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Chapter 1 - The Pilot Plant
The Role of the Pilot Plant 1-2
Major Factors in Scale-Up 1-3
12 Things to Do During Process Scale-Up 1-6
12 Things to Avoid During Process Scale-Up 1-7
Developing Scalable Reactions 1-8
The Role of Calorimetry and Process Safety Screening 1-11
The Haz-Op 1-12
The Batch Checklist 1-14
The Process Flow Diagram 1-15
The Batch Record 1-16
The Campaign Report 1-17
Notes on GMP 1-18

Chapter 2 - Equipment and Operations
The Pilot Plant Equipment Train 2-2
Notes on Equipment Selection, Installation and Maintenance 2-3
Reactors 2-4
Vessel Agitation 2-8
Charging Raw Materials 2-11
Reaction Control 2-13
Sampling for Reaction Monitoring 2-15
Workup 2-16
Partition Coefficient and Extraction Efficiency 2-17
Polish Filtration / Decolorization / Water Removal 2-18
Batch Distillation 2-19
Crystallization 2-21
Product Isolation 2-24
Filtration Scale-Up 2-27
Product Drying 2-29
Scrubbers 2-33
Reactor and Equipment Cleaning 2-34

Chapter 3 - Liquid Handling
Introduction and Terminology 3-2
Pump Sizing and Selection 3-4
Pump Installation and Operation 3-5
Rotary Pump Troubleshooting Guide 3-6
Major Pump Types 3-7
Diaphragm Pump Troubleshooting Guide 3-8
Peristaltic Pump Tubing Sizing and Flowrate Guides 3-13
Pipe, Drawn Tube and Fittings 3-14
Flanges and Gaskets 3-19
Valves 3-21
Hose and Hose Fittings 3-23
Liquid Velocity and Pressure Effects 3-24
Viscosity Effects 3-26
Standard O-Ring Size Chart 3-28
Rubber Stopper Sizes 3-29
Ground Glass Joint Sizes 3-29
Capacity of Liquid Storage Tanks 3-30
Storage Drum and Shuttle Data 3-32

Chapter 4 - Heat Transfer
Heat Transfer in Stirred Tank Reactors 4-2
Typical Batch Cooling Profiles 4-4
Reactor Heat Transfer Coefficients 4-5
Experimental Determination of Heat Transfer Coefficient 4-7
Heat Exchanger Fundamentals 4-8
Example Heat Exchanger Problem 4-9
Chart for Estimating Log Mean Temperature Difference 4-10
Temperature Control Units 4-11
System Start-up and Operation 4-12
Tips on Using Heat Transfer Fluids in TCUs 4-13
Heat Transfer Fluid Selection 4-14
Specific Heat of Various Heat Transfer Fluids vs. Temperature 4-15
Useful Temperature Ranges and Properties of Commercial HTF’s 4-16
Notes on the Use of Glycol HTFs 4-18
Specific Gravity of Aqueous Glycol Solutions 4-19
Freezing Points of Aqueous Glycol Solutions 4-20
Boiling Points of Aqueous Glycol Solutions 4-21
Specific Heats of Aqueous Glycol Solutions 4-22
Viscosity of Aqueous Ethylene Glycol Solutions 4-23
Freezing Points of Brines 4-24
Steam Pressure vs. Temperature 4-25
Notes on Process Chillers 4-26
Approximate Chiller Capacity 4-28
Effect of Condenser Cooling Water Temperature 4-28

Chapter 5 - Electricity and Istrumentation
Notes on Electrical Safety 5-2
Electric Power Basics 5-3
Wire Data 5-4
Standard Resistor Color Code 5-5
Tips on Making Electrical Connections 5-5
Receptacle Data 5-6
Electrical Enclosure Data 5-7
Hazardous Location Classifications for Electrical Equipment 5-8
Intrinsically Safe Equipment 5-10
Electric Motors 5-11
Motor Nameplate Data 5-11
Typical Current Draw of Induction Motors 5-12
Common Types of Motor Enclosures 5-13
Electric Motor Troubleshooting Guide 5-14
Standard NEMA Motor Frame Sizes 5-14
Temperature Measurement 5-15
The 4-20 mA Transmitter 5-17
Pressure Measurement 5-18
Flow Measurement 5-20
Level Measurement 5-22
pH Measurement and Control 5-24
Notes on Process Control 5-26
Analog vs. Digital Control Networks 5-27
Understanding PID Controllers 5-28

Chapter 6 - Solvents
Notes on the Safe Handling of Solvents 6-2
NFPA Solvent Flammability Classifications 6-2
Relative Flammability Hazard of Selected Solvents 6-3
Notes on Solvent Selection 6-4
Some Solvents Useful for Crystallization 6-4
Notes on Solvent Properties Table 6-5
Solvent Properties Table 6-6
Solubility Map of Common Solvents 6-16
Effect of Temperature on Specific Volume 6-17
Enthalpy of Vaporization vs. Boiling Point 6-18
Effect of Temperature on Enthalpy of Vaporization 6-19
Effect of Temperature on Viscosity 6-20
Effect of Temperature on Specific Heat 6-21
Reduced Pressure Boiling Points for Some Common Solvents 6-22
Chart for Estimating Boiling Point vs. Pressure 6-23
Chart for Estimating Vapor Pressure at Elevated Temperatures 6-24
Notes on Distillation and Azeotropes 6-25
Effect of Pressure on Azeotrope Composition 6-26
Water Azeotropes of Some Common Solvents 6-27
Binary Azeotropes of Some Common Solvents 6-28
Ternary Water-Containing Azeotropes of Some Common Solvents 6-40
Solvents Limited for Pharmaceutical Use 6-44
Common Types of Denatured Ethanol 6-44
Important Temperature Dependent Properties of Water 6-45
Common Water Purification Methods 6-47
Process Water Quality Specifications 6-47
Water Conductivity and Resistivity 6-48

Chapter 7 - Compressed Gases
Notes on the Safe Handling of Compressed Gases 7-2
Special Precautions for Gaseous Hydrogen 7-3
Precautions for Cryogenic Liquids 7-3
Estimating Partial-Cylinder Contents 7-3
Common Gas Cylinder Types and Specifications 7-4
Typical Gas Cylinder Markings 7-4
Cylinder Valve Outlet Connections for Common Gases 7-6
Recommended Torque Values for CGA Outlet Connections 7-7
CGA Fitting Specifications 7-8
Metering Gases 7-9
Heating Gas Cylinders Safely 7-9
Care and Use of Gas Pressure Regulators 7-10
Physical Properties of Gases 7-11
Properties of Some Cryogenic Liquids 7-12
Gas Leak Detection 7-13
Properties of Air 7-14
Dew Point vs. Relative Humidity 7-15
Compressed Air Systems 7-16
Compressor Horsepower Requirements 7-17
Typical Compressed Air Usage Rates 7-17
Compressed Air Tank Capacity 7-18
Equivalent Cubic Feet of Compressed Air 7-18
Air Flow Through Pipes and Tubes 7-19
Pressure Drop Through Fittings for Air, Steam, or Gases 7-19
Air Flow Through Orifices 7-20
Vacuum Systems 7-21

Chapter 8- Chemical Data
Periodic Table of the Elements 8-2
Properties of Commercial Acids and Bases 8-3
pH of Common Acid and Base Solutions 8-3
Recipes for Dilute Acid/Base Solutions 8-4
pKa of Acids, Bases and Buffers 8-6
Properties and Preparation of Buffer Solutions 8-8
Some Useful Buffer Systems 8-9
Some NBS Standardized Buffers 8-9
pH Range of Some Acid-Base Color Indicators 8-9
Aqueous Solubility 8-10
General Water Solubility Rules for Inorganic Compounds 8-10
United States Pharmacopeia Definitions of Solubility 8-10
Aqueous Solubility of Selected Inorganic Compounds 8-11
Aqueous Solubility of Selected Organic Compounds 8-12
Effect of Temperature on Aqueous Solubility of Selected Compounds 8-13
Heat of Solution 8-14
Solution Density 8-15
Density of Selected Aqueous Inorganic Solutions 8-16
SpecificGravity and Density Scales 8-17
Comparison of Various Concentration Scales 8-17
Grades of Chemical Purity 8-18
Drying Agents for Solvents and Solutions 8-18
Names of Ions 8-19
Functional Groups in Organic Chemistry 8-19
Some Common Acronyms Used in Organic Chemistry 8-20
Some Common Types of Organic Reactions 8-21

Chapter 9 - Chemical Safety and Hygiene
General Notes on the Safe Handling of Chemicals 9-2
The Chemical Hygiene Plan 9-3
Material Safety Data Sheets 9-4
Classification of Hazardous Substances 9-5
Toxicity and Health 9-6
Fire Safety 9-6
Fire Extinguishers 9-7
Chemical Labeling 9-8
List of Incompatible Chemicals 9-9
Waste Effluent Disposal 9-10
Eye and Face Protection 9-12
Hearing Protection 9-12
Hand Protection 9-13
Glove Selection Guide 9-13
Respiratory Protection 9-16

Chapter 10 - Material Selection
Properties of Common Elastomers 10-2
Properties of Common Fluoropolymers 10-3
Properties of Common Plastics 10-4
U.S. Plastics Recycling Symbols 10-4
Properties of Common Metals 10-5
Corrosion 10-6
Relative Corrosion Resistance of Various Materials 10-6
Corrosion Units Conversion Factors 10-7
Galvanic Series of Metals 10-7
Properties and Corrosion of Glass 10-8
Effect of pH on Glass Corrosion Rate 10-8
Substances Know to Attack Borosilicate Glass 10-8
Corrosion of Borosilicate Glass by Acids 10-9
Corrosion of Borosilicate Glass by Bases 10-9
MaterialsCompatibility Table 10-10
Substances Known to Attack 316 Stainless Steel 10-28
Substances Known to Attack Hastelloy C-276 10-28
Substances Known to Attack Tantalum Metal 10-28

Chapter 11 - Miscellaneous
Unit Conversion Factors 11-2
Comparison of Unit Systems 11-4
Mathematical and Physical Constants 11-5
Useful Mathematical Relationships 11-5
Exponents and Logarithms 11-5
Polynomials 11-5
Geometric Formulas 11-6
Trigonometry 11-7
Continuous Stirred Tank Dilution Effects (Feed and Bleed) 11-7
Calculations for Asymmetric Crystallizations 11-7
Temperature Conversion Diagram 11-8
Pressure Conversion Diagram 11-9
Vacuum Conversion Diagram 11-10
Useful Cold Mixtures for the Laboratory 11-11
Decimal Equivalents of Fractions of an Inch 11-11
Standard Sieve Specifications 11-12
Mill Grade Wire Cloth Specifications 11-12
Industry-Related Acronyms and Abbreviations 11-13

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