- •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
446 |
Vacuum Systems |
1.When possible, usea gas over a liquid.
2.Do not spray or squirt a liquid on. Usea cotton swab (or Kimwipe) to wipe it across parts of the system. Inaddition to safety, this method provides more control in finding leaks.
3.Solvents can damage parts of your system such as O-rings, causing a greater leak than theone you were originally trying to find. In addition, if the solvent drips on a water hose andcreates a hole, you then have a water leak and a mess. If it drips on electric wires, you mayhave a short.
4.All of the chemicals listed in Table 7.14 are dangerous to breathe or
have in contact with skin from short to extended periods of time. Some of the chemicals listed have severe OSHA restrictions foruse without a fume hood, andsome aretoxic chemicals andshould not beused at all (such ascarbon tetrachloride and xylene).
5.Do not have any open flames orsparks while working onleak detection. Unplug iongauges and other electrical equipment.
6.Besure to have plenty of ventilation andlimit yourself to thefirst three liquids in Table 7.14. These liquids are(relatively) the safest, andthey are the best from the list. Still, you should use a buddy system, and check with OSHA and/or local/state regulations to verify if there are
any legal restrictions onthe uses of any of these chemicals in your area.
7.When possible, select a low-vapor-pressure liquid over a high-vapor- pressure liquid toprovide faster cleanup time. Inaddition, nonpolar solvents aremore easily removed from glassware than polar solvents (for example, methanol vs. acetone).
8.When spraying probe gases on a vacuum system, be sure to start at the top with gases less dense than air and start at the bottom with gases denser than air.
Other aspects ofTurnbull's four factors will beconsidered further in Sec. 7.6.9.
7.6.7 The Tesla Coil
If you have a glass system andcanachieve a vacuum between approximately 10 to approximately 10~3 torr, then you can use a Tesla coil (sometimes called a "sparker") to look for moderate-size leaks. Because this range is the vacuum range of a mechanical vacuum pump, theTesla coil provides anexcellent tool for examining such systems.
The Tesla coil will ionize thegas molecules remaining in a vacuum systemand cause them to glow. Above pressures of about 10torr the gas molecules quench a discharge. That is, they aresoclose together they lose their extra energy bybumping into other molecules rather than giving off light. Below 10"3 torr, the mole-
Leak Detection and Location 7.6 |
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447 |
_ |
~. |
Insulated handle |
|
|
Control knob •—^ |
|
r |
|
|
Power cord ^ 3 |
|
> = ^ J ^ - |
Wire on tip |
|
Light-duty Tesla Coil |
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|||
Power cord |
|
|
Insulated handle |
|
^~ |
|
Control knob |
/ |
, |
Heavy-duty Tesla Coil
Fig. 7.57 The lightand heavy-duty Tesla coil.
cules are too far apart and the mean free paths are too long to maintain a discharge.
As the tip of a Tesla coil is slowly waved within 1-3 cm of an evacuated glass vacuum system, the gases remaining will discharge with a glow characteristic of the gases within the system. If you bring theTesla coil near a leak, a large white spark will jump from thetip of the coil to thespecific leak spot. This event is very dramatic anddemonstrates the location of a leak in a very effective manner. The spark is actually seeking ground, and the leak provides a path to the discharge inside the vacuum system. In turn, this discharge (which is an electrical conductor) provides a path to themechanical pump for completion of the ground.
Metal components confound Tesla coil use: Their ground is easier to obtain than the ground found by passing through a glass leak andthepoorer conducting discharge within.
There area fewlimitations to theuseof a Tesla coil:
1.It cannot be used near metal clamps or glass-to-metal seals on a glass system. Themetal provides a ground for theelectric discharge, bypassing theionization of the gasinside thesystem.
2.A large quantity of very small holes mayprevent youfrom obtaining a decent vacuum. However, none of the holes may belarge enough for the Tesla coil to indicate a leak.
3.The self-contained Tesla coils often found in many labs are recommended by themanufacturers notto be used for longer than 10minutes of continuous operation. If your needs require long continuous useona consistent basis, heavy-duty Tesla coils are available that can be used continuously. These coils areeasily identified because they have small boxes (approximately 5 in. x 5 in. x 8 in) connected to their hand-held sections. These hand-held sections arethesame asthose found on standard light-duty Tesla coils (see Fig. 7.57).
4.TheTesla coil will not find a leak within a demountable (seals such as stopcocks orjoints) that is caused by poor application of grease or old stopcock grease that hassheared.
448 |
Vacuum Systems |
5.The Tesla coil should not be used near O-ring joints because the coil can destroy the O-ring by burning a strip across its side.
6.The Tesla coil should not be used near intentionally thin sections of glass (such as a break-off) because it can punch a hole through such a section.
It is unlikely that a leak could develop on a glass tube that has not received stress or that has not been worked on by a glassblower. Therefore to save time, simply pass the Tesla coil around areas where glass sections have been joined (see Fig. 7.58).* If there is a twoor three-fingered clamp in an area that needs to be tested, the clamp must be removed to properly check the seal. To spark check for cracks around hooks placed near a joint, place a rubber stopper in the end of the joint and then open up the stopcock to evacuate that section.
The spark from a Tesla coil is very powerful and can punch its way through thin sections of glass (see Point 6 above). Keep the coil away from known thin sections in which you wish to maintain integrity, such as break-offs. Most texts on vacuum technique recommend that the Tesla coil not be allowed to sit over weak areas for fear of "punching" a hole through the glass. This author disagrees with this reticence because if there is not a hole in a potentially weak area now, there may very likely be one in the area some time in the future. Therefore, go ahead and provide some stress while you are in a position to do something about any holes that develop. Otherwise a hole may develop either in the middle of an experiment or when repair and/or personnel are not available or as convenient. In addition, It is important that all gauge controllers be turned off before initiating Tesla coil testing. The charge from the Tesla coil can destroy the controller's electronics.
Some extra Tesla coil tips are as follows:
Glass should be |
f |
\ |
Where there is no apparent distortion |
checked for leaks in |
V. |
J |
of the glass, it is unlikely that any |
locations where glass |
Jf\ |
I |
glassblowing has taken place. A leak |
has been sealed to |
<^ |
_U |
is therefore unlikely in these regions. |
other pieces of glass. |
^ ^ . f l |
X |
If glass was not properly annealed, cracks can also develop where hooks were attached.
Fig. 7.58 Suggested areas of testing with a Tesla coil.
An exception to this rule would be if a twoor three-fingered support clamp was overly tightened on a glass tube, causing the tube's wall to crack.
Leak Detection and Location 7.6 |
449 |
Table 7.15 Appearance of Discharges
in a Gas Discharge Tube at Low Pressures76
Gas |
Negative Glow |
Positive Column |
Air |
Blue |
(Reddish) |
Nitrogen |
Blue |
Yellow (red gold) |
Oxygen |
Yellowish white |
Lemon |
Hydrogen |
Bluish pink (bright blue) |
Pink (rose) |
Helium |
Pale green |
Violet-red |
Argon |
Bluish |
Deep red (violet) |
Neon |
Red-orange |
Red-orange (blood red) |
Krypton |
Green |
— |
Xenon |
Bluish white |
— |
Carbon monoxide |
Greenish white |
(White) |
Carbon dioxide |
Blue |
(White) |
Methane |
Reddish violet |
— |
Ammonia |
Yellow-green |
— |
Chlorine |
Greenish |
Light green |
Bromine |
Yellowish green |
Reddish |
Iodine |
Orange-yellow |
Peach blossom |
Sodium |
Yellowish green (whitish) |
Yellow |
Potassium |
Green |
Green |
Mercury |
Green (goldish white) |
Greenish blue (greenish) |
— indicates no distinctive color. |
|
|
() indicates a different observer's opinion of the color.
1.Turn off some (or all) of the lights in a room so that any discharge from the coil can more easily be seen (it may also be necessary to close doors and/or cover windows). In addition, try not to face an open window.
2.A metal wire (such as copper or nichrome) wrapped around the tip of the Tesla coil (see Fig. 7.57) and bent in a rightangle can extend your reach and/or reach behind glassware.
The Tesla coil can also be used to make the vacuum line a discharge tube to light up probe gases or liquids. Gases or vapors in a vacuum will light up in specific colors from a discharge caused by a Tesla coil. A list of the colors that can be achieved with pure gases in a discharge tube can be seen in Table 7.15.
Table 7.15 |
(found in several books |
or found as |
a similar table in other |
books ' o n |
vacuum technology) provides the colors |
of pure gases from dis- |
charge tubes, which have very little to do with the discharge from the Tesla coil because of the following conditions:
1. The applied voltage and pressure can vary greatly.
450 Vacuum Systems
Table 7.16 Appearance of Discharges in Gases and Vapors at Low Pressures When Excited by a Tesla Coila
Gas |
Color Observed in Discharge |
Gas Mixed with Air |
Air (room) |
Soft violet |
Same |
Argon |
Pale magenta |
Pale magenta |
CO2 |
Greenish white |
Washed out magenta |
Helium |
Soft pink |
Purplish magenta |
Nitrogen |
Too pale for magenta, not quite |
Purple |
|
purple |
|
Oxygen |
White |
Pale magenta |
Volatile Liquid |
Color Observed in Discharge |
Gas Mixed w/ Air |
Acetone |
Turquoise (then quickly to purple) |
Void6 (then quickly to purple) |
Dichloromethane |
Bluish white |
Void* (then quickly to bluish white) |
Methanol |
Void* (then slowly to soft violet) |
Void* (then slowly to soft violet) |
a From Journal of Chemical Ed.ucation, 68, pp. 526-528, (1991 Reproduced with permission.
*Void: a lack of discharge due to a loss of vacuum.
2.The Tesla coil discharge, in leak testing, is a through-glass discharge, whereas a discharge tube is a metal-electrode discharge.
3.The distance between electrodes in a discharge tube is fixed, as opposed to the distance between the Tesla coil and ground (this distance can vary constantly from as little as several centimeters to many meters during leak detection).
4.The colors indicated in the tables are for pure gases. In a working vacuum system there will always be some air and moisture mixed with the probe gases. There will also be a trace amount of hydrocarbon vapors (from the mechanical pump) as well as other gases and vapors that incidentally may be in the system.
Work by Coyne and Cobb provided a more effective list of discharge colors because the colors were observed in the act of actual leak detection. They are presented in Table 7.16. Their work demonstrated that spraying gases had limited success in leak indication, but moderate success when the item being tested was enclosed within the gas (by way of a bag). Vapors from applied liquids provided better indicators and more easily demonstrated the specific location of a leak.
If you have items with glass-to-metal seals or metal supports you wish to leakcheck with a Tesla coil, you can encase them in a bag. Initiate a discharge with the Tesla coil while filling the bag with a test gas, such as oxygen or helium. This procedure can help to verify whether or not there is a leak. However, it will not help locate the leak. To specifically locate the leak, you may wipe a probe liquid, such as acetone on a cotton swab, over the suspected areas while a discharge is main-