- •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
THE LABORATORY COMPANION
THE LABORATORY COMPANION
A Practical Guide to Materials, Equipment, andTechnique
Gary S. Coyne
California State University at Los Angeles
A WILEY-INTERSCIENCE PUBLICATION
JOHN WILEY & SONS, INC.
New York • Chichester • Weinheim • Brisbane • Singapore • Toronto
This text is printed on acid-free paper. ©
Copyright © 1997 by John Wiley & Sons, Inc. All rights reserved.
Published simultaneously in Canada.
No part of this publication may be reproduced, stored in a retrieval system or transmitted in any form or by any means, electronic, mechanical, photocopying, recording, scanning or otherwise, except as permitted under Sections 107 or 108 of the 1976 United States Copyright Act, without either the prior written permission of the Publisher, or authorization through payment of the appropriate per-copy fee to the Copyright Clearance Center, 222 Rosewood Drive, Danvers, MA 01923, (508) 750-8400, fax (508) 750-4744. Requests to the Publisher for permission should be addressed to the Permissions Department, John Wiley & Sons, Inc., 605 Third Avenue, New York, NY 10158-0012, (212) 850-6011, fax (212) 850-6008, E-Mail: PERMREQ@WILEY.COM.
Library of Congress Cataloging in Publication Data:
Coyne, Gary S.
The laboratory companion : a practical guide to materials, equipment, and technique / Gary S. Coyne,
p.cm.
Rev. ed. of: The laboratory handbook of materials, equipment, and technique. cl992.
"A Wiley-Interscience publication."
Includes bibliographical references and index. ISBN 0-471-18422-5 (alk. paper)
1. Chemical apparatus—Handbooks, manuals, etc. 2. Chemical laboratories—Handbooks, manuals, etc. I. Coyne, Gary S. Laboratory handbook of materials, equipment, and technique.
II. Title. QD53.C69 1998 542—dc21
Printed in the United States of America 10 9 8 7 6 5 4 3 2
/ dedicate this book to my wife, Mara.
If you want to find out if your spouse loves you, write a book. I am a lucky person: my wife loves me, and I have this book and our still-successful marriage to prove it. If she didn 't love me, I still might have this book, but the marriage would have been gone long ago.
Contents
Foreword |
|
xv |
|
Preface |
|
|
xvii |
1 Materials in the Lab |
1 |
||
1.1 |
Glass |
|
1 |
|
1.1.1 |
Introduction |
1 |
|
1.1.2 |
Structural Properties of Glass |
1 |
|
1.1.3 |
Phase Separation |
5 |
|
1.1.4 |
Devitrification |
7 |
|
1.1.5 |
Different Types of Glass Used in the Lab |
9 |
|
1.1.6 |
Grading Glass and Graded Seals |
18 |
|
1.1.7 |
Separating Glass by Type |
19 |
|
1.1.8 |
Physical Properties of Glass and Mechanisms of Glass Fracture |
22 |
|
1.1.9 |
Stress in Glass |
26 |
|
1.1.10 |
Managing Thermal and Physical Stress in the Laboratory |
28 |
|
1.1.11 |
Tempered Glass |
31 |
|
1.1.12 |
Glass and Internal Pressure |
33 |
|
1.1.13 |
Limiting Broken Glass in the Lab |
36 |
|
1.1.14 |
Storing Glass |
37 |
|
1.1.15 |
Marking Glass |
38 |
|
1.1.16 |
Consumer's Guide to Purchasing Laboratory Glassware |
39 |
1.2 |
Flexible Tubing |
41 |
|
|
1.2.1 |
Introduction |
41 |
|
1.2.2 |
Physical Properties of Flexible Tubing |
42 |
|
1.2.3 |
Chemical Resistance Properties of Flexible Tubing |
45 |
1.3 |
Corks, Rubber Stoppers, and Enclosures |
49 |
|
|
1.3.1 |
Corks |
49 |
|
1.3.2 |
Rubber Stoppers |
50 |
|
1.3.3 |
Preholed Stoppers |
51 |
|
1.3.4 |
Inserting Glass Tubing into Stoppers |
55 |
|
1.3.5 |
Removing Glass from Stoppers and Flexible Tubing |
57 |
|
1.3.6 |
Film Enclosures |
57 |
1.4 |
O-Rings |
58 |
|
|
1.4.1 |
O-Rings in the Laboratory |
58 |
|
1.4.2 Chemical Resistance of O-Ring Material |
58 |
|
|
1.4.3 |
O-Ring Sizes |
59 |
References |
|
63 |
|
|
|
|
vii |
viii |
Contents |
|
|
2 Measurement |
65 |
||
2.1 |
Measurement: The Basics |
65 |
|
|
2.1.1 |
Uniformity, Reliability, and Accuracy |
65 |
|
2.1.2 |
History of the Metric System |
66 |
|
2.1.3 |
The Base Units |
71 |
|
2.1.4 |
The Use of Prefixes in the Metric System |
76 |
|
2.1.5 |
Measurement Rules |
76 |
2.2 |
Length |
|
79 |
|
2.2.1 |
The Ruler |
79 |
|
2.2.2 |
How to Measure Length |
79 |
|
2.2.3 |
The Caliper |
80 |
|
2.2.4 |
The Micrometer |
83 |
2.3 |
Volume |
85 |
|
|
2.3.1 |
The Concepts of Volume Measurement |
85 |
|
2.3.2 |
Background of Volume Standards |
85 |
|
2.3.3 |
Categories, Markings, and Tolerances of Volumetric Ware |
87 |
|
2 3.4 |
Materials of Volumetric Construction #1 Plastic |
89 |
|
2.3.5 |
Materials of Volumetric Construction #2 Glass |
91 |
|
2.3.6 |
Reading Volumetric Ware |
93 |
|
2.3.7 |
General Practices of Volumetric Ware Use |
94 |
|
2.3.8 |
Calibrations, Calibration, and Accuracy |
95 |
|
2.3.9 |
Correcting Volumetric Readings |
97 |
|
2.3.10 |
Volumetric Flasks |
101 |
|
2.3.11 |
Graduated Cylinders |
104 |
|
2.3.12 |
Pipettes |
107 |
|
2.3.13 |
Burettes |
113 |
|
2.3.14 |
Types of Burettes |
115 |
|
2.3.15 |
Care and Use of Burettes |
116 |
2.4 |
Weight and Mass |
118 |
|
|
2.4.1 |
Tools for Weighing |
118 |
|
2.4.2 |
Weight Versus Mass Versus Density |
119 |
|
2.4.3 |
Air Buoyancy |
120 |
|
2.4.4 |
Accuracy, Precision, and Other Balance Limitations |
122 |
|
2.4.5 |
Balance Location |
123 |
|
2.4.6 |
Balance Reading |
125 |
|
2.4.7 |
The Spring Balance |
127 |
|
2.4.8 |
The Lever Arm Balance |
128 |
|
2.4.9 |
Beam Balances |
131 |
|
2.4.10 |
Analytical Balances |
132 |
|
2.4.11 |
The Top-Loading Balance |
136 |
|
2.4.12 |
Balance Verification |
137 |
|
2.4.13 |
Calibration Weights |
139 |
2.5 |
Temperature |
144 |
|
|
2.5.1 The Nature of Temperature Measurement |
144 |
|
|
2.5.2 |
The Physics of Temperature-Taking |
147 |
|
2.5.3 |
Expansion-Based Thermometers |
150 |
|
|
Contents |
ix |
|
2.5.4 |
Linear Expansion Thermometers |
151 |
|
2.5.5 |
Volumetric Expansion Thermometers |
151 |
|
2.5.6 |
Short-and Long-Term Temperature Variations |
156 |
|
2.5.7 |
Thermometer Calibration |
157 |
|
2.5.8 |
Thermometer Lag |
158 |
|
2.5.9 |
Air Bubbles in Liquid Columns |
158 |
|
2.5.10 |
Pressure Expansion Thermometers |
160 |
|
2.5.11 |
Thermocouples |
161 |
|
2 5.12 |
Resistance Thermometers |
167 |
References |
|
170 |
|
3 Joints, Stopcocks, and Glass Tubing |
173 |
||
3.1 |
Joints and Connections |
173 |
|
|
3.1.1 |
Standard Taper Joints |
173 |
|
3 1.2 |
Ball-and-Socket Joints |
178 |
|
3.1.3 |
The O-Ring Joint |
179 |
|
3.1.4 |
Hybrids and Alternative Joints |
180 |
|
3.1.5 |
Special Connectors |
181 |
3.2 |
Stopcocks and Valves |
184 |
|
|
3.2.1 |
Glass Stopcocks |
184 |
|
3.2.2 |
Teflon Stopcocks |
187 |
|
3.2.3 |
Rotary Valves |
189 |
|
3.2.4 |
Stopcock Design Variations |
191 |
3.3 Maintenance and Care of Joints, Stopcocks, and Glassware |
192 |
||
|
3.3.1 Storage and Use of Stopcocks and Joints |
192 |
|
|
3.3.2 |
Preparation for Use |
196 |
|
3.3.3 |
Types of Greases |
196 |
|
3.3.4 |
The Teflon Sleeve |
203 |
|
3.3.5 |
Applying Grease to Stopcocks and Joints |
203 |
3.3.6Preventing Glass Stopcocks and Joints from Sticking
|
|
or Breaking on a Working System |
204 |
|
3.3.7 |
Unsticking Joints and Stopcocks |
205 |
|
3.3.8 |
Leaking Stopcocks and Joints |
208 |
|
3.3.9 |
What to Do About Leaks in Stopcocks and Joints |
211 |
|
3.3.10 |
General Tips |
212 |
3.4 |
Glass Tubing |
212 |
|
|
3.4.1 |
The Basics of Glass Tubing |
212 |
|
3.4.2 |
Calculating the Inside Diameter (I.D.) |
213 |
|
3.4.3 |
Sample Volume Calculations |
215 |
References |
|
229 |
|
4 Cleaning Glassware |
231 |
||
4.1 |
The Clean Laboratory |
231 |
|
|
4.1.1 |
Basic Cleaning Concepts |
231 |
|
4.1.2 |
Safety |
234 |
x |
Contents |
|
|
|
|
4.1.3 |
Removing Stopcock Grease |
|
236 |
|
4.1.4 |
Soap and Water |
|
236 |
|
4.1.5 |
Ultrasonic Cleaners |
|
238 |
|
4.1.6 |
Organic Solvents |
|
239 |
|
4.1.7 |
The Base Bath |
|
240 |
|
4.1.8 |
Acids and Oxidizers |
|
242 |
|
4.1.9 |
Chromic Acid |
|
244 |
|
4.1.10 |
Hydrofluoric Acid |
|
245 |
|
4.1.11 |
Extra Cleaning Tips |
|
248 |
|
4.1.12 |
Additional Cleaning Problems and Solutions |
|
249 |
|
4.1.13 |
Last Resort Cleaning Solutions |
|
250 |
References |
|
|
251 |
|
5 Compressed Gases |
|
253 |
||
5.1 |
Compressed Gas Tanks |
|
253 |
|
|
5.1.1 |
Types of Gases |
|
253 |
|
5.1.2 |
The Dangers of Compressed Gas |
|
254 |
|
5.1.3 |
CGA Fittings |
|
256 |
|
5.1.4 Safety Aspects of Compressed Gas Tanks |
|
257 |
|
|
5.1.5 |
Safety Practices Using Compressed Gases |
|
269 |
|
5.1.6 |
In Case of Emergency |
|
272 |
|
5.1.7 |
Gas Compatibility with Various Materials |
|
273 |
5.2 |
The Regulator |
|
278 |
|
|
5.2.1 |
The Parts of the Regulator |
|
278 |
|
5.2.2 |
House Air Pressure System |
|
281 |
|
5.2.3 |
How to Install a Regulator on a Compressed Gas Tank |
|
281 |
|
5.2.4 |
How to Use Regulators Safely |
|
283 |
|
5.2.5 |
How to Test for Leaks in a Compressed Gas System |
|
283 |
|
5.2.6 |
How to Purchase a Regulator |
|
284 |
6 High and Low Temperature |
|
287 |
||
6.1 |
High Temperature |
|
287 |
|
|
6.1.1 The Dynamics of Heat in the Lab |
|
287 |
|
|
6.1.2 |
General Safety Precautions |
|
288 |
|
6.1.3 |
Open Flames |
|
288 |
|
6.1.4 |
Steam |
|
292 |
|
6.1.5 |
Thermal Radiation |
|
294 |
|
6.1.6 |
Transfer of Energy |
|
294 |
|
6.1.7 |
Hot Air Guns |
|
295 |
|
6. 1.8 |
Electrical Resistance Heating |
|
296 |
|
6.1.9 |
Alternatives to Heat |
|
300 |
6.2 |
Low Temperature |
|
301 |
|
|
6.2.1 |
The Dynamics of Cold in the Lab |
|
301 |
|
6.2.2 |
Room Temperature Tap Water (=20°C) |
|
302 |
|
6.2.3 |
Ice(0°C) |
. |
302 |
|
6.2.4 |
Ice with Salts (0°C to -96.3°C) |
|
302 |