- •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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reality, if the manufacturers are properly following the ASTM guidelines, there is little room for any volumetric ware to be poorly made.
ASTM guidelines also establish that volumetric ware is to be calibrated at 20°C. This (or any) constant is required because gases, liquids, and solids vary in size as temperature changes. Thus, any individual item is accurate only at one temperature. If manufacturers did not adhere to one temperature calibration, constant mathematical adjustments would have to be made as one switched from one brand of glassware to another.
There are four basic grades of volumetric ware:
1.Special Tolerance, also called Calibration Tolerance and Certified Ware. This glassware is calibrated not only to Class A tolerances, but to each mark on the glass. This calibration ensures high accuracy for every measurement. It needs to be specially ordered and calibrated.
2.Class A. This code is for the highest-class glassware that is production made. Some manufacturers refer to this grade as precision grade. High-quality work can be performed using glassware that has this designation. The tolerance is the same as Special Tolerance, but in Class A it is based on a container's total capacity, not for each measurement division. Containers of Class A tolerance are always designated as such in writing on the side.
3.Class B. This classification is average grade glassware and can be used for general quality work. Some manufacturers refer to this quality as standard grade or standard purpose. By ASTM designation, Class B tolerances are twice those of Class A. The tolerance is based on a container's total capacity, not for each measurement division. Containers of Class B tolerance are seldom, if ever, designated as such in writing on their side.
4.General Purpose. This glassware is not accurate for any level of quality work. It is often referred to as student grade or economy grade. Because the calibration is never verified, it is the most inexpensive volumetric glass available. The tolerance is limited to plus or minus the smallest subdivision of the container. Containers of general purpose tolerance are never specifically identified as such and therefore may be confused as Class B volumetric glassware. Such glassware made by Kimble is identified as "Tekk." Corning does not have a generic name for its student ware. General purpose glassware is often made out of soda-lime glass rather than borosilicate glass.
2.3.4 Materials of Volumetric Construction #1 Plastic
There are four types of plastic that are commonly used in volumetric ware: polypropylene (PP), polymethylpentene (PMP or TPX), polycarbonate (PC), and polystyrene (PS). Plastic can be less expensive than glass, can be more difficult to
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Measurement |
break, and can be used equally well for to contain and to deliver measurements. However, it cannot tolerate temperatures over 130° to 170°C (depending on the type of plastic), can be dissolved in some solvents, and the best quality available is Class B.
General Character of Each Type of Plastic.
Polypropylene is translucent and cannot be dissolved by most solvents at room temperature. It can crack or break if dropped from a desk.
Polymethylpentene is as transparent as glass and is almost as resistant to solvents as polypropylene. It can withstand temperatures as high as 150°C on a temporary basis and 175°C on an intermittent basis. It can crack or break if dropped from a desk.
Polycarbonate is very strong and as transparent as glass. It is subject to reactions from bases and strong acids and can be dissolved in some solvents.
Polystyrene is as transparent as glass. It can be soluble to some solvents and because it is inexpensive, it is often used for disposable ware. It can crack or break if dropped from a desk.
Resistance to Chemicals. For a comprehensive list of plastic resistance to chemical attack, see Appendix B.
Cleaning. Volumetric ware must be cleaned both to prevent contamination of other materials and to ensure accurate measurements. Because volumetric ware is often used as a temporary carrier for chemicals, it comes in contact with a variety of different materials which may be interreactive. Also, any particulate or greasy material left behind can alter a subsequent measurement.
Never use abrasive or scouring materials on plastic ware. Even though the bristles of a bottle brush are not likely to scratch plastic, the metal wire that they are wrapped on can! Scratches can alter volumetric quality, are more difficult to clean, increase the surface area open to attack by chemicals (that would otherwise be safe for short exposures), and can prevent complete draining from a to deliver container.
The following are some general cleaning guidelines for plastics:
1.Generally, mild detergents are safe with all plastic ware.
2.Do not use strong alkaline agents with polycarbonate.
3.Never leave plastic ware in oxidizing agents for an extended time because they will age the plasticizers and weaken the plastic. Chromic acid solutions are okay to use, but never soak longer than four hours.
4.Polystyrene should not go through laboratory dishwashers because of the high temperatures.
5.Polypropylene and polymethylpentene can be boiled in dilute sodium bicarbonate (NaHCO3), but not polycarbonate or polystyrene.
6.Sodium hypochlorite solutions can be used at room temperature.
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7. Organic solvents can be used cautiously only with polypropylene. However, test each solvent before use for possible negative effects on the outside of the volumetric ware, away from a calibrated area.
Autoclaving. Polypropylene can be autoclaved, and polycarbonate can be autoclaved for a limited time (<20 minutes) but can be weakened from repeated autoclaving. The quality of volumetric measurements is likely to be eroded with repeated autoclaving. Polystyrene should never be autoclaved.
2.3.5 Materials of Volumetric Construction #2 Glass
Although glass is more likely to chip, crack, or break than plastic ware, it is safe to use with almost all chemicals. Type I glass can safely be put into a drying oven, and Type I and II glass can be autoclaved (glass types are explained below). No volumetric ware should ever be placed over a direct flame. Occasionally, tips and/ or ends of burettes or pipettes are tempered to provide additional strength. The tempering process typically used is heating followed by rapid cooling.
General Characteristics of Each Glass Type. Volumetric ware made of glass provides different properties depending on the type of glass used. The ASTM refers to the different glasses used in volumetric ware as Types. The use of the terms "Class A" and "Class B" in reference to types of glass have no relationship to volumetric quality.
1.Type I, Class A glass is usually Pyrex, Kimex, or Schott glass. It can be used for all classifications of volumetric ware. This glass is chemically inert, is repairable (in nonvolumetric regions away from calibration), can safely be placed in a drying oven, and can be fused onto other similar borosilicate laboratory glassware.
2.Type /, Class B glass is an aluminosilicate glass. It can be used for all classifications of volumetric ware. The trade names used are Corning's "Corex" glass or Kimble's "Kimex-51." They are more chemically resistant than standard borosilicate. However, they have larger coefficients of expansion and therefore cannot directly be fused onto
other lab glass items made out of Pyrex or Kimex. An intermediary glass with a coefficient of expansion of about 40 x 10"6 - 42 x 10"6 is
required for fusing Type I, Class B glass to Type I, Class A glass.
3.Type II glass is often identified as soda-lime, flint, or soft glass. Sodalime glass is not as chemically resistant as Type I glass, but short duration containment is acceptable (it is generally a good idea to not leave chemicals in soda-lime volumetric ware, particularly an alkaline chemical).
Type II volumetric ware cannot be repaired if cracked or chipped, nor can it be fused onto other laboratory ware. On the other hand, it is inexpensive and therefore commonly used for disposable ware and lower standard calibration ware.
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|
|
Measurement |
|
Table 2.8 Effect of Heat Treatment on Volumetric Glassware0 |
|||||
|
Nominal |
Nature of Heat |
Initial Volume |
Finalc Volume |
|
Apparatus |
Volume |
||||
Treatment |
(mL) |
(mL) |
|||
|
(mL) |
||||
|
|
|
|
||
Pipette |
10 |
24 h @ 320°C |
9.970 ± 0.009 |
9.977 ± 0.004 |
|
Pipette |
10 |
Cycled to 320°C* |
9.954 ± 0.030 |
9.954 ± 0.020 |
|
Standard flask |
100 |
Cycled to 320°C* |
99.95 ± 0.01 |
99.94 ± 0.01 |
|
Standard flask |
100 |
168 h @ 320°C |
99.81 ±0.02 |
99.82 + 0.02 |
|
Standard flask |
25 |
168 h @ 320°C |
24.909 ± 0.010 |
24.917 + 0.010 |
0 From the Journal of Chemical Education, 64, p.1054 (1987), with permission. b Consists of eight heat-cool cycles from RT to 320°C with 15 min at 320°C.
c Mean and standard deviation of eight determinations at 26°C.
One type of Type II glass, Exax (from Kimble), has anti-static properties, which make it particularly suitable for powders.
Resistance to Chemicals. Exposure to all alkalines should be kept to a minimum (minutes). Exposure to hydrofluoric and perchloric acid should be limited to seconds. Volumetric ware used once for these materials should be downgraded (glassware that was Class A should now be considered Class B) or not used at all. If measurements of these acids or alkalines are required, use plastic ware because it is resistant to these chemicals.
Cleaning. All standard cleaning techniques used on glass are safe on volumetric ware. However, base baths and HF should never be used because they are glassstripping agents and because during the cleaning process they remove glass. This stripping would alter any calibrations, making the volumetric ware useless.
Contrary to common belief, it is safe to place borosilicate volumetric ware in a drying oven. While there has not been a study indicating the effects of heating on Type I, Class B or Type II glass, there was a study on Type I, Class A volumetric ware. The study was done by Burfield and Hefter,6 and the results (which are shown in Table 2.8) clearly indicate that any variations from the original volume are within tolerances even for Class A glassware.
The results of Table 2.8 notwithstanding, there still is the question of how to dry and/or store other types of volumetric glassware as well as plastic ware. First, plastic ware does not need oven drying because plastic does not absorb water. Second, Type II glassware measurements will not be significantly affected by remaining distilled water (from the final rinse), so again there is no reason to dry this glassware. There is also no reason to dry to contain glassware between repeated measurements of the same solution. However, all other volumetric glassware should be dried prior to use.
Because of contamination concerns, it is not recommended that you place volumetric ware on a standard drying rack because the pegs may introduce foreign