- •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 |
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Neglect or abuse can damage a balance resulting in no deflection for the original smallest units. The result is a change in the readability for the damaged balance to a new, and larger, value.
Linearity is the ability of a balance to accurately read the entire range of weights that it was designed to weigh. A balance which accurately weighs 10 mg, but poorly weighs 100 mg, but again accurately weighs 200 mg on up to its full-scale calibration, is said to have poor linearity.
Off-center errors are problems specifically associated with top-loading balances. Placing a balance pan above the fulcrum places different torques and friction on balance pieces that do not exist when a balance pan hangs. The problem is exhibited if an object has different weight readings when moved to various locations across the surface of a top-loading balance pan.
Accuracy is the ability of a balance to precisely and repeatedly read a weight. The ability for a balance to read a particular weight is based not only on the above attributes and characteristics, but also on three other factors:
1.The quality of the machine
2.The quality of the weighing process conditions [typically dependent upon the balance's location (see Sec. 2.4.5)]
3.The skill of the person operating the balance
Each of these factors is dependent on the other two, and the failure of any one of them can affect the accuracy of a weighing. For example, do not expect great accuracy from a balance that is located above a radiator. Likewise, do not expect accuracy from a balance which has just demonstrated poor precision. Finding the source of errors in weighing is a step-by-step process. You must rule out each problem before moving on to the next level.
2.4.5 Balance Location
By their nature, balances are fragile pieces of equipment. The more sensitive a balance is, the more susceptible it is to environmental influences. The following should be considered before placing permanently in any location:
1. Balances should be away from sources of vibration. Rooms used for balance work should be away from elevators and ventilation motors. They should be located near support walls (as opposed to walls that just separate rooms), which can help dampen vibration. To observe the amount of vibration your balance is receiving, lay small dishes of water at several locations on the supporting table you plan to use and float microscope cover slips on the surface of the water in each dish. Shine a light on each cover slip in turn, such that the light is reflected onto an adjacent wall. Make observations over several times during the day. Have someone walk around the room, close or open the door, and perform other activities that may cause vibrations. The more sta-
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ble the light's reflection, the better the table (and location) will be for weighing purposes.
2.Balances should be away from winds and drafts. Many buildings have sealed windows, but vents can generate drafts as well. Although fume hoods generally do not create a significant draft, opening and closing doors can.
3.Balances should be placed away from sources of varying temperature, including direct sunlight, windows, heaters, vents, drying ovens, refrigerators, doors, and rooms on the south side of buildings.
4.Balances should be kept away from rapid changes in humidity such as those that occur when steam heaters are used. Not only will steam heaters affect temperature, the change in humidity can affect the workings of the balance.
5.Balances should be kept away from stored chemicals, especially those with low vapor pressures. Because most of the internal workings of modern balances are not in plain sight, you will not be aware of any corrosion until the balance begins to malfunction. At that point, it may be too late to remedy the situation.
6.Hanging balance pans should be removed before balances are moved from one location to another to take the strain off the beam balance points as well as to prevent a swinging pan from damaging the balance.
7.Balances should be recalibrated after they have been moved.
8.Balance rooms should be maintained free of dust. Dust can affect both mechanical and electronic balances.
9.Balances should be placed on nonmagnetic, nonferrous surfaces. Cement, stone, and wood are all acceptable.
If, after reading these rules, you conclude that the best place for a balance is in a special room by itself, you are right. Such a room ideally should be windowless, with one separate, shielded entry and filtered, baffled vents. The room should be small, with support beam walls and very heavy benchtops, and should be maintained consistently at 20°C.
In lieu of a perfect room, the specific problems your room presents should be known to protect the validity of your weighing as much as possible. For example, if you are having problems limiting your vibration sources, make your weighings at odd hours when elevators are not in use or when people are unlikely to enter the
Weight and Mass 2.4 |
125 |
room. For drafts, baffle vents, place screens around the balance, or use other similar stop-gap measures.
2.4.6 Balance Reading
Consider the following scenario: Many people each make one reading on the same balance, using the same weight for each reading. All readings are within one-hundredth of a gram except that of one user, whose reading was one-tenth of a gram off. It is safe to assume that the user does not know how to use, or read, that particular balance or how to make an accurate weighing on any balance. Either way, this user needs some help in balance use.
To best examine a person's ability to use a balance, have him or her make multiple weighings (e.g., 10 times) using the same balance and weight. If he or she consistently makes the same type of error, the readings will have very little variation. If he or she makes a variety of random errors, the readings will vary with no consistent pattern or be caused by not preventing the effects of electrostatic forces (see Rule 11 below).
It is impossible to provide instruction for all types of balances in a book such as this one. However, it is possible to provide simple, generic, general rules for the operation of a balance. These general guidelines for balance operation are the same regardless of the specific type of balance:
1.Never force a lever, pan, door, or other part of a balance. If balance parts do not move smoothly and easily, there is probably a reason, and brute force will not be the cure.
2.Never drop a weight or a sample, or let one fall on any part of the balance (for that matter, do not drop a weight or sample at any time).
3.Never handle a calibration weight with your fingers. Even if the tolerances you are working with are well above the limits for weighing a fingerprint, the oils from your skin could corrode the weights. Besides, if you get in the habit of handling low-quality weights (see Sec. 2.4.12) with your fingers, you are likely to continue the habit with high-quality weights.
4.Never handle an object to be weighed with your fingers when making analytical weighings, because your fingerprints will alter the weight. Use tongs or tweezers.
5.Never let a spill sit. Keep some paper towels within reach of a balance to help mop up any spill immediately. Such a spill may pose a health danger or could damage the balance.
6.Never place or remove a weight on a balance without first verifying that the pans or trays are in the arrested position—that is, the pan(s) are securely supported and cannot move. Otherwise the action could cause the blades to slip from their pivot points and/or damage the blades.
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7. Never move, twist, or turn any part of the balance with a quick jerky motion. The balance is a delicate machine and such actions could cause the blades to slip from their pivot points and/or damage the blades.
8.Never place a powder or liquid directly on any part of the balance. Aside from the difficulty in completely removing the entire weighed sample, there is the danger of the material being corrosive to the balance pan, or the powder drifting off, or the liquid dripping off into the balance's mechanical sections. There should always be glass, a weighing pan, or weighing paper between the object and the balance.
9.Never rush. Allow time for the object to reach the balance room's ambient temperature. One way to verify such a temperature alignment is to put a comparable material and thermometer into a dummy vessel. When the material in the dummy vessel reaches ambient temperature, the weighing sample is also likely to be at an acceptable temperature.
10.Never leave a single-pan balance without first setting the pan(s) to the arrested position, and then turning the weights back to zero. Otherwise the constant pressure prematurely ages the balance's mechanical parts.
11.Never weigh objects (particularly powders or granules) if the air is dry (<40% relative humidity), and never use plastic containers.
12.Never take the calibration of a balance for granted. Likewise, the balance should be calibrated each time it is moved regardless of whether it was across the country, to a different building, or to a different table.
There are some interesting quirks as to why temperature (Rule 9) is important to weighings made on an analytical balance. Heat has some seemingly strange effects on the weight of an object. An object that is hot will weigh less than it does at room temperature due to (a) hot air rising and (b) pulling the weight and pan up with the current of air. It is also because hot materials have less adsorbed and absorbed water on them. Thus when you weigh a hot object, you are weighing the weight without any surface water. As an object cools off, water begins to attach to the surface of the object and "weigh it down." The actual significance of this water weight is generally ignored because it is too small for most purposes. Likewise, if a cool object is placed in a weighing chamber, the reverse occurs and the object will appear heavier than it really is. Because cold objects are likely to have water condense on the container's surfaces as well as on the object itself, the amount of collected water is very likely to have a significant effect on an object's measured weight.
Electrostatic problems (Rule 11) are likely to occur when atmospheric (relative) humidity is below 40%. If a container becomes positively (or negatively) charged and the weighing apparatus is likewise charged, they will repel each other and the