- •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
118 Measurement
freeze. Also, an alkaline solution will react with the glass, creating a rough surface which can scratch a Teflon plug.
The procedure for cleaning burettes is similar to general glass cleaning already discussed. Because burettes are only used to deliver, it is never necessary to dry a burette before use. However, a wet burette can change the concentration of the solution being placed within it. To avoid changing concentrations, shake the burette dry and pour a small amount of the solution you will be working with into the burette. Swirl and/or rotate it around the burette, and pour it out. If you have a very low molarity solution, you may want to repeat this process again. The prerinse (with the solution to be used) will reduce, and should eliminate, any change in concentration caused by standing water in the burette.
When first filling a burette, any air bubbles in the tip region (below the stopcock) should be removed. If a bubble remained where it originally was, there would be no problem. However, if a bubble comes out while making a measurement, it takes the place of fluid that was recorded, but never left the burette. The standard practice for removing bubbles is to overfill the burette, and open the stopcock fully to try and force the bubble out. This technique often works, but it can also be wasteful of material.
An alternate method of tip bubble removal was reported by Austin.8 First, pour about 1 mL of fluid into the burette, open the stopcock to let the fluid into the tip region and close the stopcock. Now observe the tip and see if a bubble is trapped within the liquid of the tip. If there is no bubble, fill the burette to the top and proceed with your work. If there is a bubble, turn the burette so the stopcock is on top and quickly rotate the stopcock plug 180°. This procedure will lower the liquid in the tip of the burette, but if done quickly enough, it should not empty the tip. It should, however, remove the bubble from the tip region. The advantage of this approach is that it uses less solution.
2.4Weight and Mass
2.4.1Tools for Weighing
We weigh things by comparing the unknown weight (or force) of an object with a known weight (or force). The device used to weigh things is called a balance. The word comes from the Latin bi-lancis, or two dishes. The word balance is still used despite the fact that two-dish (or two-pan) balances are seldom (if ever) used nowadays. In lieu of a second pan, the counter (opposing) force now may be springs, built-in calibrated weights, or a magnetic device called a servomotor.
There are four classes of balances, each based on their ability to split hairs as it were, or, more specifically, based on the number of intervals used within the scale capacity. For example, if a laboratory balance has a capacity of 200.00 grams and it reads to two decimals, it would have 20,000 scale intervals. The formal identifi-
Weight and Mass 2.4 |
119 |
cation of four classes was devised by the International Organization of Legal Metrology (OIML), and they are shown in Table 2.21.
Balances can be calibrated or verified for accuracy with special weights, called calibrated weights, whose specific mass is known. Calibrated weights* vary in quality and tolerance. They are classified by type, grade, and tolerance.^All calibrated weights are compared directly or indirectly to the international prototype one-kilogram mass to verify their accuracy.
2.4.2 Weight Versus Mass Versus Density
It is fair to say that an object weighing a ton is heavy and that few, if any, people could move or lift it. However, on the moon the same object would weigh only a bit over 300 lb—although the average person would still be unable to move the object. If we were on the space shuttle in a free-fall environment, anyone could move the object around with relative ease. When we weigh an object, we are measuring its inertia to Earth's gravitational pull. That measurement is its weight, not its mass. The weight of an object, not its mass, will change depending upon its inertia.
Unlike weight, which varies relative to its inertia (such as gravity), mass is an inherent and constant characteristic of any object. In any given gravitational environment, an object with a lot of material (mass) will weigh more than an object of the same type, but less material. Because of this quality, we can make calculations of, and about, an object's mass from its gravitational weighing.
Density is not directly related to mass or weight, but is calculated from an object's weight divided by its volume (g/m3). For example, a large object of little mass (such as foam rubber) is considered to have little density. On the other hand, a small object of tremendous mass (such as a neutron star) has tremendous density. Density refers to the amount of space ("volume") a given amount of mass
Table 2.21 Classifications of Weighing Equipment9, 10
Class |
Class Name |
Scale Intervals |
I |
Special accuracy (fine) |
50,000 < na |
II |
High accuracy (precision) |
5,000 < n < 100,000 |
III |
Medium accuracy (commercial) |
500 < n < 10,000 |
nil |
Ordinary accuracy (course) |
100<n< 1,000 |
' n = number of intervals.
'Calibrated weights are verified to weigh what they say they do within a given tolerance. The smaller the tolerance of a calibrated weight, the better the quality and the more expensive it will be.
trThese parameters are discussed further in the section on calibrated weights (see Sec. 2.4.13).
120 |
Measurement |
occupies. Mass refers to the amount of material in an object, not to the amount of space it occupies.
In everyday parlance, we imply an object's mass when we speak of its weight. However, because we weigh an object based on its attraction to Earth, we are, in effect, measuring its force. In a nutshell, we measure an object's force to obtain its weight, from which we can calculate its mass. The validity of this approach holds despite the fact that the force of gravity varies over the earth's surface by over 5% in addition to changes in elevation.
2.4.3 Air Buoyancy
The fact that weights occupy space creates an interesting problem. The space occupied by a weight is normally occupied by air, and because air has weight, it provides a buoyancy effect (known as Archimedes' principle) against the real weight of the object. This effect influences the measured weight of an object.
The problem is more easily explained by examining what happens when you place something in water (because water weighs more than air and provides a greater buoyancy effect, its effects are more dramatic). If you put a cube of metal in water, it sinks to the bottom of the container. That cube weighs less in the water than it did in air, by an amount equal to the weight of the water it displaced. On the other hand, if you put a similar-sized block of wood in the water, it would float because the amount of water that the wood displaces weighs more than the wood,
Table 2.22 Variation in Weight with Atmospheric Density0
|
Density |
Weight (kg) |
Weight (kg) |
|
Object |
in Denver, CO |
in Vacuum |
||
(g/cm3) |
||||
|
(dA = 0.00098 g/cm3) |
(True Mass) |
||
Oven dried eastern white pine |
0.373 |
1.000564 |
1.003077 |
|
Live oak wood |
0.977 |
1.000198 |
1.001080 |
|
Aluminum |
2.7 |
1.000054 |
1.000295 |
|
Calibration weight in Mettler AT |
7.97 |
1.000000 |
1.000001 |
|
balance |
|
|
|
|
Stainless steel as used in mass |
8.0 |
1.000000 |
1.000000 |
|
standards |
|
|
|
|
Brass |
8.4 |
0.999999 |
0.999993 |
|
Gold |
19.3 |
0.999984 |
0.999912 |
|
Platinum-indium (kilogram |
21.5 |
0.999983 |
0.999906 |
|
prototype) |
|
|
|
" From Tables 1 and 2 from "Honest Weight—Limits of Accuracy and Practicality" by W.E. Kupper from the Proceedings of the Measurement Science Conference 1990. With permission.
* 1 kg of the following materials, as weighed in sea level atmosphere of density da = 0.0012 g/cm3 against steel weights of density d = 8.0 g/cm3.
Weight and Mass 2.4 |
121 |
preventing the wood from sinking. The same phenomena occurs in air, which is why helium balloons rise and wood balloons fall.
Even if an object's density and size change, its mass does not. Thus, it is possible for two objects to have the same mass but weigh different amounts due to the effects of air buoyancy caused by the weight of air. This principle can be demonstrated by taking a calibrated weight whose density is 8.0 g/cm3 and weight (in air) is 100.000 g, then using it to weigh an equal weight of pure water whose density is 1.0 g/cm3. Because their densities are different, they will occupy different volumes of air: Their volumes are 12.5 cm3 and 100 cm3, respectively. If you were to weigh each object in a vacuum to eliminate the air buoyancy factor,* the calibrated weight would now weigh 100.015 g and the pure water would now weigh 100.120 g.
Factors that affect buoyancy are the density of a sample, ambient air pressure, and relative humidity. Thus, a barometer and humidity indicator should be located within any balance room where highly accurate readings are required. The counterbalance weights within single-pan balances are also affected by air buoyancy, but in equal amounts to the sample, so they should cancel each other out. The exact amount of the buoyancy effect varies depending on the density of the material being weighed and the density of the air at the time of weighing. This phenomenon was studied in detail by Schoonover and Jones,11 and by Kupper.12
The formula for converting a weighing result to true mass is given in Eq. (2.1):
'"if
m = M — = Mk |
(2.1) |
1 - ^ L |
|
dD |
|
where m = mass of the sample
M = weighing result, i.e., the counterbalancing steel mass
da = air density at time of weighing1^
D = density of mass standard, normally 8.0 g/cm3
d = density of sample
k = ratio of mass to weighing result for the sample
To calculate the density of the air, use the formula in Eq. (2.2):
where T = Temperature in °K (Centigrade plus 273.15)
B = Barometer reading in millimeters of mercury
'instead of making the weighings in a vacuum, you can also make use of Eq. (2.1) and Eq. (2.2). +For the density of moist air, see the Handbook of Chemistry and Physics, The Chemical Rubber Company, published annually.
122 Measurement
There are only two occasions where measured weight equals true mass, when it = 1. This occasion occurs when measurements are made in a vacuum or the density of a sample is equal to the density of the mass standard. Fortunately, the greatest differences only occur when an object's density is particularly low (0.1% for density =1.0 g/cm3 and about 0.3% for density « 0.4 g/cm3). In most situations, the effect of air buoyancy is significantly smaller than the tolerance of the analytical balance. The effects of varying densities (of objects being weighed) and varying air densities are shown in Table 2.22.
One approach to avoiding the problem of air buoyancy is to weigh an object in a vacuum (known as "weight in vacuo"). Such readings provide an object's true mass as opposed to its apparent mass. There are a variety of vacuum balances made precisely for this purpose. However, vacuum balances are expensive, require expensive peripheral equipment (such as vacuum systems), and are neither fast nor efficient to use.
2.4.4 Accuracy, Precision, and Other Balance Limitations
The amount of accuracy required in a balance, like most things in the lab, depends the balancing of your needs versus the capacities of your pocketbook. You do not need great accuracy if all you are doing is weighing letters. On the other hand, weighing volumetric flasks to calibrate volume requires tremendous accuracy. Not only is the cost greater for a more accurate balance, but the support equipment and personnel for the maintenance of such equipment are also greater. When analyzing the different attributes and characteristics that help to define the quality and capabilities of balances, many different terms are used. The following terms (and concepts) are used to describe various features of all balances:
The greater the accuracy of a balance, the closer the balance will read the nominal weight* of a calibration weight. If the calibration weight reads 10 mg, the balance should read 10 mg. If, for example, the balance reads 10.5 mg, it has less than desirable accuracy, and if it reads 12 mg, it has poor accuracy.
The precision of a balance is related to how well it can repeatedly indicate the same weight over a series of identical weighings under similar environmental conditions. Precision is not a measure of how accurately a scale can make a single weight reading. The index of precision is the standard deviation for a collection of readings. If the index of precision is greater than the readability of the balance, accuracy is significantly jeopardized.
Readability refers to the smallest measurement that a balance can indicate and that can be read by an operator when the balance is being used as intended. Generally, triple-beam balances have a readability of ±0.1 g, centigram balances have a readability of ±0.01 g, and analytical balances have a readability of ±0.0001 g.
"The nominal weight of a calibrated mass is the calibration that is printed on, or stamped into, its surface.