Chapter 1 - The Pilot Plant 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 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 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 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 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 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 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 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 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 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 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 |