- •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
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2.3Volume
2.3.1The Concepts of Volume Measurement
It does not seem that it should be difficult to calculate the volume of any given container. First you establish a unit of volume, then you base everything on that unit. Despite the apparent simplicity of such a process, two widely divergent approaches to calculating a volume unit have developed.
One approach established that a liter was the volume of space occupied by the mass of one kilogram of distilled water (at 4°C and 30 inches of mercury). The other approach required a given length measurement to be defined (one decimeter), and then it defined the cube of that measurement as the volume measurement (one liter).
The original idea of the metric system was that either approach would provide the same unit of metric volume. Unfortunately, it did not work because of the subtle differences in density caused by subtle differences in temperature. Thus, the kilogram-based milliliter equaled 1.000,027 cubic centimeters. Because of the discrepancy, the International System for Weights and Measures had to make a choice between which approach would be accepted to obtain volume measurements, and the nod was eventually given to the cubic length technique. The use of liters and milliliters in volumetric ware is therefore misleading because the unit of volume measurement should be cubic meters (cubic centimeters are used as a convenience for smaller containers). The International System of Units (SI) and the ASTM accept the use of liters and milliliters in their reports, provided that the precision of the material does not warrant cubic centimeters. Because the actual difference in one cubic centimeter is less than 3 parts in 100,000, for most work it is safe to assume that 1 cm3 is equal to 1 mL.
2.3.2 Background of Volume Standards
Rigorous standards have been established for volumetric ware. These standards control not only specific standards of allowable error for volumetric ware, but the size of the containers, the materials of construction, their bases, shapes, and sizes, the length and width of index lines, and how those lines are placed on the glass or plastic. The painstaking work to establish these guidelines was done by agencies such as the NIST (National Institute of Standards and Technology), the ASTM (American Society for Testing and Materials), and the ISO (International Standards Organization)
Occasionally you may see references to Federal Specification numbers. For example, the Federal Specification number NNN - C 940-C is for graduated cylinders. All Federal Specification numbers are no longer being updated, and these specifications are being superseded by those established by the ASTM. The preceding number for graduated cylinders is now under the specifications of ASTM 1272-89. All ASTM documents are identified by a designation number. If there
86 |
|
|
Measurement |
Table 2.6 Cross Comparison of Class A Volumetric Ware (25 mLf |
|||
Item |
Class A |
Item |
Class A |
Graduated Cylinder |
+0.17 mL |
Volumetric pipette |
±0.03 mL |
Volumetric Flask |
±0.03 mL |
Measuring pipette |
±0.05 mL |
Burette |
±0.03 mL |
Serological pipette |
(only Class B & lower) |
" Based on ASTM guidelines.
are updates to any document, the number will be followed by the acceptance year of the update. For example, the preceding example ASTM document cited shows that it was accepted by the ASTM for publication in 1989. If there is a conflict in ASTM guidelines, the document with the later publication date takes precedence.
All manufacturers abide by the standards set by these organizations. Therefore with the exception of quality and control, one manufacturer's volumetric ware (of comparable type) should not be more accurate than another manufacturer's. It is important to keep these guidelines in mind so that ASTM standards are not allowed to be used as marketing hype.
Manufacturers refer to these standards in their catalogs, both to let you know what you are buying and to enhance importance that may not otherwise be there. For instance, only glassware made to specific established tolerances can have the symbol of "A" or "Class A" on their sides, signifying highest production quality. For example, for a standard tolerance graduated cylinder, you may see statements in catalogs like "... conforms to ASTM Type I, Style 1 specs for volumetric ware." This description translates to mean "the graduated cylinder is made out of borosilicate glass (Type I) and has a beaded lip with a pour spout (Style 1)." In reality, this enhanced description is harmless and is much safer than statements saying "the most accurate graduated cylinder in town."
Do not let the designation Class A mean more than it was meant to. Class A can only mean that it is the best tolerance readily available for that specific type of volumetric ware. Class A volumetric ware is not consistent across volumetric ware type. For example, a Class A volumetric pipette does not have the same degree of tolerance as a Class A measuring pipette. Equally, a Class A graduated cylinder does not have the same degree of tolerance as a Class A volumetric flask. See Table 2.6 for a representative cross comparison of Class A tolerances.
In addition, do not be misled by ASTM designations. The words "Class," "Style," and "Type" are constantly used to describe different attributes to different types of variables in ASTM literature. They seldom refer to the same attribute. Thus it is important to know what the identifying word is attributed to before assuming that you know what it is signifying. An example of these differences are shown in Table 2.7. The ASTM always refers to itself in its own specifications for equipment when describing one of its own procedures for a given test. That is, when they are performing a test, they must ensure that their guidelines are used when their equipment is selected. However, when you see manufacturer state-
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ments in catalogs describing (for example) a graduated cylinder that "... meets specifications of ASTM E133 for use in tests D86, D216, D285, D447, and D 850
...," all the manufacturer is saying is that if you are performing any of these particular ASTM tests, this graduated cylinder satisfies ASTM requirements for use. However, if the graduated cylinder meets ASTM El 33 requirements, by definition it can be used for tests D86, D216, etc. These descriptive entries not only are confusing if you are unfamiliar with the numbers, but also provide blah-blah for marketing.
2.3.3 Categories, Markings, and Tolerances of Volu-
metric Ware
There are four categories of containers used to measure volume: volumetric flasks, graduated cylinders, burettes, and pipettes. Of the four, volumetric flasks are used exclusively to measure how much has been put into them. This use is known as "to contain." Graduated cylinders and a few pipettes are used to measure how much has been put into them as well as how much they can dispense. The latter measurement is known as "to deliver." Burettes and most pipettes are used solely to deliver.
The term to deliver is based on the concept that when you pour a liquid out of a glass container, some of that liquid will remain on the walls of that container. Because not all of the measured liquid is completely transferred, the material left behind should not be considered part of the delivered sample. Pipettes have two different types of to deliver. One which requires you to "blow out" the remaining liquid, and one that does not. Some volumetric containers are made out of plastic which does not "wet" like glass. Because these containers drain completely, the to contain is the same as the to deliver. Because some materials (i.e., mercury) do not "wet" the walls of any container, they should be used with only to contain measuring devices.
The abbreviations TC and TD are commonly used to denote to contain and to deliver, respectively, in the United States. Old glassware might be labeled with a simple "C" or "D." The ISO (International Standards Organization) uses the
Table 2.7 "Style" Has Different Meanings'3
Graduated Cylinder Pharmaceutical Cylinder
Here the term "Style" refers to the physical structure of the opened end.
Here the term "Style" refers to the calibrations.
Style 1 |
Beaded lip with pouring spout |
Metric calibration |
Style 2 |
Top with ground glass stopper |
English (in.-lb) calibrations |
Style 3 |
Beaded lip with pouring spout and |
Both English and metric calibrations. |
|
reinforced rim |
|
a From ASTM specifications E 1094-86 (Standard Specification for Pharmaceutical Glass Graduates) and E 1272-89 (Standard Specification for Graduated Cylinders).
88 Measurement
The stated volume of a flask will approximately fill to where the neck attaches to the flask.
Fig. 2.13 The volume of flasks
abbreviations IN for to contain and EX for to deliver. These abbreviations come from the Latin root found in intra (within) and extra (out of). This classification has been accepted for use in the United States by the ASTM and is slowly being introduced by U.S. manufacturers. Because there have been no formal deadlines set, manufacturers are waiting for their current silkscreen printing setups to wear out by attrition and then replacing them using the new classification. Although some volumetric ware may be labeled with both English and metric calibrations, glassware is seldom labeled with both TD and TC calibrations. If you are ever using a volumetric container that is double-labeled, be careful that you are reading the scale relevant to what you are doing.
Other common laboratory containers such as beakers, round bottom flasks, and Erlenmeyer flasks often have a limited graduated volume designated on their sides. These markings provide an approximate volume and cannot be used for quantitative work. The required accuracy of these containers is only 5% of volume. When there are no calibration lines on a flask, it still is possible to obtain an approximate volume measurement based on the stated volume: In general, the stated volume will approximately fill any given nonvolumetric container to the junction of the neck and container (see Fig. 2.13). Thus, if you need about 500mL of water, it is safe to fill a 500-mL flask up to the neck and you will have approximately the needed volume.
The quality of any given volumetric ware is based on how accurate any given calibration line will deliver the amount it claims. For example, say that a one-liter flask is accurate to ±5%, meaning that the flask is likely to contain anywhere from 950 mL to 1050 mL of liquid. For comparison, a one-liter Class B volumetric flask is accurate to ±0.60 mL, or +0.06% accuracy, and a one-liter Class A is accurate to ±0.30 mL, or ±0.03% accuracy. Needless to say, it costs more for greater accuracy.
Precision volumetric glassware must be made following the standards set by ASTM Standards E542 and E694. These standards establish not only the degree of tolerance, but how the container is to be made, how the lines are engraved, the width and length of calibration lines, the type of glass used, the design and type of base (if any), the flow rate of liquids through tips, and many other limitations. In