- •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
Measurement
2.1Measurement: The Basics
2.1.1Uniformity, Reliability, and Accuracy
We do not measure things. Rather, we measure properties ofthings. For example, we cannot measure a box, but we can measure its properties such as its mass, length, and temperature.
To properly compare and analyze the things in our universe, weneed to compare and analyze their properties. Because people all around the world are making measurements, we must ensure there isagreement on all the various types ofmeasurements used. Difficulties arise because measurements have both quantitative and qualitative aspects. The fact that the two lines onthe international prototype platinum-iridium bar inFrance are one meter apart isquantitative; how you measure other objects with that baris qualitative. The ability to match uptwo lines may seem simple, but, depending the desired accuracy, such simple operations are in fact difficult. This difficulty is why using measuring equipment is a qualitative art.
No one uses the prototype meter as anactual measuring tool; rather, copiesare made from the original prototype, and these copies are used as masters to make further copies. By thetime you purchase a meter stick, it is a fardistant cousin from the original meter prototype. However, despite the length of the progeny line, you hope that the copy you have is asgood as the original. Depending on the expertise of theengineers andmachinists involved, it should be very close.To obtain that quality, theengineers andmachinists were guided by three factors; uniformity, reliability, and accuracy. Without these basic tenets, the quality of the meter stick you usewould be in doubt. Likewise, thequality of the use of the meter stick isalso dependent on the same three factors, without which all readings made would be indoubt.
Uniformity requires that all people use the same measurement system (i.e., metric vs. English) and that all users intend that a given unit ofmeasurement represents thesame amount andis based on thesame measurement standard used
65
66 Measurement
everywhere else. It is theuser's responsibility to select equipment that provides measurements that agree with everyone else.
Reliability requires theability to consistently read a given measurement device and also requires a given measurement device to perform equally well, test after test. It is the user's responsibility toknow how to achieve repeatable data from the equipment being used.
Accuracy refers tohow well a measurement device is calibrated and how many significant figures onecanreliably expect. It is theuser's responsibility to know how to read hisequipment andnotinterpolate data to be anymore accurate (i.e., significant figures) than they reallyare.
Laboratory research is dependent onreliable quality measurements andthe use of uniformity, reliability, and accuracy to achieve this goal and this cannot be emphasized enough. Poor or inaccurate measurements can only lead to poor or inaccurate conclusions. A good theory can be lost if the experimental data are misread.
Commerce is equally dependent onuniformity, reliability, and accuracy of measurement systems. The potential economic liabilities of mismeasurements and misunderstanding areeasy to understand. In fact, it was theeconomic advantages of uniformity that ledto themetric system's expansion after the Napoleonic wars. What canupset and/or confuse consumers and businesses is when thesame word (which may have varying meanings) is applied to different weights. Westill confuse the weight value of a ton and the volume of a gallon: In theUnited States,the ton is equal to 2000 lb; however, in Great Britain it is equal to 2240 lb. Similarly, in the United States, the gallon is established as 231cubic inches; however, in Great Britain it is 277.42 cubic inches. If you areaware of these differences, you can make theappropriate mathematical corrections. But realistically, it should not be a problem to be dealt with. Rather, theproblem of different measurement systems should be avoided in the first place. That is specifically was what themetric system was designed to do.
2.1.2 History of the Metric System
Overcoming the incongruities of inconsistent measurement systems on an international basis wasconsidered for centuries. Thebasics of the metric system were first proposed by Gabriel Mouton of Lyon, France, in 1670. This vicar (of St. Paul's Church) proposed three major criteria for a universal measurement system: decimalization, rational prefixes, andusing parts of the earth as a basis of measurement (length was to be based on the arc of one minute of the earth's longitude). There wasalso a desire to find a relationship between thefoot and gallon (i.e., a cubic foot would equal one gallon). Unfortunately, these measurement units were already in use, andbecause there was nobasis for these measurements
Measurement: The Basics 2.1 |
|
67 |
Table 2.1 Base SI Units* |
|
|
Quantity |
Unit |
Symbol |
length |
meter |
m |
mass |
kilogram |
kg |
time |
second |
s |
electric current |
ampere |
A |
thermodynamic temperature |
kelvin |
K |
amount of substance |
mole |
mol |
luminous intensity |
candela |
cd |
* From the ASTM document E380-86, Table 1. With permission.
to have any easy mathematical agreement, they did not. No simple whole number could be used to correct the discrepancy.
Gabriel Mouton's ideas were discussed, amended, changed, and altered for over 120 years. Eventually, a member of the French assembly, Charles Maurice Talley- rand-Perigord, requested the French Academy of Sciences to formalize a report. The French Academy of Sciences decided to start from scratch and develop all new units. They defined the meter as one ten-millionth of the distance from the North Pole to the equator. They also decided that the unit for weight would be based on the weight of a cubic meter of water in its most dense state (at 4°C). This plan allowed the interlinking of mass and length measurement units for the first time. In addition, they proposed prefixes for multiples and submultiples of length and mass measurements, eliminating the use of different names for smaller and larger units (i.e., inch/foot or pint/quart units).
On the eve of the French Revolution, June 19, 1791, King Louis XVI of France gave his approval of the system. The next day, Louis tried to escape France but was arrested and jailed. A year later from his jail cell, Louis directed two engineers to make the measurements necessary to implement the metric system. Because of the French Revolution, it took six years to complete the required measurements. Finally, in June 1799 the "Commission sur l'unite de poids du Systeme Metrique decimal" met and adopted the metric system. It was based on the gram as the unit of weight and the meter as the unit of length. All other measurements were to be derived from these units. The metric system was adopted "For all people, for all time."
The metric system sought to establish simple numerical relationships between the various units of measurement. To accomplish this goal, the Commission took a cubic decimeter* of water at its most dense state (4°C), designated this volume as one "liter," and designated its mass (weight) as one "kilogram." In so doing, the commission successfully unified mass, length, and volume into a correlated mea-
For a description of how the meter was derived, see Sec. 2.1.3.
68 Measurement
surement system for the first time. Official prototypes of the meter and kilogram were made and stored in Paris.
Because of Napoleon's conquests, the metric system spread rapidly throughout Europe. However, it was not in common usage in many areas (even in France) until international commerce took advantage of its simplicity and practicality. By the mid-1800s, it was the primary measurement system in most of Europe. In 1875 the International Bureau of Weights and Measures was established near Paris, France. It formed a new international committee, called the General Conference on Weights and Measures (CGPM), whose goal was to handle international matters concerning the metric system. The CGPM meets every six years to compare data and establish new standards. Every member country of this committee* receives a copy of the meter and kilogram prototype with which to standardize their own country's measurement system.
Over the years there has been ongoing fine-tuning of the measurement system because the greater the precision with which our measurement units can be ascertained, the better we can define our universe. A new era in the measurement system came in 1960, at the 11th meeting of the CGPM, when the International System of Units (SI) was established. This system established four base units: the meter, kilogram, second, and ampere. They are collectively known as the MKSA system. Later, three more base units were added: kelvin (for temperature), candela (for luminous intensity), and mole (for the amount of substance) (see Table 2.1). In addition, two supplementary base units (which are dimensionless) were added: radian (plane angles) and steradian (solid angles) (see Table 2.2).
From the nine base units, over 58 further units have been derived and are known as derived units. There are two types of derived units: those that have special names (see Table 2.3) and those that have no special names (see Table 2.4). An example of a derived unit with a special name is force, which has the unit newton (the symbol N) and is calculated by the formula "N = kg-^s2." An example of a derived unit that does not have a special name is volume, which has the unit of cubic meter (no special symbol) and is calculated by the formula "volume = m3."
Table 2.2 Supplementary SI Units"
Quantity |
Unit |
Symbol |
Plane angle |
radian |
rad |
Solid angle |
steradian |
sr |
" From the ASTM document E380-86, Table 2, with permission.
"The National Institute of Standards and Technology (formally the National Bureau of Standards) represents the United States at the CGPM. They store the United States' copies of the original measurement prototypes.
Measurement: The Basics 2.1 |
69 |
Table 2.3 Derived SI Units with Special Names*
Quantity |
Unit |
Symbol |
Formula |
|
Frequency (of a periodic phenomenon) |
hertz |
Hz |
1/s |
|
Force |
newton |
N |
kg-m/s2 |
|
Pressure, stress |
pascal |
Pa |
N/m2 |
|
Energy, work, quantity of heat |
joule |
J |
N-m |
|
Power, radiant flux |
watt |
W |
J/s |
|
Quantity of electricity, electric charge |
coulomb |
C |
A-s |
|
Electrical potential, potential difference, elec- |
volt |
V |
W/A |
|
tromotive force |
|
|
|
|
Electric capacitance |
farad |
F |
C/V |
|
Electric resistance |
ohm |
a. |
V/A |
|
Electric conductance |
Siemens |
s |
A/V |
|
Magnetic flux |
weber |
V-s |
||
Wb |
||||
Magnetic flux density |
tesla |
Wb/m2 |
||
T |
||||
Inductance |
henry |
H |
Wb/A |
|
Celsius temperature |
degree |
°C |
Kc |
|
Luminous flux |
lumen |
lm |
cd-sr |
|
Illuminance |
lux |
lx |
lm/m2 |
|
Activity (of a radionuclide) |
becquerel |
Bq |
1/s |
|
Absorbed dose* |
gray |
Gy |
J/kg |
|
Dose equivalent |
sievert |
Sv |
J/kg |
° From theASTM document E380, Table 3, reprinted with permission.
h Related quantities using the same unit are:specific energy imparted, kerma, and absorbed dose index.
c Celcius temperature (t) is related to thermodynamic temperature (T) by the equation: t =T- To where To = t0 273.15 K by definition.
Table 2.4 Some Common Derived Units of SI
Quantity |
Unit |
Formula |
Absorbed dose rate |
gray per second |
Gy/s |
Acceleration |
meter per second squared |
m/s2 |
Angular acceleration |
radian per second squared |
rad/s2 |
Angular velocity |
radian per second |
rad/s |
Area |
square meter |
m2 |
Concentration (of amount of |
mole per cubic meter |
mol/m2 |
substance) |
|
|
Current density |
ampere per square meter |
A/m2 |
Density, mass |
kilogram per cubic meter |
kg/m2 |
70 |
Measurement |
Table 2.4 Some Common Derived Units of SI (continued)
Quantity |
Unit |
Electric charge density |
coulomb per cubic meter |
Electric field strength |
volt per meter |
Electric flux density |
coulomb per square meter |
Energy density |
joule per cubic meter |
Entropy |
joule per kelvin |
Exposure |
coulomb per kilogram |
Heat capacity |
joule per kelvin |
Heat flux density |
watt per square meter |
Irradiance |
|
Luminance |
candela per square meter |
Magnetic field strength |
ampere per meter |
Molar energy |
joule per mole |
Molar entropy |
joule per mole kelvin |
Molar heat capacity |
joule per mole kelvin |
Moment of force |
newton meter |
Permeability (magnetic) |
henry per meter |
Permittivity |
farad per meter |
Power density |
watt per square meter |
Radiance |
watt per square meter steradian |
Radiant intensity |
watt per steradian |
Specific heat capacity |
joule per kilogram kelvin |
Specific energy |
joule per kilogram |
Specific entropy |
joule per kilogram kelvin |
Specific volume |
cubic meter per kilogram |
Surface tension |
newton per meter |
Thermal conductivity |
watt per meter kelvin |
Velocity |
meter per second |
Viscosity, dynamic |
pascal second |
Viscosity, kinematic |
square meter per second |
Volume |
cubic meter |
Wave number |
1 per meter |
" From the ASTM document E380, Table 4, reprinted with permission.
Formula
C/m3
V/m
C/m2
J/m3
J/K
C/kg
J/K
W/m2
cd/m2
A/m
J/mol
J/(mol)K)
J/(mol)K) N-m
H/m
F/m
W/m2
W/(m2-sr)
W/sr
J/(kgK)
J/kg
J/(kg-K)
m3/kg
N/m
W/(mK)
m/s
Pas
m2/s
m3
1/m
Among the advantages of the International System of Units system is that there is one, and only one, unit for any given physical quantity. Power, for instance, will always have the same unit, whether it has electrical or mechanical origins.
In the United States, measurements made with metric units were not legally accepted in commerce until 1866. In 1875 the United States became a signatory to the Metric Convention, and by 1890 it received copies of the International Prototype meter and kilogram. However, rather than converting our measurement system to metric, in 1893 Congress decided that the International Prototype units