A PRACTICAL MANUAL OF PHARMACEUTICAL ENGINEERING

Transcription

1 A PRACTICAL MANUAL OF PHARMACEUTICAL ENGINEERING

2

3 A PRACTICAL MANUAL OF PHARMACEUTICAL ENGINEERING P.S. SONA M Pharma Associate Professor, Department of Pharmaceutics Parul Institute of Pharmacy, Limda, Waghodia Vadodara, Gujarat UNIVERSITY SCIENCE PRESS (An Imprint of Laxmi Publications Pvt. Ltd.) BANGALORE CHENNAI COCHIN GUWAHATI HYDERABAD JALANDHAR KOLKATA LUCKNOW MUMBAI RANCHI INDIA USA GHANA KENYA

4 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 A PRAC MAN PHARMA ENGG-SON ISBN Price: ` 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. All trademarks, logos or any other mark such as Vibgyor, USP, Amanda, Golden Bells, Firewall Media, Mercury, Trinity, Laxmi appearing in this work are trademarks and intellectual property owned by or licensed to Laxmi Publications, its subsidiaries or affiliates. Notwithstanding this disclaimer, all other names and marks mentioned in this work are the trade names, trademarks or service marks of their respective owners. Published in India by UNIVERSITY SCIENCE PRESS (An Imprint of Laxmi Publications Pvt. Ltd.) 113, GOLDEN HOUSE, DARYAGANJ, NEW DELHI , INDIA Telephone : , Fax : , C info@laxmipublications.com Printed at: Branches & Bangalore & Chennai , & Cochin , & Guwahati , & Hyderabad , & Jalandhar & Kolkata & Lucknow & Mumbai , & Ranchi

5 Dedication Dedicated to my parents and my daughter

6

7 PREFACE This book has been written with an intention to cover all the possible experiments which are to be conducted in the pharmaceutical engineering laboratory at the under graduate level. I have tried to incorporate all the experiments suggested under pharmaceutical engineering by different universities. Though I have taken long time to complete this book, I have no regrets because the designed experiments are all practically performed in the laboratory by my students and that has given me ample chance to improve the quality of the experiments. During this period I could observe the difficulties of the students in collecting primary informations which are the part of the main experiments. The usage of vernier calipers, screw gauge, colorimetry, different standard value like specific heat and radiation constants of different materials, and conversion of units are examples. I have included all such informations in the appendices so that students are benefited to get them in a single book. Today I am so proud to present before you my book A Practical Manual of Pharmaceutical Engineering. Hope that it will be well accepted by the pharmaceutical science fraternity. The suggestions are encouraged and acknowledged. Author (vii)

8 ACKNOWLEDGEMENT I express my indebtedness to my husband Mr. C. Muthulingam who has been an inspiration and support for completing the book. I extend my sincere thanks to my students of Grace College of Pharmacy (First Batch) and Ramgopal College of Pharmacy (First and Second Batch) for their support. I thank my brother Mr. Sujith. P.S, B Tech, for his valuable suggestions. I express my gratitude to publisher for publishing my book. Author (viii)

9 CONTENTS Preface Acknowledgement vii viii EXPERIMENT 1 Determination of Radiation Constant of Metal Cylinder 1 EXPERIMENT 2 Determination of Radiation Constant for Painted and Unpainted Metal Cylinders 6 EXPERIMENT 3 Determination of Overall Heat Transfer Co-efficient 11 EXPERIMENT 4 Determination of Type of Flow by Reynold s Apparatus 16 EXPERIMENT 5 Determination of Flow Rate by Direct Weighing or Measuring 21 EXPERIMENT 6 Determination of Pressure Difference During Liquid Flow Using Simple Manometer 23 EXPERIMENT 7 Determination of Pressure of Gas Flow by U Tube Manometer 26 EXPERIMENT 8 Determination of Pressure of Gas Flow by Inclined Manometer 29 EXPERIMENT 9 Determination of Flow of Fluid Rotameter 32 EXPERIMENT 10 Determination of Frictional Pressure Loss During Fluid Flow Through a Pipe 35 EXPERIMENT 11 Determination of Coefficient of Discharge by Orifice Meter 39 EXPERIMENT 12 Determination of Coefficient of Discharge by Venturi Meter 45 EXPERIMENT 13 Determination of Efficiency of a Centrifugal Pump 51 EXPERIMENT 14 Determination of Effect of Number of Balls on Grinding Operation of Ball Mill 56 EXPERIMENT 15 Determination of Effect of Time on Grinding Operation of a Ball Mill 60 EXPERIMENT 16 Size Reduction-Homogenization 63 EXPERIMENT 17 Particle Size Separation by Sieveing 69 EXPERIMENT 18 Particle Size Separation Beaker Decantation 73 EXPERIMENT 19 Particle Size Separation by Sedimentation Method 77 EXPERIMENT 20 Mixing Determination of Uniformity Index 83 (ix)

10 (x) EXPERIMENT 21 Liquid-Liquid Mixing Determination of Uniformity of Mixing 88 EXPERIMENT 22 Determination of Critical Point of Settling Sedimentation 91 EXPERIMENT 23 Sedimentation Effect of Sedimentation Rate on Concentration 94 EXPERIMENT 24 Determination of Temperature Humidity Index THI 97 EXPERIMENT 25 Determination of Humidity by Psychrometric Method 100 EXPERIMENT 26 Determination of Humidity Dew Point Method 104 EXPERIMENT 27 Determination of Relative Humidity by Wet Bulb Depression Method 108 EXPERIMENT 28 Determination of Relative Humidity by Sling Psychrometer 111 EXPERIMENT 29 Drying Determination Rate of Drying 114 EXPERIMENT 30 Drying Comparison of the Drying Pattern of Solids 118 EXPERIMENT 31 Determination of Equilibrium Moisture Content 121 EXPERIMENT 32 Filtration Effect of Filter Aids on Rate of Filtration 124 EXPERIMENT 33 Effect of Filter Aid Concentration on Rate of Filtration 127 EXPERIMENT 34 Evaluation of Filter Media 130 EXPERIMENT 35 Centrifugation Determination of the Yield Stress of Centrifuged Cake 133 EXPERIMENT 36 Centrifugation Determination of Centrifugal Effect 137 EXPERIMENT 37 Simple Distillation Ethanol Water System 140 EXPERIMENT 38 EXPERIMENT 39 Determination of Boiling Point of the Components in a Liquid Mixture by Simple Distillation 146 Determination of Distillation Range in a Liquid Mixture of Ethanol Water Simple Distillation 149 EXPERIMENT 40 Steam Distillation Determination of Efficiency of Distillation 152 EXPERIMENT 41 Vacuum Distillation Effect of Vacuum on Distillation of Aspirin Reaction Mixture 156 EXPERIMENT 42 Determination of Number of Theoretical Plates Fractional Distillation 162 EXPERIMENT 43 Crystallization by Cooling 166 EXPERIMENT 44 Crystallization Verification of Material Balancing Equation 170 EXPERIMENT 45 Evaporation Evaluation of Factors Affecting Rate of Evaporation 173 EXPERIMENT 46 Evaporation Verification of Material Balancing Equation 179

11 (xi) EXPERIMENT 47 Evaluation of Materials Used in Pharmaceutical Packaging Corrugated Board 182 EXPERIMENT 48 Evaluation of Packaging Material Glass 185 EXPERIMENT 49 Determination of Rate of Corrosion Total Immersion Test 190 EXPERIMENT 50 Determination of Factors Affecting Corrosion Rate Total Immersion Test 194 APPENDICES 198 REFERENCES 238 INDEX 239

12

13 Determination of Radiation Constant of Metal Cylinder 1 EXPERIMENT 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. 1

14 2 A Practical Manual of Pharmaceutical Engineering Radiative cooling is described by Stefan-Boltzmann Law which states that the rate of heat loss per unit surface area of a body at temperature T is proportional to T 4 T s 4 (T s is temperature of the surrounding). The rate of heat loss due to combined convection and radiation can be determined by the following equation. M dt dt h1 = S C h2 (T T air ) + S C (T 4 T s 4 ) (Eq : 1.1) Where, M = Mass of the body (Kg) dt/dt = The rate of change of temperature (Rate of heat loss) (K/sec) h 1 = Heat transfer coefficient for pure convection. (W/ m 2.K) S= Surface area of the hot body (m 2 ) T= Temperature of the metal surface (K) T air = Temperature of the surroundings (K) T s = Temperature of the surroundings h 2 = Radiation constant (W/m 2.K 4 ) C = Specific heat of the metal. (J/kg K) All the other values are determined experimentally and substitute in the equation to determine the radiation constant of the metal. Digital thermometer Metal cylinder Hotplate Fig. 1.1: Hot pad Arrangement for the determination of radiation constant. PROCEDURE 1. Take a metal cylinder (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 a thermometer would fit nicely) and clean the surfaces. 2. Find out the surface area and weight of the cylinder (Refer appendix V). 3. Keep it over a heating plate. (Bunsen burner-tripod stand arrangement can also be used) 4. Insert the digital thermometer to the hole present in the cylinder. (A simple 360 C thermometer can also be used) 5. Switch on the hot plate. 6. Heat the metal to a maximum temperature. (Depending upon the thermometer maximum)

15 Determination of Radiation Constant of Metal Cylinder 3 7. Remove it carefully from the heating source with the help of a tong S. 8. Place it over a hot pad or on the table to minimize the heat loss by conduction. 9. The temperature of the metal cylinder starts to decrease. 10. The temperature readings are noted at an interval of 2 min. 11. Take the readings till the hot body reaches the normal room temperature. 12. The readings are tabulated. 13. Find out the dt/dt. 14. Plot the cooling curve by taking time in min on X axis and temperature on Y axis (Fig. 1.2). 15. Plot another Graph by taking Temperature in C in X axis and dt/dt in Y axis (Fig. 1.3) 16. Find out the slope of the plot. (Slope = h 1 S/C) 17. Calculate the co-efficient of convection. 18. Substitute the values in the equation to get the radiation constant (h 2 ). 19. The same procedure can be used for the determination of radiation constant of cylinders/ cubes made up of other metals. OBSERVATIONS & CALCULATIONS Diameter of the cylinder (d) =. cm =... m Radius of the cylinder (r) = D/2 =. m. Height of the cylinder (h) =. cm =.. m Surface area of the cylinder (S) = 2p r(r + h) =...m 2 Mass of the body =. gm =.kg Room temperature =. C = K Specific Heat of the metal ( C) =.J/Kg.K (Refer the appendix XIII) Table 1.1: Data for the Construction of Cooling Curve Sl No Time in min Temperature in C

16