
- •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
406 Vacuum Systems
7.5.4 The Liquid Gauge Family
The liquid gauge family is identified simply as vacuum gauges that have some liquid (usually mercury or a low-vapor-pressure diffusion pump oil) directly in contact with the vacuum. The amount of liquid movement is directly proportional to the force exerted on it, and the (measured) amount of movement is read as the vacuum. Because mercury has traditionally been used for vacuum measurement, the term "millimeters of mercury" is commonly used even with nonliquid gauges.
Low-vapor-pressure oils can be substituted for some operations, but calibrations for density must be made so that their measurements can be interpreted as millimeters of mercury, torr, or Pa. Unfortunately, vacuum measurements can take a considerable amount of time when using oil because it takes a long time for a film of oil to settle from the walls of a manometer.
Despite the limitations and problems that the liquid gauge family presents, perhaps the biggest problem with the liquid gauge family is that its members can be very difficult to keep clean because the liquid is in direct contact with materials in the vacuum system. As mercury becomes dirty or contaminated, it tends to stick to the walls of glass tubing, thus decreasing its accuracy. As oil becomes dirty, its density can change and may provide inaccurate measurements. Realistically though, any vacuum system whose upper range is 10"3 torr is not likely to be significantly affected by limited contamination.
On the other hand, a liquid trap is essential between any liquid vacuum gauge and the manifold itself. The simplest accident can cause hours of needless delay as the vacuum line is cleaned out. Normally a simple splash trap is sufficient (see Sec. 7.4.6). Vacuum systems that go below 1(T5 torr should consider to have a cold trap placed between their liquid vacuum gauges and vacuum systems. This placement will keep vapors from contaminating either side of the system.
When a vacuum system is first started and brought from atmospheric pressure to a vacuum state, parts within the vacuum system need to be outgassed. When liquids are outgassed, they boil. This process needs to be done slowly, otherwise the liquids will "bump" (boil) violently, possibly causing the mercury (or oil) to splash across the system. This splashing could waste some time minimally by trying to get the liquid back into the gauge, or more time by requiring the system to be cleaned up; maximally, an extended period of time could be wasted by breaking the system. Therefore, slowly open the stopcock to your liquid manometer for outgassing (Sec. 7.5.8 provides specific information on how to let the liquid outgas in a McLeod gauge). It is not necessary to open the stopcock all the way to full open. If the stopcocks to the liquid vacuum gauge are kept closed to atmospheric pressures, the outgassing process needn't be repeated. However, if the gauge is brought to atmospheric pressure for an extended time (about a day), gases can re-enter the gauge and the full outgassing process must be repeated.
Vacuum Gauges 7.5 |
407 |
7.5.5 The Manometer
Second only to the mechanical gauge as the easiest device to measure and read a vacuum (and decidedly easiest in construction) is the liquid manometer (see Fig. 7.37). A well-made mercury manometer, kept very clean, can measure vacuums of up to 10"3 torr. This sensitivity can be increased by up to 15 times if a liquid with less density, such as diffusion pump oil, is used. However, diffusion pump oil is far more difficult to keep clean and can require either (a) a very tall (and thereby impractical) column or (b) a manometer of very limited range. In addition, because of the strong surface tension between diffusion pump oil and glass, long waiting periods between readings are required as the oil settles into place.
The mechanics of a U-tube manometer are simple: "The difference between the levels of two interconnected columns of liquid is directly proportional to the difference between the pressures exerted upon them, assuming equal capillary effects on both tubes."46 In practice, one end of a manometer is attached to an unknown pressure, and the other end is attached to a reference pressure that is known. For all practical purposes, the known value needs only to be a much smaller order of magnitude than the unknown value.
By maintaining a manometer at a constant temperature, the liquid within will maintain a consistent density. From 0° to 30°C the density of mercury changes about 0.5%. Therefore, a consistent reading of accurate vacuums can only come from a consistent room temperature. Manometer reading techniques (see Fig. 7.38) are consistent and simple regardless of the design and type of manometer. All that is necessary is some basic subtraction, a good metric ruler, and a steady eye. The manometer is read by observing and measuring the difference of the mercury column heights within the manometer.
To the system |
To the system |
Open |
Closed |
Manometer |
Manometer |
Fig. 7.37 Open manometers are used to measure pressures relative to atmospheric whereas closed manometers are used for pressures far smaller than atmospheric. From Vacuum Science and Engineering, Fig. 3-1, by C. Van Atta, © 1965 by McGraw-Hill, New York, reproduced with permission.
408 |
Vacuum Systems |
Fig. 7.38 In this example, take the measurement from the closed side (439 mm) of the manometer, and subtract from it the measurement from the side of the manometer connected to the vacuum system (426 mm) to obtain the vacuum reading (13 mm Hg). Remember, avoid parallax problems, and with mercury, read the top of the meniscus.
The choice of mercury for manometers is often a matter of convenience, or rather the acceptance of the least amount of inconvenience. Mercury has a rather high vapor pressure (10~3 torr), but this vapor pressure is also at the upper ranges of what can be read by a manometer. Low-vapor-pressure oils (as used in diffusion pumps) can be used, but these oils wet the walls of a manometer and can take a long time to settle before reading can be made. Mercury is fairly nonreactive and retains a limited amounts of condensable vapors.
One of the biggest reasons why mercury is used is because it is a very heavy liquid. Atmospheric pressure can only push mercury about 76 cm, while it pushes water some 30 feet. Manometers using lighter-density liquids can be so tall they become beyond inconvenient. Additionally, because mercury doesn't wet the glass walls of the manometer, there is never a time lag for reading as there is with oil.
Fortunately, the mechanics of reading manometers is generally irrelevant to the amount of mercury (or any other liquid) within the device. Reading manometers can be difficult because of parallax problems. This difficulty can be complicated by the fact that manometers lack lines encircling them like burettes. Carroll found that by placing graph paper behind a mercury manometer, it was possible to see problems of parallax by the line's reflection off the glass and mercury (see Fig. 7.39).
For very accurate manometer readings, the NIST (National Institute of Standards and Testing) has a compiled list of eight possible errors that can develop while reading manometers.48 These errors introduce extremely small variations and therefore are not included here. If you need to read a manometer to the sensi-
Vacuum Gauges 7.5 |
409 |
Eye |
Eye |
Eye |
Below |
Level |
Above |
Fig. 7.39 Using graph paper lines to help avoid parallax problems while reading manometers. From the Journal of Chemical Education, 44, p. 763 (1967), reproduced with permission.
tivity required for these variations to show up, it is better to use a different gauge type with higher sensitivity.
At first glance, it seems that one ought to be able to attach a vacuum line 77 or 78 cm above the lowest part of a gauge because at STP it is not possible for a vacuum to pull mercury any higher than 76 cm. While it is true that a vacuum cannot pull mercury higher than 76 cm, momentum can. If the mercury is being outgassed or there is an unexpected pressure surge, momentum can carry the mercury farther than your worst nightmares. Therefore, always include a liquid trap on all liquid systems (see Sec. 7.4.6).
7.5.6 The McLeod Gauge
Rather than using mercury as a piston that is pushed about by the forces within a vacuum system, the McLeod gauge traps a known volume of gas of unknown pressure and compares it to a known volume of gas at a known pressure using Boyle's law:
|
|
P0V0 = PtVf |
(7.13) |
|
where |
Po |
is the original pressure |
|
|
|
Vo |
is the original volume |
|
|
|
Pf |
is the final |
pressure |
|
|
Vf |
is the final |
volume. |
|
The advantages of the McLeod gauge are as follows:
1.The wide range of pressures it can read.
2.Its great accuracy (McLeod gauges are used to calibrate electronic gauges).
3.Readings are unaffected by the type of gas species within the system (although condensable vapors can affect readings).
The disadvantages of the McLeod gauge are as follows:
1. It can only read the pressure at single points in time, not continuously as
410 |
Vacuum Systems |
can mechanical or electronic gauges.
2.The McLeod gauge uses mercury, which can be a nuisance because the gauge is difficult to clean and may be illegal in some areas. In addition, backstreamed mercury can sometimes affect your work.
3.The McLeod gauge has no ability to compensate for condensable vapors.
McLeod gauges are always made of glass. Figure 7.40 shows two typical McLeod gauge designs. There are many different configurations and designs of the standard McLeod gauge, but all have the same general configuration:
1.A lower bulb for mercury storage.
2.An upper bulb whose volume has been accurately determined.
3.One capillary tube extending from the vacuum bulb with its other end fused shut (in Fig. 7.40 it is labeled Capillary B).
4.A second capillary tube (in Fig. 7.40, it is labeled Capillary A), both ends of which are attached to a larger tube.
5.A larger tube which connects the McLeod to the vacuum system.
Ideally, the McLeod gauge should only be open to the system when a vacuum reading is being made to limit the amount of mercury vapors back-streamed into the vacuum system as well as the amounts of materials that drift into (and contaminate) the McLeod gauge from the system. The mercury in a McLeod gauge must be kept clean because dirty mercury tends to stick on the walls of the capillary tubing and leave trails that prevent accurate readings. It is much easier to keep the mercury in a McLeod gauge clean than it is to clean the capillaries of a McLeod gauge.
A liquid trap can be placed between the McLeod gauge and the rest of the system to prevent mercury from accidentally spraying throughout your system. If you do not want condensable vapors affecting the McLeod gauge readings or do not want mercury vapors to enter your system, a cold trap can be placed between the liquid trap (shown in Fig. 7.41) and the main vacuum line.
Unfortunately, placing traps between the McLeod gauge and vacuum system increases the time needed to make a reading because the physical restrictions decrease the throughput and increase the time for gas equilibration. The efficiency lost by slower McLeod gauge readings (due to traps) must be balanced by other needs such as limiting the amount of mercury that gets into your system and/or keeping condensable gases out of the McLeod gauge.
An interesting problem occurs when a liquid nitrogen cold trap is placed between the system and McLeod gauge. The cold trap becomes a cryopump and draws mercury vapor from the gauge. This effect, called "mercury streaming," effectively limits the number of molecules that can enter the gauge (like salmon trying to swim upstream), and inaccurately low readings may result. Only readings in vacuums less than 10"4 torr are significantly affected, and atoms of higher