- •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
Weight and Mass 2.4 |
131 |
compensated for in the electronics, especially when used in conjunction with servo-controlled balances.
2.4.9 Beam Balances
Beam balances fall into the unequal arm balance category. Generally, they are not capable of weighing very light objects (<0.1 g). They obtain greater precision by having a separate beam for each decade of weight capability (by splitting up the measurements on different beams, you obtain greater distance for each subdivision of weight. Otherwise, the gradations are closer together, making it more difficult to distinguish between them).
As seen in Fig. 2.27, the higher weight readings (the 100and 10-unit beams) of a beam balance have notches at regular intervals, which forces the sliding weight to consistently land in the same spot each time the weight is moved to that location. This design helps ensure precision (repeatability) for those weight ranges as well. The 1.0-unit beam has no notches, which allows the user to slide the counter weight along the beam until the balance arm is in balance.
Before using a balance, be sure that it is level with the surface of the table. Some beam balances have a built-in level for this purpose. Screw the legs of the balance until the balance is level. Balances that do not have built-in levels are not expected to have the accuracy of those requiring precision-leveling. Regardless, you should always level the balance as best you can by eye.
Before an object is weighed, the balance should first be nulled, or zeroed. This zeroing procedure is done with nothing on the balance pan and by placing all of the weights (on each beam) to their zero points. If the balance does not indicate "centered," rotate the balancing screw (on the pan side of the balance) as necessary to zero, or "balance" the balance. Balances that require you to complete (finish) the balance process with the beam in the same balanced (null) position at which you started are called null-type balances.
To weigh an object, place the unknown object on the center of the balance pan. Move the heaviest weight over, a few notches at a time, until the beam side is heavier than the pan side. Move that weight back one notch, then take the next heaviest weight and slide it over, a few notches at a time, until the beam side is again heavier than the pan side. Move that weight back one notch. Repeat this process for all of the weights on notched beams.
The lightest-weight beam has no notches. Slide the counter-weight until the beam and pan are balanced. Reading the weights on the balance involves adding up the weights on the various beams. Figure 2.27 shows the counter-weights on the three beams at "70," "8,"and "0.76." Thus, the reading of this triple-beam balance is "78.76."
After you complete a weighing and record the value in your log book, remove the object and return the counter-weights to their zero value.
132 |
Measurement |
|
1.0 |
v |
v—i |
9 |
10 I |
Fig. 2.27 The calibration readings of a three-beam balance.
2.4.10 Analytical Balances
Analytical balances are those ofClass I and Class II (see Table 2.21) and require a division of the scale's capacity that is typically smaller than 10~5of the total capacity with a readability of0.1 \\g to0.1 mg (IO"7 to 10"4 g). Analytical balances have thegreatest precision forthe most demanding work. Formany years, only a properlymade two-pan balance* could achieve the precision required toobtain the required level of accuracy. Despite their accuracy, weighings made on two-pan balances were slow andinefficient. Eventually, technology improvements in sin- gle-pan balances brought them to meet andeventually exceed thecapabilities of two-pan balances, yetmaintain their speed and efficiency.
As can be seen in Table 2.23, a balance that can read 5 grams to 4 decimal points is inthe same class as a balance that can read 500 grams to 1decimal point. Thus, an analytical balance is not onethat canread only small amounts to very small intervals, but is practically anybalance that can read its capacity to very
Table 2.23 Laboratory Analytical Balances14
Balance name |
Capacity |
Scale |
|
Divisions" |
|||
|
|
||
Macrobalance |
100-200g |
io-5 |
|
Semimicrobalance |
30-100g |
io-5 |
|
Microbalance |
3-50 g |
io-5 |
|
Ultramicrobalance |
3-5 g |
IO6 |
" Scale divisions are the number of divisions of the total capacity of a balance.
It isunlikely that you will find the classic two-pan balance inuse inlaboratories. In a way this omission is a pity because they are typically beautifullymade instruments. For those of you who may still use them, I cannot fault you foryour romantic actions. For those of you who are considering getting rid of one to make room, please do not. You do notneed to useit,just keep it and let its beautiful construction remind youof the art that is possible in technology. Because of the rarity of two-pan balances in contemporary labs, there will be nodiscussion of their use oroperation inthis book.
Weight and Mass 2.4 |
133 |
Fig. 2.28 The single pan balance.
small intervals. The terms microbalance or semimicrobalance do not refer to the size of the calibrations, rather they refer to the capacity of the scale. In fact, an analytical balance can have a capacity as great as 50 kg so long as the scale divisions are smaller than 10"5 of the total capacity. The names of the standard analytical balances used in the laboratory are shown in Table 2.23.
A single-pan balance (Fig. 2.28) is typically one in which all that the user sees is a single pan in a container with several knobs and levers on the front or sides. There also will likely be some optical component that the user may see as a frosted screen or digital readout. There are four major types of single-pan balances: mechanical, mechanical with an optical deflector (for the smallest measurements), servomotor, and hybrids of mechanical (for larger weights) and servomotor (for smaller weights). Although you will still find the former two types of balances in laboratories, most of the balances currently in production today are of the latter two types.
Most of these balances will have either a magnetic or air damper, which arrests the free movement of the balance beam. This damper also allows the balance to come to a rest position much faster than otherwise possible. In addition, hybrid mechanical single-pan balances have a lever arm that can prevent, partially free, and completely free the balance beam's movement. This three-part varying restriction is important, for it protects the knife edge on which the balance beam rocks during gross, or rough, movement actions, yet it allows free and easy movement when final measurements are made. When objects are being placed on the pan, the lever should be in the fully arrested position to prevent any movement of the beam and protect the balance's mechanical parts. Partial movement of the balance beam allows safe addition and subtraction of heavier weights. Full motion of the balance beam is necessary when light (mg) weights or optics are used for final weighing.
The mechanical aspect of these balances typically employs a crankshaft or rocker arm assembly that supports the weights. The weights are engaged or disengaged on the balance beam as the shaft is turned. Typically, only four weights per
134 |
|
|
|
|
Measurement |
Table 2.24 The Addition of Weights From 0 to 10 |
|
||||
|
Nothing |
|
|
|
0 |
1 |
|
|
|
|
1 |
1 |
+ |
1 |
|
|
2 |
3 |
|
|
|
|
3 |
1 |
+ |
3 |
|
|
4 |
5 |
|
|
|
|
5 |
1 |
+ |
5 |
|
|
6 |
1 |
+ |
1 |
+ |
5 |
7 |
decade are required. An example of the weights necessary to go from 0 to 10 would be 1, 1, 3, and 5 (the 0 to 10 range as shown in Table 2.24). The selection of weights is handled internally by the crankshaft. The user simply rotates the dial until the proper deflection is noted on the balance's viewing screen.
The counterbalance weights within a single-pan balance are described as having an apparent mass. The term apparent mass is used because what you are reading is different from true mass due to the effects of air buoyancy. If corrections are made for air buoyancy (see Sec. 2.4.3), you have true mass. In more recently manufactured single-pan balances,* the apparent mass has been changed from 8.3909 g/cm3 (brass) to the current 8.0 g/cm3 (stainless steel). This change was made to better approximate the density of grade S weights (see Sec. 2.4.13 and Table 2.26). The density of the apparent mass used within a balance should be identified somewhere on the balance and/or in its literature. If you are using a balance with the older apparent mass and switch to a balance with the newer apparent mass, you would need to add a 0.0007% correction to the total weight. This correction is equivalent to 7 mg in 1 kilogram and is so significantly lower than the tolerance of most balances that the correction is not really necessary.
Regardless of whether a single-pan balance is completely mechanical or a hybrid, there are several advantages of the single-pan balance over the two-pan balance:
1.Because the weights are inaccessible to the user, there is no chance for the weights to be accidentally touched. Analytic balances are so sensitive that fingerprints, or corrosion from fingerprints, can alter the weight of analytic weights.
2.The single-pan balance can make use of optics and/or servomotors (see next section) to obtain the smallest weight measurements. By eliminating mechanical deflection of weights for the final part of the mea-
*This was changed in the mid-1970s.
Weight and Mass 2.4 |
135 |
surement process (such as a gold chain* or rider1), repeatability is substantially improved.
3. Single-pan balances typically have damping devices that help to minimize the free swinging of the lever arm. This device speeds the weighing process immensely over the time spent "counting swings" for two-pan balances.
There are many different brands and models of single-pan balances. Each has its own mechanism for weighing an object. As in all other lab equipment, the original manual, or a copy of the same for information on how to use the balance, should be readily available. Regardless, the general procedures are typically similar: The larger weights are invariably manipulated by dials for each decade of weight. These dials are rotated until the appropriate weight is obtained or until the final weighing is complete.
Weighing an object on a single-pan balance typically involves first making sure that the balance is nulled. This procedure is done by setting all dials to "0," rotating the lever arm to the free arm position, and manually setting the servomotor or optical window to "0.00" to verify its "null" starting point. Once the balance is set, return the lever arm to the arrest position before placing the object to be weighed on the center of the pan, inside the door of the balance. For very sensitive weighing, do not handle the object with your bare hands. Select tongs that are sufficiently long so that your hands do not get into the weighing chamber area. Close the door and wait a few minutes to allow the internal sections of the balance to regain equilibrium for both drafts and temperature.
The weighing procedure is made by rotating the lever arm to the semi-release position. Slowly rotate the weight knobs from lighter to heavier. When the scale deflects, back up one weight calibration (for instance, if the scale deflects when the gram dial is rotated to "7," rotate the dial back to "6"). Continue the process for each weight dial until the final weight measurement is attained.
It is not possible to specifically explain how to make the smallest weight division weighing for single-pan balances in a book like this one because there are so many different ways it can be done depending on the brand or model of balance. Regardless, the general procedure for a final measurement is made by rotating the arresting arm from the partial freedom position to the full freedom position. Then dial, turn, or observe the smallest weight division for the completed weight. Once the weight has been determined, return the arresting arm back to the full arrest
A gold chain was used on one design of the single-pan balance. The gold chain was unwound onto the balance pan until the sample and internal weights balanced. The length of chain on the pan was directly equal to its proportional weight and therefore the length of chain was used to make the final measurement digit.
tThe rider is a sliding counterbalance that is used to make the final weight calibration on two-pan balances.