- •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 |
161 |
to use) thermometers. In addition, they are used to determine the temperatures of melting, boiling, and transformation points of various materials. Because of their limited use in the average laboratory, further discussion of pressure expansion thermometers is beyond the scope of this book.
2.5.11 Thermocouples
Thermocouples are robust and inexpensive. Reading the temperature from a thermocouple is invariably as easy as reading a controller's dial, liquid crystal, or LED. The following commentary is intended to provide a basic understanding of the operation of thermocouples and their limitations. If you have any questions about the final selection of a thermocouple, controller, lead, and extension for any specific type of job or desired use, contact a thermocouple manufacturing company because it will likely provide you with the best information on how to make your system work.
Table 2.33 Thermocouple Types and Characteristics
ANSI Symbol |
Composition (pos. - neg. lead) |
J |
Iron - Constan- |
|
tan (Cu-Ni) |
Temperature
Range (°C)
Comments
(Thermocouple)
(Extension)
0 to 750 |
Recommended for reducing atmosphere. Displays |
0 to 200 |
poor conformance characteristics due to poor iron |
|
purity. Above 538°C, oxidation of Fe in air is rapid |
|
so heavy-gauge wire is recommended for extended |
|
use. Should not be used bare in sulfurous atmo- |
|
spheres above 538°C. |
T Copper - Con- |
-200 to 350 |
Recommended for mildly oxidizing and reducing |
stantan (Cu- |
-60 to 100 |
atmospheres as well as moist environments. Per- |
Ni) |
|
forms very well at low temperatures and limits of |
|
|
error are guaranteed in the subzero range, although |
|
|
type E may be preferred due to higher emf. The cop- |
|
|
per lead makes secondary compensation unneces- |
|
|
sary. |
K Chromel - |
-200 to 1250 |
Alumel |
0 to 200 |
Recommended for clean oxidizing atmospheres. They can be used in reducing atmospheres, but they should not be cycled from reducing to oxidizing and back repeatedly. The higher temperature ranges can only be achieved with heavy-gauge wires. They should not be used in vacuums and should not be bare in sulfurous atmospheres.
*LED stands for light emitting diode. These devices are the lighted numerals typically seen on digital clocks.
162 |
Measurement |
Table 2.33 Thermocouple Types and Characteristics (continued)
ANSI Symbol |
Composition (pos. - neg. lead) |
E |
Chromel - Con- |
|
stantan (Cu- |
|
Ni) |
Temperature
Range (°C)
Comments
(Thermocouple)
(Extension)
-200 to 900 |
Recommended for vacuum use or for inert, mildly |
0 to 200 |
oxidizing or reducing atmospheres. These thermo- |
|
couples produce the greatest amount of emf and |
|
therefore can detect small temperature changes. |
S Platinum - Plati- |
0 to 1450 |
num 10%, |
0 to 150 |
Rhodium |
|
Recommended for use in oxidizing or inert atmospheres to 1400°C, although it may be brought to 1480°C for a short time. Most stable, especially at high temperatures. Type S is used for standard calibration between the antimony point (630.74°C) and gold point (1064.43°C). Should only be used inside nonmetallic sheaths such as alumina due to metallic diffusion (from metal sheaths) contaminating the Pt.
R |
Platinum - Plati- |
0 to 1450 |
|
num 13%, |
0 to 150 |
|
Rhodium |
|
B |
Platinum - Plati- |
50 to 1700 |
|
num 30%, |
0 to 100 |
|
Rhodium |
|
Na |
Omega-P™ |
-270 to 1300 |
|
"Nicrosil" (Ni- |
0 to 200 |
|
Cr-Si) - |
|
|
Omega-N™ |
|
|
"Nisil" (Ni-Si- |
|
|
Mg) |
|
Ga |
Tungsten - |
0 to 2320 |
|
Tungsten |
0 to 260 |
|
26%, Rhodium |
|
Ca |
Tungsten 3% |
0 to 2320 |
|
Rhodium - |
0 to 870 |
|
Tungsten |
|
|
26%, Rhodium |
|
Da |
Tungsten 3% |
0 to 2320 |
|
Rhodium - |
0 to 260 |
|
Tungsten |
|
|
25%, Rhodium |
|
Recommended for use in oxidizing or inert atmospheres to 1400°C. although it may be brought to 1480°C for a short time. Should only be used inside nonmetallic sheaths such as alumina.
These thermocouples are excellent for vacuum use. The output between 0 and 50°C is virtually flat and therefore is useless at these temperatures. The reference junction can be between 0° to 40°C. Should only be used inside nonmetallic sheaths such as alumina.
Similar to type K, but with improved oxidation resistance at higher temperatures.
Useful in reducing or vacuum environments at high temperature, but not for oxidizing atmospheres.
Useful in reducing or vacuum environments at high temperature, but not for oxidizing atmospheres.
Useful in reducing or vacuum environments at high temperature, but not for oxidizing atmospheres.
" Not ANSI designations.
Temperature 2.5 |
163 |
Junction 3
Junction 1
CM |
. |
C
Voltmeter I V
Junction 2
Fig. 2.31 A simple diagram of a copper-constantan thermocouple.This illustration is from The Temperature Handbook©1989 by Omega Engineering, Inc. All rights reserved. Reproduced with the permission of Omega Engineering, Inc., Stamford, CT 06907
In 1821 Thomas Seebeck discovered that when two different types of metal wires were joined at both ends and one of the ends was heated or cooled, a current was created within the closed loop (this current is now called the Seebeck effect). Specifically, heat energy was transformed into measurable electrical energy.
Unfortunately, there is not enough current produced to do any work, but there is enough to measure (1 to 7 millivolts). This rise in potential energy is called the emf or electromotive force.
By hooking the other end of joined dissimilar wires up to a voltmeter and measuring the emf (output), it is possible to determine temperature. Such a tempera- ture-measuring device is called a thermocouple.
There are seven common thermocouple types as identified by the American National Standards Institute (ANSI). They are identified by letter designation and are described in Table 2.33. There are four other thermocouple types that have letter designations; however, these four are not official ANSI code designations because one or both of their paired leads are proprietary alloys. They are included at the end of Table 2.33. Although Table 2.33 lists the standard commercially available thermocouples, there are technically countless other potential thermocouples because all that is required for a thermocouple is two dissimilar wires.
At a basic level, it seems that one should be able to take any thermocouple, attach it to a voltmeter, and determine the amount of electricity generated from the heat applied to the dissimilar junction. Then the user could look in some predetermined thermocouple calibration table* to determine the amount of heat that the amount of electricity from that specific type of joined wires produces.
One of the negative complications of thermocouples is that they do not have a linear response to heat. In addition, as temperature changes, thermocouples do not
'Thermocouple calibration tables have been compiled by the NIST and can be found in a variety of sources such as the Handbook of Chemistry and Physics by the Chemical Rubber Company, published yearly.
164 Measurement
produce a consistent emf change. Therefore, there must be individual thermocouple calibration tables for each type of thermocouple.
If you look at a thermocouple calibration table, you will see that it has a reference junction at 0°C. This reference point is used because of an interesting complication that arises when a thermocouple is hooked up to a voltmeter. To explain this phenomenon, first look at one specific type of thermocouple, a type T (cop- per-constantan design). Also, assume that the wires in the voltmeter are all copper. Once the thermocouple is hooked to the voltmeter, we end up having a total of three junctions (see Fig. 2.31):
Junction 1. The original thermocouple junction of copper and constantan.
Junction 2. The connection of the constantan thermocouple wire to the copper wire of the volt meter.
Junction 3. The connection of the copper thermocouple wire to the copper wire of the volt meter.
We are hoping to find the temperature of Junction 1, but it seems we now have two more junctions with which to be concerned. Fortunately, Junction 3 can be ignored because this connection is of similar, not dissimilar, metals. Therefore, no emf will be produced at this junction. Junction 2 presents a problem because it will produce an emf, but of an unknown temperature; this means that we have two unknowns in the same circuit, and we are unable to differentiate between the two. Any voltmeter reading taken at this point will be proportional to the temperature difference between the first and third junction.
If we take Junction 2 and place it in a known temperature, we can eliminate one of the two unknowns. This procedure is done by placing Junction 2 (now known as the reference junction) in an ice bath of 0°C (known as the reference temperature). Because the temperature (voltmeter) reading is based on an ice-bath reference temperature, the recording temperature is referenced to 0°C (see Fig. 2.32).
Junction 1
Junction 2 (Reference temperature)
Junction 4 |
\^.^mj - ^ ^ |
IC6 bath
Fig. 2.32 A thermocouple using an ice bath for a reference temperature.This illustration is from The Temperature Handbook©1989 by Omega Engineering, Inc. All rights reserved. Reproduced with the permission of Omega Engineering, Inc., Stamford, CT 06907
Temperature 2.5 |
165 |
References for voltmeter/thermocouple readings (found in such books as the CRC Handbook) will usually indicate that they are referenced to 0°C. Because Junctions 3 and 4 are of similar metals, they have no effect on the emf.
This example is limited because it is representative only of thermocouples with copper leads. In all other thermocouples, there are likely to be four dissimilar metal junctions and therefore up to four Seebeck effects. However, by extending the copper wires from the voltmeter and attaching them to an isothermal block, placing the same type of wire from one of the thermocouple leads to the part between the icebath and the isothermal block, and then attaching the thermocouple wires to the isothermal block (to eliminate thermal differences at these two junctions), it is possible to cancel out all but the desired Seebeck effect (see Fig. 2.33).
It is obvious that the use of an ice bath is inconvenient and impractical. Maintaining a constant 0.0°C temperature can be difficult, and there always is the possibility of the icebath tipping over. Fortunately there are two convenient techniques to circumvent the need for an actual ice bath for thermocouple measurements.
One approach requires measuring the equivalent voltage of the ice-bath reference junction and having a computer compensate for the equivalent effect. This technique, called software compensation, is the most robust and easiest to use. However, depending on the equipment used, the lag time involved for the compensation may be unacceptable.
Alternatively, it is possible to have hardware compensation by inserting an electric current (typically from a battery) to provide a voltage which electronically offsets the reference junction. This approach is called an electronic ice-point reference. This method has the simplicity of an ice bath, but is far more convenient to
|
Isothermal |
Junction 3 |
Block |
|
Junction 1 |
|
Fe |
|
Junction 2 |
|
(Reference |
|
temperature) |
|
Ice |
|
bath |
Fig. 2.33 An iron-constantan thermocouple using an isothermal block and an ice bath. This illustration is from The Temperature Handbook©! 989 by Omega Engineering, Inc. All rights reserved. Reproduced with the permission of Omega Engineering, Inc., Stamford, CT 06907
166 |
|
Measurement |
|
Table 2.34 American Wire Gauge |
|||
|
Size Comparison Chart |
||
AWGa |
Diameter |
Diameter |
|
(mils) |
(mm) |
||
|
|||
8 |
128 |
3.3 |
|
10 |
102 |
2.6 |
|
12 |
81 |
2.1 |
|
14 |
64 |
1.6 |
|
16 |
51 |
1.3 |
|
18 |
40 |
1.0 |
|
20 |
32 |
0.8 |
|
22 |
25 |
0.6 |
|
24 |
20 |
0.5 |
|
26 |
16 |
0.4 |
|
28 |
13 |
0.3 |
|
1 American Wire Gauge. |
|
||
use. The major disadvantage is that a different |
electric circuit is required for each |
||
type of thermocouple. |
|
|
Ironically, the sophistication of modern controllers typically makes most of the concerns about how temperature is determined irrelevant. The greatest concern for the user is to select the right type and size of thermocouple for the specific job and environment, then to select the proper controller for that type of thermocouple.
Although there are many overlapping temperature ranges among various thermocouple types, all types of thermocouples perform better for some jobs than others. For example, Type K is significantly less expensive than Type R, although both thermocouples can read into the 1000°C range. This similarity would lead one to believe that either choice is adequate, however Type K is preferred because of its lower cost. If all you need are occasional readings of such temperatures, you could get by with Type K. However, if you expect to do repeated and constant cycling up to temperatures in the 1000°C range, Type K would soon fail and would need to be replaced. Unfortunately, you are not likely to notice failure developing until something has obviously gone wrong. Because the potential costs of failure are likely to be greater than the additional cost of the more expensive thermocouple, it may be more economical to obtain the more expensive type R at the outset.
Sample size should also be considered when selecting thermocouple size. If a large thermocouple (with a high heat capacitance) is used on a small sample (with a low heat capacitance), the sample's temperature could be changed. As stated before, the act of taking an object's temperature can change its temperature.