- •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
Temperature 2.5 |
167 |
Because thermocouples come with varying wire diameters (see Table 2.34), select the thermocouple wire size best suited to measure your sample.
Be advised that the upper range of temperatures cited (within thermocouple catalogs) for a given thermocouple are related to the larger wire sizes. Thus, a smallwire thermocouple is likely to fail at the upper temperature ranges for that particular thermocouple type.
Environment also influences the selection of thermocouples. The condition of the region where the thermocouple will be placed can be oxidizing, reducing, moist, acidic, or alkaline, or it can present some other condition that could cause premature failure of the thermocouple. Selection of the right type of thermocouple can help avoid premature failure. Fortunately, there are sleeves and covers available for thermocouples that prevent direct contact with their various environments. These covers are made of a variety of materials, from metals to ceramics, making selection of the right material easy. On the other hand, covers add to the heat capacitance of the entire probe and therefore can slow thermocouple response time; and because of a greater heat capacity, they are more likely to affect the temperature of the material being studied.
2.5.12 Resistance Thermometers
In 1821, Sir Humphrey Davy discovered that as temperature changed, the resistance of metals changed as well. By 1887 H.L. Callendar completed studies showing that purified platinum wires exhibited sufficient stability and reproducibility for use as thermometer standards. Further studies brought the Comite International des Poids et Measures in 1927 to accept the Standard Platinum Resistance Thermometer (SPRT) as a calibration tool for the newly adopted practical temperature scale.
Platinum resistance thermometers are currently used by the NIST for calibration verification of other thermometer types for the temperature range 13.8 to 904 K. In addition, they are one of the easiest types of thermometers to interface with a computer for data input. On the other hand, platinum resistance thermometers are very expensive, extremely sensitive to physical changes and shock, have a slow response time, and therefore can take a long time to equilibrate to a given temperature. Thus, resistance thermometers are often used only for calibration purposes in many labs.
Platinum turned out to be an excellent choice of materials because it can withstand high heat and is very resistant to corrosion. In addition, platinum offers a reasonable amount of resistivity (as opposed to gold or silver), yet it is very stable and its resistance is less likely to drift with time. However, because it is a good
168 |
Measurement |
conductor of electricity, the SPRT requires a sufficiently long enough piece of platinum wire* to record any resistance.
One of the easiest ways to get a long piece of material in a small (convenient) area is to wrap or wind the material around a mandrel. The typical mandrel used on SPRTs is made of either mica or alumina. The sheaths covering the wrapped thermometer may be borosilicate, silica glass, or a ceramic (see Fig. 2.33). Note that both examples in Fig. 2.33 show four leads where, logically, there should be only two. This is done to reduce any unwanted resistance from the region beyond the thermometer.
An alternative approach to "loose winding" the wires is to form the platinum wire and then flow melted glass around the wire to "lock" the wire in place. This method protects the wire from shock and vibration. These resistance thermometers are, unfortunately, limited to temperatures where the expanding platinum will not crack the containment glass. To limit this occurrence, the expansion of the platinum must closely match the glass around which it is wrapped. Resistance thermometers of this design are more rugged, and therefore, they are more likely to be used in the laboratory.
There are many challenges in the construction and use of resistance thermometers, including:
1. The wire itself must be very pure; any impurities will affect the linearity and reliability of the resistance change. The wire itself must also be uniformly stressed, meaning that after construction, the wire must be temperature-annealed to achieve uniform density. Uniform density provides uniform resistance.
Fig. 2.34 Two different SPRT wrapping designs.
'Currently, about 61 cm of 0.075-mm platinum wire is typically used on resistance thermometers.
Temperature 2.5 |
169 |
2.When the wire is wound on the support device, it must be left in a strainfree condition, as any strain can also affect the resistance of metals. Because the platinum will expand and contract as the temperature changes, it must be wound in such a manner that there is no hold-up or strain. Even this strain could affect the resistance of the metal.
3.Although it is doubtful that a lab will make its own SPRTs, I mention construction demands to impress upon the user the importance of maintaining a strain-free platinum wire. Strain on the wire can be introduced not only during construction, but also in use. The most likely opportunities for wire strain are through vibration and bumping.
4.The SPRT must not receive any sharp motions or vibrations. Such actions can affect the resistance of the metal by creating strain. To place this challenge in the proper perspective, consider a SPRT rapped against a solid surface loud enough to be heard (but not hard enough to fracture the glass sheath). The temperature readings could be affected by as much as 0.001°C. Although this variation may not seem like much, over a year's time, such poor use could cause as
much as 0.1°C error.19
Transportation of SPRTs should be as limited as possible. If you are shipping, special shock-absorbing boxes are recommended. If you have an SPRT shipped to you, keep the box for any future shipping needs and storage. Calibrated SPRTs should be hand-carried whenever possible, to minimize shock or vibration. For instance, you should not lay an SPRT on a lab cart for transportation down the hall. The vibration of the cart may cause changes in subsequent temperature readings.
Other precautions that should be taken with SPRTs include the following:
1.When SPRTs are placed into an apparatus, they should be inserted carefully, to avoid bumps and shocks.
2.Try to avoid rapid dramatic changes in temperature. A cold-to-hot change can cause strains as the wire expands within the thermometer. A hot-to-cold change can cause fracture of the glass envelope encasing the thermometer, or of any glass-to-metal seals (which are structurally weak). A hot-to-cold heat change can also cause a calibration shift of the thermometer.
3.Thermometers with covers of borosilicate glass should not be used in temperatures over 450-500°C without some internal support to prevent deformation.
4.Notable grain growth has been observed in thermometers maintained at 420°C for several hundred hours.20 Such grain growth causes the
170 References
thermometer to be more susceptible to calibration changes from physical shock and therefore, inherently unstable.
There are several inherent complications in the use of SPRTs. One involves the fact that an SPRT is not a passive responding device. What the SPRT records is the change in resistance of an electric current going through the thermometer. The mere fact that you are creating resistance means that you are creating heat. Thus, the device that is designed to measure heat also creates heat. The resolution of this situation is to 1) use as low a current as possible to create as little heat as possible and 2) use as large an SPRT as possible (the larger the SPRT, the less heat generated).
Although an SPRT is not a thermocouple, an emf is created at the junction of the SPRT's platinum wires and the controller's copper wires. Fortunately, this emf is automatically dealt with electronically by the controller with the offset-com- pensation ohms technique and can be ignored by the user.
References
1.Verney Stott, Volumetric Glassware H.F. & G.Witherby, London, 1928, pp. 13-14.
2.R.B.Lindsay, "The Temperature Concept for Systems in Equilibrium" in Temperature; Its Measurement and Control in Science and Industry, Vol. 3, F.G. Brickwedde, ed., Part 1, Reinhold Publishing Corporation, New York, 1962, pp.5-6.
3.W.E. Knowles Middleton, A History of the Thermometer and Its Use in Meteorology, TheJohn Hopkins Press, Baltimore, Maryland, 1966, pp. 58-61.
4.A.V. Astin, "Standards of Measurement," Scientific American, 218, pp. 50-62 (1968).
5.E. Ehrlich, et al, Oxford American Dictionary Oxford University Press, 1980.
6.D.R. Burfield and G. Hefter, "Oven Drying of Volumetric Glassware," Journal of Chemical Education, 64, p. 1054(1987).
7.H.P. Williams and F.B. Graves, "A Novel Drying/Storage Rack for Volumetric Glassware," J. of Chem. Ed., 66, p. 771 (1989).
8.D.J. Austin, "Simple Removal of Buret Bubbles," Journal of Chemical Education, 66, p. 514(1989).
9.Dr. L. Bietry, Mettler, Dictionary of WeighingTerms, Mettler Instrumente AG, Switzerland, 1983, p. 12.
10.W.E. Kupper, "Validation of High Accuracy Weighing Equipment," Proceedings of Measurement Science Conference 1991,Anaheim, CA.
11.R.M. Schoonover and F.E. Jones, "Air Buoyancy Correction in High-Accuracy Weighing on Analytical Balance," Analytic Chemistry, 53,pp. 900-902 (1981).
12.W.E. Kupper, "Honest Weight — Limits of Accuracy and Practicality," Proceedings of Measurement Science Conference 1990, Anaheim, CA.
13.From "Weighing the Right Way with METTLER," © 1989 by Mettler Instrumente
References |
171 |
AG, printed in Switzerland.
14.Ibid, Ref. 9, pp. 69. 74, 100, and 118.
15.Jacquelyn A. Wise, Liquid-in-Glass Thermometry, U.S. Government Printing Office, Washington, D.C., 1976, p. 23.
16.E.L. Ruh and G.E. Conklin, "Thermal Stability in ASTM Thermometers," ASTM Bulletin, No. 233, p. 35, Oct. 1958.
17.W.I. Martin and S.S. Grossman, "Calibration Drift with Thermometers Repeatedly Cooled to -30° C," ASTM Bulletin, No. 231, p. 62, July, 1958.
18.W.P. White, "Lag Effects and Other Errors in Calorimetry," Physical Review, 31, pp. 562-582 (1910).
19.J.L. Riddle, G.T. Furukawa, and H.H. Plumb, Platinum Resistance Thermometry, National Bureau of Standards Monograph No. 126, U.S. Government Printing Office, April 1972, p. 9.
20.Ibid, Ref. 19, p. 11.