- •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
420 Vacuum Systems
7.5.15 The Pirani Gauge
The Pirani gauge uses the principle that (usually) the hotter a wire gets the greater its electrical resistance. Therefore, if the resistance of a wire is going up, it must be getting hotter. This relationship implies that less air/gas is available to conduct heat away from the wire, and therefore a higher vacuum is being achieved.
The accuracy of a Pirani gauge is typically ±20%, although an individual (clean) gauge properly used over a two-year period may show a sensitivity drift of only 2%.53
One immediate complication of the Pirani gauge is ambient temperature: As the room temperature gets hotter, the filament gets hotter, making the gauge read a false "better vacuum" To solve this problem, a dummy filament is included in the Pirani gauge. The dummy filament is evacuated and sealed off (at a lower vacuum than what is likely to be used with the Pirani gauge) and is used as a standard to help calibrate a zero point.
An electrical diagram for a Pirani gauge is shown in Fig. 7.47, where V and D comprise the Pirani tube. D is the dummy filament tube that is sealed off, and V is the tube that is exposed to the vacuum system. The filaments in the V tube are connected to a bridge circuit called a Wheatstone bridge with two resistance units called Rj and R2. Power from the power supply passes across the Wheatstone bridge and is adjusted to the proper setting by R3, whose value is read on the mil-
Table 7.12 Properties of Various Gases0
Gas |
Sensitivity |
Viscosityc |
Thermal |
|
Constant* |
Conduct!vityrf |
|||
|
|
|||
Air |
1.00 |
1.80 |
0.057 |
|
Butane |
2.5 |
|
|
|
Carbon monoxide |
1.00 |
|
|
|
Carbon dioxide |
1.10 |
145 |
0.034 |
|
Helium |
1.00 |
194 |
0.344 |
|
Hydrogen |
1.30 |
87 |
0.416 |
|
Krypton |
0.45 |
|
|
|
Mercury (vapor) |
0.34 |
|
|
|
Neon |
0.90 |
310 |
0.110 |
|
Nitrogen |
1.00 |
173 |
0.057 |
|
Xenon |
0.35 |
|
|
" Adapted from Spinks, Vacuum Technology,Franklin Publishing Co., p. 22, and from Guthrie, Vacuum Technology,John Wiley & Sons., p 504 (1963).
* Sensitivity constant: These constants are accurate ± 10% over any given range of pressures.
cViscosity: At 15°C, given in micropoises.
dUnits are 103AT, where K = thermal conductivity at 0°C, cal/cm/sec/°C.
Vacuum Gauges 7.5 |
421 |
liammeter M2. The current read on Mj is proportional to the vacuum. An ammeter will read the current, which is proportional to resistance in ohms.
To set a Pirani gauge, the vacuum on V is set to a pressure lower than what the gauge can normally read. Next Ml is set on its zero point by adjusting the resistance of R2. Thereafter Mj will give proper readings as the pressure is raised to the range of the gauge.
The advantages of a Pirani gauge are as follows:
1.It has a rapid response to changes in pressure.
2.The electrical circuitry in the gauge leads to easy adaptation to recording, automatic devices, and computer sensing.
3.Electrically it is very simple.
4.It measures the pressure of permanent gases as well as vapors.
The disadvantages of a Pirani gauge are as follows:
1.Because not all gases have the same thermal conductivity, different gases will provide different pressure readings for the same pressure.
2.It is limited to the pressure range of about 10"1 to about 10~4 torr.
3.If there is any change in the filament wire's surface condition within the Pirani gauge, there will be a change in the heat loss. This change will result in a change of the gauge calibration as well as a change in the zero.
7.5.16 Cleaning Pirani Gauges
If a Pirani gauge becomes contaminated with backstreamed oil, rinsing the gauge with a suitable solvent should be sufficient. Be sure to rinse with distilled water followed by a methanol rinse. Be gentle with the gauge so as not to break the internal wire, which is fragile. Cleaning is likely to change the calibration, so be prepared to recalibrate the gauge after cleaning.
D
Supply
Fig. 7.47 Pirani gauge schematic.
422 |
Vacuum Systems |
7.5.17 The Thermocouple Gauge
The thermocouple gauge is more straightforward than the Pirani gauge and less complicated electronically. The thermocouple gauge has a thermocouple attached to a filament under constant electrical load, and it measures the temperature at all times. If the filament becomes hotter, it means that there is less air/gas available to conduct heat away from the wire, and therefore there is greater vacuum within the system.
There are two different types of thermocouple gauges: One has three wires and the other has four. Both have a dc meter (or voltmeter) that reads the voltage from the thermocouple. The three-wire unit uses ac to heat the filament wire, whereas the four-wire unit may use ac or dc. Although there are essentially no differences in performance between the two, they will likely require different controllers (or different settings) for use.
The advantages of the thermocouple gauge are fairly consistent with the four stated for the Pirani gauge with a few exceptions:
5.Thermocouple gauges can be made smaller and are more rugged than Pirani gauges.
6.Although the thermocouple gauge is subject to the same variations in apparent readings from real pressure (because of variations in the thermal conductivity of different gases), the differences are less apparent than the Pirani gauge.
The disadvantages of the thermocouple gauge are somewhat different from those of the Pirani gauge:
1.Because not all gases have the same thermal conductivity, you will get different pressure readings for the same pressure with different gases, although the differences for the thermocouple gauge are not as great as those for the Pirani gauge.
2.It is limited to the pressure range of about atmospheric to about 10"3 torn
3.The thermocouple gauge scale is nonlinear, but the readings can be accurately interpreted by the controller.
4.A thermocouple gauge should not be placed on any system with mercury unless there is strict controls set to trap and prevent the mercury from reaching the gauge. The reason for this is that the mercury can contaminate the wires of the thermocouple gauge and create false readings of a (virtual) leak (see Sec. 7.6.4).
Physical abuse, improper cleaning, and age can all cause a thermocouple to break. The symptoms may either be no response to the controller or a jerky twitching of the controller's needle. In either case, the thermocouple is not likely repairable and a new one will be necessary.
Vacuum Gauges 7.5 |
423 |
7.5.18 Cleaning Thermocouple Gauges
The thermocouple gauge is more durable than the Pirani gauge, which means that after you pour in the appropriate solvents for cleaning, you can shake the gauge for cleaning agitation. This cleaning procedure should be followed by rinses of water, distilled water, and, finally, methanol. There is no viable cleaning technique to remove mercury from a thermocouple gauge.
7.5.19 The lonization Gauge Family
All previously mentioned gauges require a certain level of particle density for operation. Once the level of particle density has dropped below a certain level (approximately 1018 particles/m3), it is not possible to detect transfer of momentum forces either from gas to solid wall or from gas to gas. On the other hand, it is possible to ionize gas particles and then "count" the ionized molecules.
A molecule in a "normal" state has a neutral charge; there is an equal number of electrons and protons. If you subject the molecule to a high amount of energy and knock out one of the electrons, the molecule is now ionized with a positive charge. This charge allows you to force the molecule to travel, bend, be focused (if necessary), and be counted. The number of (positive) ions created is always directly proportional to the molecular number density. It is only proportional to the pressure if the temperature is known and kept constant, and the type of gas being analyzed has known calibration constant for the type of gauge you are using.
There are essentially two types of ionization gauges used in the laboratory: The hotand the cold-ion gauges. A third type, the radioactive ionization gauge, is so limited in both scope and use that it will not be discussed in this book.
The concept of the ionization (ion) gauge is quite simple. Under a given electrical load, the available gas within the vicinity of the vacuum gauge is ionized either by heat or by a high-field (electrical) emission. Then, the ionized gas is collected and counted. From this count you can interpret what you have read as a unit(s) of vacuum and thereby infer the vacuum within the system.
One ironic peculiarity of ion gauges is that the ions collected by the gauges for counting are not re-released to the vacuum system and therefore are bound up as in getter pumps. Therefore an ion gauge also acts as a pump. This feature itself sounds great: What vacuum system couldn't use a little extra pumping? However, this feature adds an accuracy problem because there is no way of knowing whether the vacuum within the confines of the gauge (where active pumping is going on) and the vacuum within the rest of the system is the same. Thus, to maintain accuracy between the pressure within the gauge and within the system, the gauge should not be left on for extended periods of time and the gauge should be connected to the system with large-diameter tubing. This setup decreases the opportunities for a pressure gradient to be established and facilitates equalization between the gauge and the system if a gradient condition occurs.
Hot-cathode gauges are considered fast pumps, but cold-cathode gauges pump 10 times faster. At 10"10 torr there are only 106 molecules per cubic centimeter. If