- •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
Traps 7.4 |
391 |
prevent cross-contamination during periods of nonuse. Any trap design that allows baking should have some barrier that limits (or prevents) human contact with the trap while heating is taking place to prevent burns. Because liquid nitrogen cold traps present special safety and use concerns, the next two sections provide more detailed instruction of their use.
7.4.3 Proper Use of Cold Traps
It is not uncommon for those using vacuum systems to consider trap functionality as limited to catching condensable vapors as they leave the vacuum system on their way to the pumping devices. It all too common for people to forget that besides the trap protecting the pump(s), the traps also protect the vacuum system from materials backstreaming from the pumps. Optimally, this second (but no less important) function of traps increases potential vacuum by limiting backstreaming.
For something so important, it is surprising how neglected the traps on a vacuum systemare, and how poorly they are maintained. Just as one can do significant damage to a car by neglecting the oil filter and motor oil, many a vacuum system is not performing as well as it could due to a few oversights to trap use. Aside from the issue of maintenance, issues for optimum system performance should include trap selection, how the trap is designed, and how the trap is attached to the vacuum system.
For the many vacuum processes that do not generate, or release, any significant quantities of condensable vapors, trap orientation is for the most part irrelevant. However, for the many other vacuum processes that do generate, or release small to significant quantities of condensable vapors, the orientation can have significant ramifications. If the liquid nitrogen trap is attached the one way, there can be a build-up of excess frozen materials in the center tube resulting in a reduction of the trap's throughput. With sufficient amount of vapors, this reduction could eventually lead to a complete cutoff of all gas flow through the trap (see Fig. 7.31). By simply orienting the trap the other way, the buildup of frozen vapors collects on the outer wall, leaving the center tube free for gas transport.
In addition to more efficient throughput, the trap arrangement on the right of Fig. 7.31 allows one to remove the condensate while frozen. This helps prevent the condensate from drifting back into the system after it has defrosted, and if there are any particularly dangerous materials, they can be moved to a fume hood for dealing with in a safe manner.
There is an argument in favor of the design on the left of Fig. 7.31: If there is poor trap maintenance, and the frozen vapors defrost (and collect on the bottom of the trap), there is no chance for these liquids to be sucked into the pumps by someone throwing a switch or stopcock at the wrong time. However, for this amount of liquid to reach the level of the inside tube indicates poor trap maintenance. In addition, this amount of condensate had to have effected gas transport.
392 |
Vacuum Systems |
Table 7.10 Trap Selection0
TA»
TA*
TA*
TA6
TA>
TA"
TMC
TMC
TMC
TMC
TO*
1C"
Molecular
Coaxial Traps Particulate Traps
Sieve
(•"revent oil
back-stream- ing
Trap water vapor Trap organics (e) Trap acidic vapors Trap ironcontaining vapors Trap particulates Time interval to leplace elements Regeneration in situ Need only clean trap Refrigerant hold time (hrs) Trapping mech. operating temperature Limiting pressure Can lower pump base pressure
Stainless Steel Element |
Copper Element |
Activated Alumina Element |
Activated Charcoal Element |
Magnetic Element |
Synthetic Zeolite Charge |
|
* * |
•fr** |
-fr-ft-ft- |
N/R |
* * |
*** |
|
N/R |
N/R |
-fr-ft- |
N/R |
N/R |
N/R |
|
N/R |
N/R |
N/R |
KK |
N/R |
N/R |
|
N/R |
N/R |
KK |
N/R |
N/R |
N/R |
|
N/R |
N/R |
N/R |
N/R |
•ft-* |
N/R |
|
•ft-* |
||||||
|
|
|
|
|
||
/ |
f |
N/R |
N/R |
(2) |
N/R |
|
Six |
Six |
Vapor |
Vapor |
Load |
Vapor |
|
months |
months |
load? |
load? |
? |
load? |
|
No |
No |
No |
No |
No |
Yes |
|
No |
No |
No |
No |
No |
|
|
- |
|
- |
- |
- |
- |
Room Room Room Room Room Room temp. temp. temp. temp. temp. temp.
|
10^ |
104 |
W4 |
1CT4 <10J t |
|
- |
- |
Yes |
- |
- |
Yes |
|
|
Activated Alumina |
Charge |
* * *
N/R
N/R
N/R
N/R
N/R
Vapor
load?
Yes
-
-
Room
temp.
<10"3
Yes
Liquid Nitrogen |
Dry-Ice Slurry |
Water-Cooled |
Polyester Element |
Drop-out |
-ft-* |
• f r * |
N/R |
* * |
•ft- |
|
* * |
* * • |
N/R |
•ft-ft- |
•ft- |
|
•ft-ft- |
• f t - * |
-ft-* |
**
* * |
•ft- |
N/R |
|
•ft- |
|||
|
|
||
N/R |
N/R |
N/R |
|
N/R |
N/R |
N/R |
|
- |
- |
- |
|
- |
- |
- |
|
Yes |
Yes |
Yes |
|
2 to |
>24 |
Cont |
|
4 |
|
|
|
|
|
l t o |
|
198° |
79° |
20° |
|
C |
C |
C |
|
10"5 |
lO"3 |
IO-4 |
|
Yes |
- |
- |
N/R N/R
N/R N/R
N/R N/R
N/R N/R
>0.01 >0.02 mm mm
>0.01 >0.02 mm mm
--
-
-
Yes Yes
--
Room Room
temp. temp.
io-3 10"3
--
a From Vacuum Products by Welch Vacuum, Thomas Industries, Inc., p. 107, © 1988 by Welch Vacuum Technology, Inc., reproduced with permission.
~fr - Fair: -fr-fr - Good: -fr-fr-fr - Very Good: -k~k~k-k - Excellent: N/R - Not Recommended
b Trap applications (ratings are qualitative guidelines, if you have questions, call the manufacturer of your pump).
c Trap Maintenance.
dTrap Characteristics.
eExamples: paraffins, solvents, organic acids, alcohols.
^Coaxials can trap large particulates, but are not designed for this purpose.
Traps 7.4 |
|
393 |
System |
Vacuum A |
|
|
/T\ |
System |
|
|
Frozen vapor |
Frozen vapor |
|
buildup |
buildup |
|
|
If the system is attached to the center inlet, the material will freeze as it enters the liquid nitrogen area, thus reducing the flow potential. It can eventually close up.
When the system is attached to the side inlet, the material will freeze on the side walls as it passes through the cold trap. There is no restriction of flow with this orientation.
Reduced |
Continuous |
throughput |
throughput |
-ig. 7.31 If a cold trap is improperly oriented, the system may clog up. |
Constant removal of the trapped materials should always be done, but with this orientation, it is less critical.
One other disadvantage of the reduced throughput orientation is that as the vacuum improves, the trap's ability to trap decreases. This is due to less air to conduct the cold of the coolant to the inside of the trap. The continuous throughput orientation, on the other hand, has the coolant on direct contact with the outer walls of the trap, ensuring a constant temperature at any vacuum.
The best throughput is obtained by using the ratio that Dushman38 recommends where the inside diameter of the inner tube divided by the inside diameter of the
outer tube. When this ratio is 0.62, the cold trap's throughput is at its most |
effi- |
cient, regardless of the orientation.* Rosebury studied the ratio between |
the |
inside and outside tube with consideration to the length of the cold trap for maximum trapping efficiency. He found that a short, fat cold trap has much better conduction than a long, thin cold trap, but such a trap's ability to trap condensable vapors will be severely handicapped due to limited opportunities for the vapors to come into contact with a wall. Although there is a penalty for a longer trap, if the ratio of 0.62 is maintained, maximum (for that length) conductance will be at a maximum.
*If the traps are oriented as shown on the right of Fig. 7.31, the quality of throughput is maintained regardless of the amount of frozen vapors.
394 Vacuum Systems
Improper selection of coolant for a cold trap may artificially limit the potential vacuum of your system. For instance, the vapor pressure of water (which is often the primary condensable vapor in many vacuum systems) is quite high without any cold trapping, moderate at dry-ice temperatures, and negligible at liquid nitrogen temperatures (see Table 7.11). If your vacuum needs are satisfied within a vacuum of 5 x IO"4 torr, you can safely use dry ice (and save money because dry ice is less expensive than liquid nitrogen). Another temperature option for a coolant is the slush bath (for more information on coolants see Sec. 6.2).
Starting a vacuum system should include the following trap use procedures for safe and efficient vacuum system operation:
1. Prevent Air (Oxygen) from Condensing within the Cold Trap. One of the more common laboratory accidents can occur when air (oxygen) is frozen in a cold trap. This accident is caused by placing a cold trap within liquid nitrogen while there is still sufficient oxygen within the trap to be condensed. Later, once the liquid nitrogen is removed (either intentionally or is boiled off) the condensed air vaporizes. The excess pressure created by this frozen air can result in anything from stopcock plugs being blown across the room to an explosion of the entire line. Many labs have "horror stories" of these potentially dangerous, and always costly, occurrences.
To prevent oxygen from freezing in cold traps, be sure that there is no air in the trap when pouring liquid nitrogen around the cold trap. If you suspect that you
Table 7.11 Vapor Pressure of Various Substances
as a Function of Temperature0
Temperature Vapor Pressure, torr
°C |
K |
Water |
NH3 |
co2 |
Hg |
100 |
373.1 |
760 |
|
|
2.7 X 10"1 |
50 |
423.1 |
93 |
|
|
1.3 x 102 |
0 |
273.1 |
4.6 |
3,220 |
|
2X10"4 |
-40 |
233.1 |
0.1 |
540 |
|
1 x IO6 |
-78.5* |
194.6 |
5. x IO4 |
42 |
760 |
3 x 10"9 |
-120 |
153.1 |
io-7 |
0.2 |
10 |
10"13 |
-150 |
123.1 |
io-14 |
6X10"4 |
6 x 10"2 |
|
-195.8** |
77.3 |
= 1 0 " 2 4 |
io-11 |
10"8 |
|
" From VacuumScience and Engineering by CM. Van Atta, © 1965, McGraw-Hill, Inc., p. 331, reproduced with permission.
* Sublimation temperature of dry ice at 760 torr (one atmosphere). c Boiling point of liquid nitrogen at 760 torr (one atmosphere).
Traps 7.4 |
395 |
may have air condensed in the cold trap,* be sure the frozen air has room to expand. There are three ways to prevent explosions from frozen air:
1.Leave that section of the vacuum system in a continuous state of vacuum, never bringing it up to room pressure. (This is not always possible because traps often need to be removed to empty their contents.)
2.Begin pumping with the mechanical pump for a few minutes to make sure that the trap is below =1 torr before placing liquid nitrogen around the cold trap. A pump running against atmospheric pressure is noisier than one running against a vacuum. Thus, once the pump noise has dropped, it is safe to place the trap within liquid nitrogen.
3.Leave a stopcock open (to the atmosphere) at the end of an experiment to vent the system after the work is done. However, if you do this, be sure to remove the liquid nitrogen from the trap before opening the vent. Otherwise you will be condensing oxygen that is drawn in by the open vent.
Suggestion 1 should always be practiced whenever possible. The re-entry of atmosphere into a vacuum system reintroduces copious amounts of moisture onto the vacuum system's walls and reintroduces gases back into the liquids within your system (oil and/or mercury). The next time the system is used, the walls will need to be re-dried and the liquids re-outgassed. Thus, a greater amount of time than would otherwise be necessary will be required the next time you wish to obtain a vacuum. This extra time will also place more wear and tear on your pumps and expose them to extra condensable vapors.
Suggestion 2 should always be done as standard practice. Assuming your traps are emptied of liquids and condensable vapors, there should be nothing available to damage the pumps. Therefore, the practice of running the pumps for a few minutes (before placing liquid nitrogen around the cold traps) helps ensure that an insufficient amount of air is available for the oxygen to be condensed.
Suggestion 3 has limited practicality. It can only be effective after work on the vacuum line is complete and you wish to shut down the system. This plan will not help vacuum lines left unattended and/or whose liquid nitrogen has boiled off. Regardless, if frozen oxygen boils off faster than can be released by the vent, the results would be the same as if no vent were available. Thus, the potential for disaster is still present.
In practice, use Suggestions 1 and 2. It is better to ensure that no air freezes within the system than to develop techniques to deal with problems that should be avoided.
2. Limit the Amount of Moisture Near the Top of Your Cold Trap. A common error when first starting up a vacuum system is pouring liquid nitrogen too high into a Dewar. People often overfill Dewars in the early startup process
*Frozen oxygen will appear as a lightly blue-tinged liquid in the bottom of the trap. Oxygen is one of the few materials to remain a liquid at liquid nitrogen temperatures.