liquid flow rate, liquid specific gravity and viscosity, diameter of pipe (inside), length, and internal conditions of the pipe( smooth -rough). In order to find out the frictional loss, the fanning�s frictional equation is used,

 

Ch_11_F

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Determination of Coefficient of Discharge by Orifice Meter 39

EXPERIMENT

11

DETERMINATION OF COEFFICIENT OF

DISCHARGE BY ORIFICE METER

AIM

To demonstrate the use of orifice meter as flow meter.

To determine the coefficient of discharge.

To study the effect of flow rate on Reynolds number of the liquid.

REQUIREMENTS

Orifice Meter Assemble

(1)

Stop clock

(1)

Water supply

Drain

PRINCIPLE

An orifice meter consists of a flat circular plate with circular hole called orifice which is concentric with the pipe axis. The orifice meter is fitted with the pipe line. If a constriction is placed in a closed channel carrying a stream of fluid there will be increase in the velocity and therefore increase in kinetic energy. According to the Bernoulli�s theorem the total energy at any given point during flow is a constant. So because of the increment in the kinetic energy the pressure energy at the constriction is reduced to balance the increment in the kinetic energy. Rate of discharge from the constriction can be calculated by knowing this pressure reduction, the area at the constriction, the density of the fluid, and the coefficient of discharge.

 

Ch_12_F

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Determination of Coefficient of Discharge by Venturi Meter 45

EXPERIMENT

12

DETERMINATION OF COEFFICIENT OF

DISCHARGE BY VENTURI METER

AIM

To demonstrate the use of venturi meter.

To determine the coefficient of discharge during fluid flow.

To study the effect of flow rate on Reynold�s number of liquid.

REQUIREMENTS

Venturi meter Assemble

(1)

Stop clock

(1)

Water supply

Drain

PRINCIPLE

To control the industrial process, it is essential to know the material entering and leaving the process. If materials are transported in the form of fluids, the determination of flow rate is so important. Venturi meter is one of the flow meters commonly used in the industry for the determination of flow rate of fluids.

A venturi meter consist of a short conical inlet section which leads to throat section then to a long discharge cone. Manometer connections are done at the start of the inlet section and at the throat of the venturi meter. When the fluid is entering to the constricted portion (throat of venturi) there will be an increase in the velocity, and hence increase in the kinetic energy. So according to the Bernoulli�s theorem there should be a reduction in pressure energy. This pressure drop in the cone is used to determine the flow rate. It is also desirable to know the density of the fluid flowing, diameter ratio, and venturi coefficient of discharge. The coefficient of discharge is determined experimentally. For a well designed venturi meter this will be about 0.98 for pipe diameter of 2-8 inches and 0.99 for large sizes.

 

Ch_13_F

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Determination of Efficiency of a Centrifugal Pump 51

EXPERIMENT

13

DETERMINATION OF EFFICIENCY

OF A CENTRIFUGAL PUMP

AIM

To determine the co efficient of discharge of a centrifugal pump.

To determine the overall efficiency of centrifugal pump.

To determine the efficiency of the centrifugal pump.

REQUIREMENTS

The centrifugal pump assemble

(1)

Stop watch

(1)

Energy meter

(1)

PRINCIPLE

Pump is a device which converts mechanical energy to hydraulic energy. Hydraulic energy is in the form of Pressure energy. In a centrifugal pump the mechanical energy is converted into pressure energy by centrifugal force.

A Centrifugal Pump is a roto dynamic pump that uses a rotating impeller to increase the pressure of a fluid. They are commonly used to move liquids through a piping system. Its purpose is to convert energy of a prime mover (an electric motor or turbine) first into velocity or kinetic energy and then into pressure energy of a fluid that is being Pumped. The energy change occurs by virtue of two main parts of the pump, the impeller and the volute or diffuser. The impeller is the rotating part that converts driver energy into the kinetic energy. The volute or diffuser is the stationary part that converts the kinetic energy into pressure energy. The overall system efficiency is dependent on motor efficiency, pump efficiency (velocity of the impeller, impeller diameter, number of blades etc) and the total head developed.

 

Ch_14_F

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56 A Practical Manual of Pharmaceutical Engineering

EXPERIMENT

14

DETERMINATION OF EFFECT OF

NUMBER OF BALLS ON GRINDING

OPERATION OF BALL MILL

AIM

To study the effect of number of balls on grinding operation of a ball mill.

REQUIREMENTS

Ball mill

(1)

Balls (same size and density)

(Quantity sufficient)

Sieve 120 mesh

(1)

Weighing balance

(1)

Butter paper

(1)

Spatula

(1)

Weighing box

(1)

Sugar

PRINCIPLE

Ball mill consist of a horizontally rotating hollow cylinder with length slightly greater than its diameter. The mill is partially filled with balls of steel or pebbles. In ball mill size reduction happens by impact and attrition.

The speed of rotation of the mill is important, as the slow speed of rotation contribute only a sliding action and high speed a centrifugal action. At both this speed, no significant size reduction happens. The ideal speed of a ball mill is a speed at which the balls just begins to centrifuge within the mill contributing a cascading action and hence a significant size reduction. The critical speed of rotation can be determined by the following equation.

 

Ch_15_F

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60 A Practical Manual of Pharmaceutical Engineering

EXPERIMENT

OF

15

DETERMINATION OF EFFECT

TIME ON GRINDING OPERATION

OF A BALL MILL

AIM

To study the effect of time on grinding rate of a ball mill.

REQUIREMENTS

Ball mill

(1)

Balls (same size and density)

(12)

Sieve 120 or 85 mesh

(1)

Weighing balance

(1)

Butter paper

(1)

Spatula

(1)

Weighing box

(1)

Sugar

PRINCIPLE

Ball mill consist of a horizontally rotating hollow cylinder shape with the length slightly greater than its diameter. The mill is partially filled with balls of steel or pebbles. In ball mill size reduction happens by impact and attrition. The speed of rotation is so important, as the slow speed of rotation contribute only a sliding action and high speed a centrifugal action. At both this speed, no significant size reduction happens. The optimum speed of a ball mill is a speed at which the balls just begins to centrifuge within the mill contributing a cascading action and hence a significant size reduction.

The optimum speed of rotation can be determined by the following equation,

 

Ch_16_F

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64 A Practical Manual of Pharmaceutical Engineering mortar and pestle, the mechanical energy given is comparatively less so that the dispersed globules are comparatively larger and not uniform in size. This will leads to the instability of emulsion while storage.

Homogenization is the process of converting two immiscible bulk phase liquids into an emulsion (primary homogenization) or of reducing the size of the droplets in a pre-existing emulsion

(secondary homogenization) this can be achieved by passing the fluid through restricted orifices under high pressure. e.g., silverson emulsifier.

The high speed rotation of the rotor blades creates a powerful suction which draws the liquid into the work head. The materials are subjected to intense shear in the confined area of the work head. Agglomerates are broken down in the gap between the rotor blades and stator wall. A lump free mixture is rapidly obtained. The product is forced out of the stator as fresh material is drawn into the work head. A circulatory mixing cycle develops in which all the material passes through the Silverson work head produces efficient mixing and desirable size reduction.

 

Ch_17_F

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Particle Size Separation by Sieveing 69

EXPERIMENT

17

PARTICLE SIZE SEPARATION

BY SIEVEING

AIM

To perform the particle size separation of the given sample and determine the arithmetic mean of the given sample.

REQUIREMENTS

Sieves of different mesh size

(Quantity sufficient)

Mechanical shaker

(1)

Weighing balance

(1)

Weighing box

(1)

Butter paper

Powder sample

PRINCIPLE

Size separation can be defined as a unit operation that involves the separation of various sizes of particles into two or more portions by means of screening surfaces. Performance of size reduction equipments, or crushing and grinding equipments involve the determination of the amount of material of different size present after the process. The only general and simple method for this is to determine the fraction of the sample that will go through a screen with known size of openings. A screen analysis of the sample is performed by placing a sample on the coarsest of a set of standard screens. Below this, the screens are arranged in the order of decreasing size of the openings in the mesh. The total assemble is shaken with help of a mechanical oscillator or manually, for a definite length of time and the material collected on each sieve is removed and weighed. The result obtained can be represented graphically.

 

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