
- •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
Weight and Mass 2.4 |
127 |
object will appear heavier than it really is. Conversely, if the container and balance are oppositely charged, they will attract and the object will appear lighter than it really is. There are several ways to prevent this problem13:
1.Use a humidifier to increase the humidity to between 45% and 60%,
2.Place weighing vessels in a metal container to screen electrostatic forces.
3.Use an appropriate weighing vessel (plastic is poor, glass is good, and metal is best) to avoid electrostatic forces.
4.Anti-static guns are commercially available, but they should not be relied on.
5.The balance is likely to be grounded through the power cord's third wire. Therefore do not bypass this wire if using an extension cord. Be sure to use a three-wire extension cord and an appropriate wall socket.
Although the need to calibrate (see Rule 12) a balance that was moved to a different table is just to verify that nothing got misaligned, the changes in gravity forces of a balance moved cross-country can be significant. Likewise, a balance move in a vertical motion some 10 meters can show signs of miscalibration. Aside from the need to recalibrate a balance to counter the effects of changing gravity, the wear and tear of moving balances should be enough reason to not move a balance any more than necessary.
2.4.7 The Spring Balance
A spring balance compares two different forces (gravitational attraction vs. tensile forces of the spring) to weigh an object. Assuming that the tensile forces of a spring balance remain constant, as any inertial forces (i.e., gravity) change, weight readings will change. A spring balance therefore is typically used to illustrate differences in weight when the gravitational effects of celestial bodies are compared. A lever arm (pan) balance compares the same force and thereby cannot reflect changes in gravity.
Unfortunately, metal spring balances suffer from a variety of problems. For instance, the spring in a balance can suffer from hysteresis (extended beyond the point of resiliency, the spring cannot return back to its original position). In addition, very accurate spring balances need to be calibrated for changes in gravity depending on where on the Earth they are being used.
Perhaps the biggest problem with spring balances is that the linear motion of the spring is typically converted to some type of circular motion for reading the weight. Such gear reductions introduce friction, which decreases readability, pre-
128 |
Measurement |
cision, and accuracy. Linear spring balances, such as those used for weighing fish on a boat, also have built-in friction from the parts that rub on the scale face.
Despite their general lack of accuracy, their popularity is understandable. Their limited accuracy and reliability are more than sufficient, however, for the demands of grocery stores or bathroom scales. To use anything more complicated or expensive when the need is not justified is a waste of time and money.
There is an interesting story, from the gold rush days, about people taking advantage of the inaccuracies peculiar to the spring balance. As you go from the north or south pole toward the equator, the centrifugal force caused by the earth spinning increases, which counter-effects the force of gravity. In addition, the earth is somewhat oblate (due to centrifugal force) and the effects of gravity are somewhat less at the equator because the earth's surface is farther from the earth's center. Thus, using a spring balance, an object weighs less at the equator than it does at a pole. During the California gold rush, some people would purchase gold in California, using a spring balance for weight measurement, and sell the same gold in Alaska using the same balance. Because the gold weighed more in Alaska, it was worth more. Thus, a (good) living was made by buying and selling gold at the same price per ounce. Such a practice would not be possible with a two-pan balance.
Some highly accurate spring balances are typically made out of fused silica (quartz glass) and used in vacuum systems. The use of fused silica has two advantages. For one, the material is extremely nonreactive. Thus it is unlikely to corrode as a metal might when in contact with acids and/or oxidizers. In addition, glass is considered perfectly elastic until the point of failure. Thus, there are no hysteresis problems.
These balances simply are a hanging coil of fused silica with a glass basket on the bottom. An optical device with a calibrated vertical measurement system sights on a point on the glass basket. A calibrated weight is placed within the basket, and the optical device is moved down so the system can sight on the same point and the new calibration is noted. Several more weight measurements are made to verify linearity. By observing the amount of spring travel for a given amount of weight, very accurate measurements can be made. Unfortunately, the amount and type of supporting equipment for this type of spring balance are expensive.
2.4.8 The Lever Arm Balance
The lever arm balance compares the mass of an object to the mass of calibrated weights. There are two major types of lever arm balances. The equal arm balance [see Fig. 2.23(a)] works by directly comparing a known weight to an unknown weight, both of which are placed an equal distance from the fulcrum. Once in balance, there is a one-to-one ratio (of the weights) between the unknown and known weights. A well-made balance of this type is capable of high accuracy and preci-
Weight and Mass 2.4 |
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129 |
Pivot |
|
|
|
point |
Fulcrum |
Fulcrum |
|
(a) |
Equal arm |
y |
(b) Unequal arm |
|
balance |
balance |
|
|
|
Fig. 2.23 Two basic lever arm designs.
sion. The disadvantage of this type of balance is that many standard weights are needed to provide the balance with its full range of weighing capabilities.
The unequal arm balance [see Fig. 2.23(b)] compares an unknown weight to the distance a known weight is to the fulcrum. When weighing an object, the further the balance weight is moved from the fulcrum, the heavier the object. The primary advantage of the unequal arm balance is that it needs only a limited number of calibrated weights. The disadvantage of this type of balance is that its accuracy is limited by how many divisions can accurately be defined between the units on the balance arm.
Another problem of the equal arm balance is ensuring that the weight is directly under its pivot point. This alignment is important because the pivot point helps define how far the weight is from the fulcrum. As the unequal arm balance demonstrates, variations in the distance a weight is from the fulcrum can change its effective weight. In the 17th century, a mathematician named Roberval devised a balance arm that guaranteed that weights would act as if they were under the pivot point, regardless of how far they were placed from the fulcrum. The basic configuration of a balance utilizing the Roberval principle is shown in Fig. 2.24, and the
Pivot |
Fulcrum |
|
Axis - |
||
|
\
Fig. 2.24 The Roberval principle balance. From The National Bureau of Standards Handbook 94, Figure 5, "The Examination of Weighing Equipment" by M.W. Jensen and R.W. Smith.,U.S. Printing Office, 1965, p. 155. Reprinted courtesy of the national Institute of Standards and Technology, Technology Adminstration, U.S. Department of Commerce. Not copyrightable in the United States.
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Measurement |
Fig. 2.25 Applications of the Roberval principle used with top loading balances.* From The National Bureau of Standards Handbook 94, Figure 6, "The Examination of Weighing Equipment" by M.W. Jensen and R.W. Smith, U.S. Printing Office, 1965, p. 155. Reprinted courtesy of the national Institute of Standards and Technology, Technology Adminstration, U.S. Department of Commerce.
Roberval principle used in equal and unequal style top-loading balance designs is shown in Fig. 2.25.
The advantage of the Roberval principle balance is that the placement of the weights has no effect on weight readings because the momentum of the weights is transferred to (and located at) the pivot axis. As far as the functions of the balance are concerned, the effective location of the weight is at the pivot axis regardless of its real location. The Roberval principle is used on all top-loading balances and many pan balances. The major drawback to this system is that it doubles the axis points and therefore doubles the friction on the system, which can reduce the balance's sensitivity.
The pivot axes of laboratory balances are not drawn correctly in either Fig. 2.24 or Fig. 2.25, but instead are either a knife edge or flexural pivot as shown in Fig. 2.26. The knife edge has the advantage of freedom of movement and no inherent restrictions. Its disadvantage is that its edge can wear or collect dust at its edge contact point. Either of these conditions causes friction, decreasing the accuracy and reliability of the balance. Static electricity can also reduce the freedom of movement of a knife edge.
The flexural pivot is free of the problems associated with the knife edge. However, it can act as a spring and therefore may add an extra force to the weighing process. This force may artificially subtract from an object's true mass and provide inaccurate readings. This effect may arise as a result of time or as temperature changes.* Manufacturing design may decrease this effect, and it may also be
(a) Knife edge |
(b) Flexural pivot |
Fig. 2.26 Pivot axes.
The flexural pivot may become more or less stiff due to time and/or temperature.