- •Contents
- •Foreword
- •Preface
- •1 Materials in the Lab
- •2 Measurement
- •3 Joints, Stopcocks, and Glass Tubing
- •4 Cleaning Glassware
- •5 Compressed Gases
- •6 High and Low Temperature
- •7 Vacuum Systems
- •8 The Gas-Oxygen Torch
- •APPENDIX
- •Appendix A Preparing Drawings for a Technician
- •Index
- •Foreword
- •Preface
- •For the Second Edition
- •Please note:
- •1 Materials in the Lab
- •1.1 Glass
- •1.1.1 Introduction
- •1.1.2 Structural Properties of Glass
- •1.1.3 Phase Separation
- •1.1.4 Devitrification
- •1.1.5 Different Types of Glass Used in the Lab
- •1.1.6 Grading Glass and Graded Seals
- •1.1.7 Separating Glass by Type
- •1.1.9 Stress in Glass
- •1.1.11 Tempered Glass
- •1.1.13 Limiting Broken Glass in the Lab
- •1.1.14 Storing Glass
- •1.1.15 Marking Glass
- •1.1.16 Consumer's Guide to Purchasing Laboratory Glassware
- •1.2 Flexible Tubing
- •1.2.1 Introduction
- •1.2.2 Physical Properties of Flexible Tubing
- •1.3 Corks, Rubber Stoppers, and Enclosures
- •1.3.1 Corks
- •1.3.2 Rubber Stoppers
- •1.3.3 Preholed Stoppers
- •1.3.4 Inserting Glass Tubing into Stoppers
- •1.3.5 Removing Glass from Stoppers and Flexible Tubing
- •1.3.6 Film Enclosures
- •1.4 O-Rings
- •1.4.2 Chemical Resistance of O-Ring Material
- •1.4.3 O-Ring Sizes
- •2 Measurement
- •2.1 Measurement: The Basics
- •2.1.1 Uniformity, Reliability, and Accuracy
- •2.1.2 History of the Metric System
- •2.1.3 The Base Units
- •2.1.4 The Use of Prefixes in the Metric System
- •2.1.5 Measurement Rules
- •2.2 Length
- •2.2.1 The Ruler
- •2.2.2 How to Measure Length
- •2.2.3 The Caliper
- •2.2.4 The Micrometer
- •2.3 Volume
- •2.3.1 The Concepts of Volume Measurement
- •2.3.2 Background of Volume Standards
- •2.3.4 Materials of Volumetric Construction #1 Plastic
- •2.3.5 Materials of Volumetric Construction #2 Glass
- •2.3.6 Reading Volumetric Ware
- •2.3.7 General Practices of Volumetric Ware Use
- •2.3.8 Calibrations, Calibration, and Accuracy
- •2.3.9 Correcting Volumetric Readings
- •2.3.10 Volumetric Flasks
- •2.3.11 Graduated Cylinders
- •2.3.12 Pipettes
- •2.3.13 Burettes
- •2.3.14 Types of Burettes
- •2.3.15 Care and Use of Burettes
- •2.4 Weight and Mass
- •2.4.1 Tools for Weighing
- •2.4.2 Weight Versus Mass Versus Density
- •2.4.3 Air Buoyancy
- •2.4.5 Balance Location
- •2.4.6 Balance Reading
- •2.4.7 The Spring Balance
- •2.4.8 The Lever Arm Balance
- •2.4.9 Beam Balances
- •2.4.10 Analytical Balances
- •2.4.11 The Top-Loading Balance
- •2.4.12 Balance Verification
- •2.4.13 Calibration Weights
- •2.5 Temperature
- •2.5.1 TheNature of Temperature Measurement
- •2.5.2 The Physics of Temperature-Taking
- •2.5.3 Expansion-Based Thermometers
- •2.5.4 Linear Expansion Thermometers
- •2.5.5 Volumetric Expansion Thermometers
- •2.5.7 Thermometer Calibration
- •2.5.8 Thermometer Lag
- •2.5.9 Air Bubbles in Liquid Columns
- •2.5.10 Pressure Expansion Thermometers
- •2.5.11 Thermocouples
- •2.5.12 Resistance Thermometers
- •3.1 Joints and Connections
- •3.1.1 Standard Taper Joints
- •3.1.2 Ball-and-Socket Joints
- •3.1.3 The O-Ring Joint
- •3.1.4 Hybrids and Alternative Joints
- •3.1.5 Special Connectors
- •3.2 Stopcocks and Valves
- •3.2.1 Glass Stopcocks
- •3.2.2 Teflon Stopcocks
- •3.2.3 Rotary Valves
- •3.2.4 Stopcock Design Variations
- •3.3.1 Storage and Use of Stopcocks and Joints
- •3.3.2 Preparation for Use
- •3.3.3 Types of Greases
- •3.3.4 The Teflon Sleeve
- •3.3.5 Applying Grease to Stopcocks and Joints
- •3.3.6 Preventing Glass Stopcocks and Joints from Sticking or Breaking on a Working System
- •3.3.7 Unsticking Joints and Stopcocks
- •3.3.8 Leaking Stopcocks and Joints
- •3.3.9 What to Do About Leaks in Stopcocks and Joints
- •3.3.10 General Tips
- •3.4 Glass Tubing
- •3.4.1 The Basics of Glass Tubing
- •3.4.2 Calculating the Inside Diameter (I.D.)
- •3.4.3 Sample Volume Calculations
- •4 Cleaning Glassware
- •4.1 The Clean Laboratory
- •4.1.1 Basic Cleaning Concepts
- •4.1.2 Safety
- •4.1.3 Removing Stopcock Grease
- •4.1.4 Soap and Water
- •4.1.5 Ultrasonic Cleaners
- •4.1.6 Organic Solvents
- •4.1.7 The Base Bath
- •4.1.8 Acids and Oxidizers
- •4.1.9 Chromic Acid
- •4.1.10 Hydrofluoric Acid
- •4.1.11 Extra Cleaning Tips
- •4.1.12 Additional Cleaning Problems and Solutions
- •4.1.13 Last Resort Cleaning Solutions
- •5 Compressed Gases
- •5.1 Compressed GasTanks
- •5.1.1 Types of Gases
- •5.1.2 The Dangers of Compressed Gas
- •5.1.3 CGA Fittings
- •5.1.4 Safety Aspects of Compressed Gas Tanks
- •5.1.5 Safety Practices Using Compressed Gases
- •5.1.6 In Case of Emergency
- •5.1.7 Gas Compatibility with Various Materials
- •5.2 The Regulator
- •5.2.1 The Parts of the Regulator
- •5.2.2 House Air Pressure System
- •5.2.4 How to Use Regulators Safely
- •5.2.6 How to Purchase a Regulator
- •6 High and Low Temperature
- •6.1 High Temperature
- •6.1.1 TheDynamics of Heat in the Lab
- •6.1.2 General Safety Precautions
- •6.1.3 Open Flames
- •6.1.4 Steam
- •6.1.5 Thermal Radiation
- •6.1.6 Transfer of Energy
- •6.1.7 Hot Air Guns
- •6.1.8 Electrical Resistance Heating
- •6.1.9 Alternatives to Heat
- •6.2 Low Temperature
- •6.2.1 TheDynamics of Cold in the Lab
- •6.2.2 Room Temperature Tap Water (=20°C)
- •6.2.8 Safety with Slush Baths
- •6.2.9 Containment of Cold Materials
- •6.2.10 Liquid (Cryogenic) Gas Tanks
- •7 Vacuum Systems
- •7.1 How to Destroy a Vacuum System
- •7.2.1 Preface
- •7.2.2 How to Use a Vacuum System
- •7.2.4 Pressure, Vacuum, and Force
- •7.2.5 Gases, Vapors, and the Gas Laws
- •7.2.6 Vapor Pressure
- •7.2.7 How to Make (and Maintain) a Vacuum
- •7.2.8 Gas Flow
- •7.2.9 Throughput and Pumping Speed
- •7.3 Pumps
- •7.3.1 The Purpose of Pumps
- •7.3.2 The Aspirator
- •7.3.3 Types and Features of Mechanical Pumps
- •7.3.4 Connection, Use, Maintenance, and Safety
- •7.3.5 Condensable Vapors
- •7.3.6 Traps for Pumps
- •7.3.7 Mechanical Pump Oils
- •7.3.8 The Various Mechanical Pump Oils
- •7.3.9 Storing Mechanical Pumps
- •7.3.11 Ultra-High Vacuum Levels Without Ultra-High
- •7.3.12 Diffusion Pumps
- •7.3.13 Attaching a Diffusion Pump to a Vacuum System
- •7.3.14 How to Use a Diffusion Pump
- •7.3.15 Diffusion Pump Limitations
- •7.3.17 Diffusion Pump Maintenance
- •7.3.18 Toepler Pumps
- •7.4 Traps
- •7.4.1 The Purpose and Functions of Traps
- •7.4.2 Types of Traps
- •7.4.3 Proper Use of Cold Traps
- •7.4.4 Maintenance of Cold Traps
- •7.4.5 Separation Traps
- •7.4.6 Liquid Traps
- •7.5 Vacuum Gauges
- •7.5.2 The Mechanical Gauge Family
- •7.5.4 The Liquid Gauge Family
- •7.5.5 The Manometer
- •7.5.6 The McLeod Gauge
- •7.5.7 How to Read a McLeod Gauge
- •7.5.8 Bringing a McLeod Gauge to Vacuum Conditions
- •7.5.10 The Tipping McLeod Gauge
- •7.5.11 Condensable Vapors and the McLeod Gauge
- •7.5.12 Mercury Contamination from McLeod Gauges
- •7.5.13 Cleaning a McLeod Gauge
- •7.5.14 Thermocouple and Pirani Gauges
- •7.5.15 The Pirani Gauge
- •7.5.16 Cleaning Pirani Gauges
- •7.5.17 The Thermocouple Gauge
- •7.5.18 Cleaning Thermocouple Gauges
- •7.5.19 The lonization Gauge Family
- •7.5.20 The Hot-Cathode Ion Gauge
- •7.5.21 Cleaning Hot-Cathode Ion Gauges
- •7.5.24 The Momentum Transfer Gauge (MTG)
- •7.6 Leak Detection and Location
- •7.6.1 AllAbout Leaks
- •7.6.3 False Leaks
- •7.6.4 Real Leaks
- •7.6.5 Isolation to Find Leaks
- •7.6.6 Probe Gases and Liquids
- •7.6.7 The Tesla Coil
- •7.6.8 Soap Bubbles
- •7.6.9 Pirani or Thermocouple Gauges
- •7.6.10 Helium Leak Detection
- •7.6.11 Helium Leak Detection Techniques
- •7.6.13 Repairing Leaks
- •7.7 More Vacuum System Information
- •7.7.1 The Designs of Things
- •8 The Gas-Oxygen Torch
- •8.1.2 How to Light a Gas-Oxygen Torch
- •8.1.3 How to Prevent a Premix Torch from Popping
- •8.2.2 How to Tip-Off a Sample
- •8.2.3 How to Fire-Polish the End of a Glass Tube
- •8.2.4 Brazing and Silver Soldering
- •Appendix
- •A.2 Suggestions for Glassware Requests
- •B.1 Introduction
- •B.2 Polyolefins
- •B.3 Engineering Resins
- •B.4 Fluorocarbons
- •B.5 Chemical Resistance Chart
- •C.1 Chapter 1
- •C.4 Chapter 4
- •C.5 Chapter 5 & Chapter 6
- •C.6 Chapter 7
- •C.7 Chapter 8
- •D.1 Laboratory Safety
- •D.2 Chemical Safety
- •D.3 Chapter 1
- •D.4 Chapter 2
- •D.5 Chapter 3
- •D.6 Chapter 4
- •D.7 Chapter 5 and the Second Half of Chapter 6
- •D.8 Chapter 7
- •D.9 Chapter 8
- •Index
Compressed Gases
5.1Compressed GasTanks
5.1.1Types of Gases
A gas is defined as any material that boils within the general ranges of STP standard temperature (25°C) and Pressure (I atmosphere).* Although there are many compounds that satisfy these conditions, only 11 elements do, and these are argon, chlorine, fluorine, helium, hydrogen, krypton, oxygen, neon, nitrogen, radon, andxenon.
There aretwomajor groups of gases. Thefirst group is known as thenon-lique- fied gases (also known as cryogenic gases). These gases do not liquefy at room temperatures nor at pressures from 25 to 2500 psig. They liquefy at very low temperatures (-273.16°C to ~ -150°C). Thesecond group of gases, known as the liquefied gases, canliquefy at temperatures easily made in thelaboratory (-90°C to~ -1°C) and at pressures from 25 to 2500 psig. These gases become solid at those temperatures at which the cryogenic gases become liquid. Carbon dioxide (dry ice), generally considered a liquefied gas, could also be known as a solidified gas as it does nothave a liquid state at STP.
As far as gasphysics goes, there areonly these twotypes of gases. However, the shipping industry has a third classification known as the dissolved gases. Acetylene is a dissolved gas, whic.h without special equipment, can explode at pressures above 15 psig. Because of this property, efficient shipping of this gas becomes almost impossible. Toavoid this problem, thegasis shipped dissolved in acetone and placed in cylinders that are filled with an inert, porous material. Under these special conditions, acetylene can be safely shipped at pressures of 250 psig.
Gases are stored and shipped in a compressed state in cylinders designed to withstand the required pressure. The cryogenic gases, such as oxygen and nitrogen, are shipped in both liquefied and gaseous states, but the liquid state requires expensive equipment. Other gases, such as propane, are typically shipped and
*A vapor is a gasthat is near its condensation point within thegeneral range of STP.
253
254 |
Compressed Gases |
stored in their liquid states. The region above a liquefied gas is an area called the head space, which is the gas form of the liquefied gas. The pressure of the gas in the head space depends on the vapor pressure of the gas, which, in turn, depends on the temperature of the liquid gas. The greater the temperature of the liquefied gas is and the greater the amount of gas released from the liquid, the greater the pressure in the head space. If the pressure is sufficient, the container can rupture. To prevent this, all tanks have some sort of pressure release valve that release excess pressure at some determined value.
To control the rate of flow and releasing pressure, gases are released from compressed gas cylinders by regulators (see Sec. 5.2) at a user-defined pressure. A regulator can display the amount of gas remaining in a compressed gas tank (in cubic feet of gas), but not in a liquefied gas tank.
The remaining liquid gas in a tank can be estimated by observing any floats that may exist [most commonly seen in cryogenic tanks (see Sec. 6.2.10)], but it can always be accurately determined by weighing the tank. First you must subtract the weight of the empty tank by the weight of the partially filled tank (known as the tare weight*) to determine the weight of any remaining liquid. Then you divide the difference by the weight of the liquid gas per liter to calculate the remaining volume.
Tank-weighing should be done with everything you plan to use with it (i.e., regulators, tubing, and so forth) attached, making sort of a "ready-to-use tare weight." This ready-to-use weight means you do not have to strip the tank of all equipment to make remaining gas determinations. Otherwise, if it was originally weighed without a regulator but later weighed with one, you might assume that you have more gas than really exists.
5.1.2 The Dangers of Compressed Gas
Compressing a gas allows a lot of gas to exist in a small amount of area for transportation, storage, and use. It is physically easier to deal with a compressed, gas tank that is 9 in. in diameter and 51 in. tall than to store the approximately several hundred cubic feet1^ of gas contained within.
Regardless of the inherent danger of any given gas, once a gas is compressed its potential for danger takes on a completely different light. A completely safe gas compressed in a container at some 2000 lb/in.2 could act like a bomb if improperly handled! Your safety, and the safety of your equipment, is therefore dependent on:
1.
*A11tanks that require weighing for volume content have their tare weight stamped on the side of the tank. This weight is exclusively the tank and does not include any regulators, valves, straps, or other fittings the user may have added.
fA tank of this size will contain (for example) 282 cu ft of oxygen, 257 cu ft of nitrogen, or 290 cu ft of ultrapure argon.
Compressed Gas Tanks 5.1 |
255 |
2.The materials and equipment selected to be used with the compressed gases
3.The proper use of the compressed gas cylinders and associated equipment
The first two points of the above list can best be controlled by strict industry standards and the conscientious matching of equipment to the needs and demands of the user. The third requires education, and unfortunately the user often does not have the opportunity (or desire) to learn everything there is to know about how to use compressed gases safely. Therefore, there have been a variety of industrystandard "idiot-proof controls to minimize the possibility of mistakes. To make compressed gas cylinders consistently safe, reliable, and as idiot-proof as possible, these strategies took the study, analysis, and deliberation of at least 18 different private and governmental agencies (see Table 5.1).
The first level of safety for quality and control is the construction of compressed gas cylinders. The specifications for their construction in North America is denned by Department of Transportation (DOT) and Canadian Transport Commission (CTC) regulations. Cylinders are made from carbon steel or alloy steel with seamless, brazed, or welded tubing that is formed by billeting (drawing flat
Table 5.1 Agencies involved
in Standardization of Compressed Gas Tanks
American Gas Assoc.
American Petroleum Inst.
American Society for Testing and Materials
American Welding Society
Association of American Railroads
Canadian Transport Commission (CTC)
Compressed Gas Association (CGA)
Compressed Gas Manufacturer's Assoc. Inc.
Connections Standards Commission of the CGA (This was first known as the Gas Cylinder Valve Thread Commission of the CGA. Later it became the Valve Standards Com. of the CGA, and in 1971 it received its current name.)
Department of Transportation (DOT)
Interdepartmental Screw Thread Commission
International Standards Organization (ISO)
National Institute of Standards and Technology (This is the new name of the National Bureau of Standards)
National Fire Prevention Assoc.
Standards Associations (representing Great Briton, Canada, and the U.S.)
U.S. Army
U.S. Dept. of Commerce
U.S. Navy
256 Compressed Gases
sheets to a cylindrical shape) or by using punch-press dies. Ends are sealed by forging or spinning at great heat. Alternatively, closed ends are drilled out and a metal piece is plugged into the hole. In the United States, one tank design can be used for a variety of gases (except for acetylene). In Europe, a tank can only be used for the gas it was designed for.
Generally, cylinders that are broad and squat in contour are for low-pressure service, such as the propane tanks used on automobiles or with campers. Those that are tall and thin are generally used for high-pressure containment, such as for oxygen, hydrogen, or nitrogen.
A series of letters and numbers are stamped on the shoulders of compressed gas tanks (see Fig. 5.2) to provide coded information for tank inspectors. These numbers tell under what codes the tank was made, the manufacturer, service pressure, serial number of the tank, and when it was last inspected and by whom. The manner in which the codes are laid out varies, and it may be difficult for an untrained person to interpret. However, to the compressed gas industry, they are important for preventing mistakes from the misuse of the containers.
5.1.3 CGA Fittings
To prevent gases from being attached to the wrong system, the Compressed Gas Association (CGA) implemented a variety of different fittings for attaching a regulator to a compressed gas tank. These fittings prevent a user from accidentally taking a regulator that is used (for example) for nitrogen and attaching it to a hydrogen tank. By itself, such an attachment may not seem too bad, but if the nitrogen regulator was already connected to a system expecting nitrogen, the consequences of hydrogen could be dramatic.
Table 5.2 lists a number of gases and the appropriate CGA fittings or threaded connections that a regulator must have to be attached to a tank of such a gas (in this table, when a second CGA number follows a first entry, it is the CGA fitting for a lecture bottle). Alternatively, if you have a regulator and want to know what gases it can be used with—or what other gases use the same regulator—see Table 5.3.
If, after looking at Table 5.2 or Table 5.3, you wish to know what a fitting looks like, Fig. 5.2 illustrates the 15 most common CGA fittings used on full-sized compressed gas tanks within the laboratory. Please note that right-handed threads close with CW rotation, and left-handed threads close with CCW rotation. Lefthanded thread fittings can be easily identified by the notch on the closing nut (see Fig. 5.2) as opposed to right-handed fittings, which are notchless.
Never spray or drip oil onto compressed tank cap threads to ease removal or to replace the tank cap. Minimally, the oil could contaminate the CGA fitting, but oil near compressed oxygen can explode! If you are unable to remove or replace a tank cap, obtain help from the manufacturer or the distributor of the compressed tank.