- •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
184 |
Joints, Stopcocks, and Glass Tubing |
Q
Step
Tubing cannot move in anymore due to the step.
Fig. 3.16 Internal motion of the inserted tube is blocked by the addition of an internal step.
be ideal for high-vacuum work, pieces can wiggle around, and you need to be careful about the materials that come in contact with the particular O-rings being used.
3.2Stopcocks and Valves
3.2.1Glass Stopcocks
The stopcock is more than just an on/off valve because it may also be used to direct liquid or gas flow through a system. In addition, depending on their design, stopcocks have limited-to-excellent ability to vary gas or liquid flow rates. Stopcock size is identified by the size of the hole through the plug. The internal diameter of each arm is likely to be much larger than the size of the plug hole and should not be used for stopcock size identification.
Like the ground joint, glass stopcocks are made in a 1:10 taper. Interchangeability of new plugs and barrels (a plug from one stopcock placed in a like-sized barrel) used to be a standard feature by all manufacturers. Currently not all manufacturers guarantee interchangeability of new plugs and barrels. Talk with a glassblower, or your supplier, about the interchangeability of any particular brand. Even with brands that claim interchangeability, older or well-used stopcocks are less likely to be interchangeable because of uneven wear during use. Therefore, look for potential leaks when placing a new plug within an old.
To verify if a stopcock plug and barrel are a good match, assemble the pieces, then sight down the inside of a side arm to see how well the holes align. Misalignment may be minor, causing a slight decrease in potential flow, or may be so great that nothing can pass through (see Fig. 3.17)
The primary difference between a regular and a high-vacuum stopcock is the final grind. Stopcocks and joints are ground (lapped) with abrasive compounds
A small film of grease on the O-ring can ease sliding the O-ring onto glassware and help provide a better vacuum seal.
Stopcocks and Valves 3.2 |
185 |
If the plug is too small, the plug hole will not align with the barrel hole.
Only when the plug is ground the proper amount will the plug hole and barrel holes align
If the plug is too large, the plug hole will not align with the barrel hole.
Fig. 3.17 Plugs of the wrong size can prevent flow in a stopcock.
just as rocks are ground in lapidary work. The finer the grade of grinding compound, the smoother the finish on the ground (lapped) surface. The smoother the finish on the glass parts, the easier they will slide past each other when rotated. Joints can be used for high-vacuum purposes without the same degree of grinding because they are not rotated.
Vacuum stopcocks are not meant to be interchangeable. Each plug and barrel receive their final grind together, and therefore they are mated for life. To prevent mismatching a plug and barrel set, numbers and/or letters are inscribed for each stopcock on the handles of the plug and on the side of the barrels (see Sec. 3.3.1). Aside from alignment problems, cross-matched plugs and barrels of high-vacuum stopcocks may leak or jam when rotated.
A simple, basic two-way glass stopcock (shown in Fig. 3.17) will have a single hole drilled through a solid plug. The arms are straight and placed 180° from each other. The plug is typically held in place by a rubber washer or metal clip at the small end. This stopcock design is easy to make and is inexpensive. The usual problems that arise from this type of stopcock are as follows:
1. Dirt can collect on the grease and work its way into the plug's hole. From there the dirt can eventually wear a groove on the inside of the barrel. This groove, leading from one arm to another, can eventually become great enough to prevent a complete seal when the plug is rotated to the "off' position.
2. As stopcock grease becomes old and/or cold, it becomes brittle, and rotation can cause a "shear"-type break, allowing the plug to be free from the barrel.
186 |
Joints, Stopcocks, and Glass Tubing |
Oblique bore |
(a) |
(b) |
Fig. 3.18 Standard and vacuum designs of an oblique two-way stopcock.
By setting the two arms oblique to each other on the barrel and having a hole drilled diagonally in the plug (Fig. 3.18), two advantages are achieved:
1.If the first of the above problems arises, the grooves will not line up with the opposite arm and potential leakage is reduced considerably.
2.This configuration allows only one position (in 360° of rotation) for material flow.
As mentioned in Sec. 1.1.5, which discussed different types of glass, glass expands or contracts with temperature. Thin glass does not expand (or contract) the same relative amount as thick glass under the same conditions. Because of this difference, all vacuum stopcocks have hollow plugs so that the plugs may expand and contract at the same relative amount as the barrels. Thus, when there is a drop in temperature, the plug will not loosen by contracting a greater amount than the barrel. Likewise, if there is a sharp rise in temperature, the plug will not jam within the barrel by expanding a greater amount within the barrel. This quality
|
Oblique |
u PPe r |
L |
oblique |
|
arm |
B o r e d ^ * " ^ |
|
h 0 l e |
Vacuum
side
Vacuum
side
plug
(b)
When the plug is rotated so the System bored hole faces the vacuum
side direction (the lower arm), a vacuum is pulled from inside the barrel.
System
sids |
t h e p | u g jg r o t a t e d t h e |
|
other way, a passage is made |
||
|
||
|
through the two (oblique) arms. |
Fig. 3.19 How to evacuate the vacuum bulb of a vacuum stopcock.
Stopcocks and Valves 3.2 |
187 |
Offset design L design
Fig. 3.20 The offset and "L" design of two-way vacuum stopcocks.
can be critical if an experiment or environment has rapid temperature changes. Figure 3.18(a) shows a solid plug. The holes in solid plugs are drilled. Figure 3.18(b) shows a hollow plug. The hole in a hollow stopcock plug is a glass tube sealed obliquely within and later ground to fit the barrel. This inner tube provides the passageway for gases* through the hollow plug.
Oblique arm stopcocks are not immune from "shear" breaks caused by cold or old stopcock grease. Because an accidental rush of air into a vacuum system can cause damage to the system or destroy oxygen sensitive materials within the system, vacuum stopcocks have a design feature to prevent accidental removal of the plug from the barrel. The stopcock design shown in Fig. 3.19 demonstrates how a vacuum stopcock uses a vacuum to secure its plug from slipping out of the barrel. The bottom of the barrel is closed with a bulb [see Fig. 3.19(a)]. A hole is bored opposite the low opening of the oblique tube [see Fig. 3.19(b)]. Aligning the hole with the lower oblique arm of the stopcock [see Fig. 3.19(c)] creates a passage for the vacuum that holds the plug securely in the barrel. A 180° rotation from this position is the "open" position for this stopcock [see Fig. 3.19(d)]. The only way to separate the plug from the barrel is to release the vacuum from inside the stopcock by rotating the bored hole toward the lower oblique arm when no vacuum is present.
Figure 3.20 shows two different alignments of the same type of stopcock. This plug design is simpler, and therefore it is somewhat less expensive. There is no advantage of the "offset" design to the "L" design. The choice depends on how your system is built—that is, whether the "offset" design or the "L" design stopcock physically fits better into your given system or apparatus. With these stopcocks, the vacuum of the system holds the plug in continuously. However, once the system loses its vacuum, its ability to hold the plug is lost as well.
3.2.2 Teflon Stopcocks
Teflon stopcocks provide excellent alternatives to standard glass stopcocks because no grease is required. They can be used in distillation systems where organic solvents, UV radiation, or oxidizing gases would normally make using a glass stopcock impossible. This advantage does not come without some cost because Teflon stopcocks are generally more expensive than standard glass stop-
Vacuum stopcocks are not intended for liquid transport use.
188
White plastic washer ^-
(front view)
Joints, Stopcocks, and Glass Tubing
White plastic |
|
washer |
Locking nut |
|
O-ring lock washer
The Teflon stopcock has a 1:5 taper on its plug to be within the guidelines of" <P," known as Product Standard.
Fig. 3.21 Proper orientation of the parts of a Teflon stopcock.
cocks. The Teflon stopcock design looks essentially the same as its glass counterpart. However, it is not possible to take a Teflon plug and use it with a standard stopcock because Teflon stopcocks are made with a 1:5 taper rather than the 1:10 taper of glass. Because Teflon flows, or "creeps," it is likely to stick at a 1:10 taper by flowing into the arm holes, but far less likely to stick at a 1:5 taper. Teflon stopcocks with a 1:5 taper follow ASTM guidelines and are known as Product Standard.
There was a period of time when some Teflon stopcocks were made with 1:7 tapers, but this line was discontinued. I mention this point because some of you may have found one of these stopcocks and are having difficulty finding a replacement plug or are frustrated by trying to fit an old 1:7 plug in a new 1:5 barrel. The taper variations are small and subtle, so it is easy to confuse the two. Because the 1:7 taper design is no longer made, it is recommended that you phase any pieces with that design out of your lab.
The Teflon stopcock has more pieces (see Fig. 3.21) than the glass stopcock, and often the pieces are assembled in the wrong order. Inserting the plug into the barrel provides no challenges, but the white and black washers invariably get inverted. Each piece serves a specific function for the successful operation of the Teflon stopcock: The white washer helps everything on the plug shaft rotate together when the plug is turned; the colored locking nut helps maintain a certain amount of tension on the plug; and finally, the black washer (O-ring) serves as a lock washer to prevent the locking nut from rotating itself off the threaded section of the plug.
If the lock washer is placed on the plug shaft before the white washer, the washer's friction will grab the surface of the barrel and tend to make everything past the black washer not rotate while the plug is turned, causing the plug to tighten when rotated clockwise and loosen when rotated counterclockwise.
The white washer has a flat side on the hole through the center to maintain its nonslip position on the plug. Occasionally, the flat spot on the white washer