- •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
386 |
Vacuum Systems |
a Toepler can be seen in Fig. 7.27. In operation, the gas to be pumped enters the inlet at the top of the piston chamber. The pumping action begins when air is allowed into the lower chamber by the stopcock at C. The air forces the mercury up into the piston chamber and into the inlet and exhaust tubes. Finally, the mercury pushes up the float valves, preventing the mercury from going out the inlet. Once the mercury makes contact with the tungsten wire at D, the circuit with the tungsten wire at F is complete. Then, the stopcock at C is rotated to evacuate the lower portion of the pump. The mercury finally is drawn back into the lower portion of the pump. The float valve at exhaust tube (at B) prevents gas being pumped from re-entering the Toepler pump. As the mercury fills the lower chamber, it fills the small chamber (with tungsten wire at E) which completes the circuit with the tungsten wire at F. This completion activates the stopcock at C to re-admit air into the pump, and the process repeats until it is manually turned off.
The major problem with this type of setup is when the mercury makes (and unmakes) contact with the tungsten wire at D. A spark may form that reacts with the gas being pumped through the exhaust. Mechanisms to by-pass this problem have included either placing the air/vacuum cycling on a timer, thereby bypassing the need of electrical contacts, or placing a photosensitive relay on the side of the exhaust tube, which is activated when the opaque mercury fills the transparent glass tube.
As with most items on a vacuum line that contain mercury, place the Toepler pump in a secondary container that is firmly attached to another surface to contain any mercury that may spill from an accident as well as protect the pump from accidental bumps (see Fig. 7.28). Plastic containers (such as plastic milk cartons) are particularly good because the mercury will not affect plastic. Conversely, mercury may amalgamate with the metals in a metal can, which could destroy any containment capabilities. In addition, it is easier to get mercury out of a plastic container (with smooth walls) than out of a metal one (with a narrow rim). The plastic tub can be glued onto the table with some epoxy. The epoxy will stick better if you roughen up the bottom surface of the plastic container with sandpaper. Because not all epoxies stick to plastic, test the epoxy before assuming that it will hold.
7.4Traps
7.4.1The Purpose and Functions of Traps
Traps (and baffles and filters) are used on vacuum systems because of the need to remove, catch, or bind condensable vapors, paniculate matter, and aerosols. To obtain a vacuum, you must remove everything from a given area. However, like the environmental adage "you cannot throw anything away," you may not want everything that is removed from a vacuum system passed into the pumping sys-
Traps 7.4 |
|
|
|
|
387 |
|
|
|
|
|
Exhaust line |
|
Vacuum line |
Vacuum hose |
7 |
to fume hood |
|
1 |
£ ? |
> |
I |
|
|
I |
I |
|
|
Cold trap
Fig. 7.29 A cold trap is worth the trouble on even a simple vacuum system.
tem, or into the air you breath. Solvents (and their vapors) can impair or severely damage mechanical pumps by dissolving seals or by breaking down mechanical pump oils. Paniculate matter passing into a mechanical pump can severely damage veins and seals. Condensed vapors in pump oil can impair a pump's performance. Volatile compounds that pass through a pump and leave as aerosols can expose technicians to an unacceptable health risk. Thus, the use of traps in vacuum systems can protect equipment and the people who are using the equipment.*
Traps (specifically foreline traps) can also improve the vacuum in a vacuum system either by becoming a separate vacuum station (such as the cryogenic capabilities of a cold trap) or by limiting the backflow of oils from a pump (either a cold trap or a molecular sieve type trap).
Traps can also do more than protect vacuum systems. By placing a series of traps in a line, and by using successively cooler coolants (see Sec. 6.2 for different coolant materials)one can separate compounds by their condensation or freezing points (see Sec. 7.4.5).
The simplest way to protect a pump, pump oil, and pump seals, reduce maintenance time, and protect the worker from the effects of condensable gases in a vacuum system is to place a trap between the vacuum line and pump (see Fig. 7.29). For example, although water vapor is not likely to damage a mechanical pump or worker, it can still impair pump performance by hydrating the pump oil. This problem can be resolved (after the fact) by keeping the pump running for an extended period of time (overnight) against a small dry air (or dry nitrogen) leak. However, this problem can easily (and should) be prevented by trap use at the outset.
As mentioned, a trap prevents condensable vapors from damaging pump components as they are removed from the vacuum system. Additionally, a trap can improve the quality of the vacuum by preventing condensable vapors and pump oil vapors from drifting back into the system. Remember that once a pump has achieved its potential vacuum, gas flow drops to zero leaving materials to drift
Traps are supposed to prevent exhausts from being released into the working environment. However, they should not be relied on to the extent of the possible negligence of the user(s) or other possible accidents causing failure. Therefore,all exhaustsfrom mechanical pumps should be vented to fume hoods (see Fig. 7.14 on exhausting mechanical pumps to fume hoods).
388 Vacuum Systems
upstream or downstream. This means that pump oils and condensable vapors from the mechanical pump can return back to the diffusion pump (if there is one on the system) and into the system itself.
The movement of condensable vapors from the mechanical pump can potentially decrease diffusion pump performance. If your system has diffusion and mechanical pumps, there should be a trap between the two pumps in addition to the cold trap between the system and the diffusion pump (see Fig. 7.30). The use of properly designed and placed cold traps can allow diffusion-pumped vacuum systems to achieve vacuums in the region of 10"9 torr35 and greater!*
7.4.2 Types of Traps
The decision of what type of trap to use is typically more likely made by what one is familiar with, what is available, and/or what is economically viable. For example, you may be inclined to use liquid nitrogen in a situation where dry ice would be adequate if you're in a facility that has a lot of liquid nitrogen available. On the other hand, you might try to get by with dry ice when you don't have access to liquid nitrogen. Alternatively, perhaps there is a situation where a molecular sieve trap would be optimum. If you are not familiar with that type of trap, it is less likely to be used.
There are four basic foreline trap designs (and one post-pump trap):
1.Cold traps that rely on condensation or freezing to trap a condensable vapors.
2.Paniculate traps that physically block the passage of large pieces (>2 microns) of materials from getting into mechanical pump.
3.Molecular sieves primarily used to trap hydrocarbon oils—they also trap water vapor to a limited extent.
4.Coaxial traps that contain various fibrous materials loosely strung within the container to trap (primarily) pump oils. Table 7.10 provides a list of
Diffusion |
|
Mechanical |
I |
|
pump |
||
pump |
|
||
|
(fore pump) |
||
Vacuum |
|
||
|
|
||
line |
|
|
|
|
|
Exhaust to |
|
|
Cold Trap 2 |
Fume Hood |
|
|
|
|
|
Cold Trap 1 |
(Fore Trap) |
|
|
Fig. 7.30 Cold Trap 1 protects the diffusion pump, mechanical pump, and the user from materials that could otherwise drift in from the vacuum line. Cold Trap 2 protects the diffusion pump from any oils that may drift from the mechanical pump.
This vacuum region can only be achieved on special (usually metal) systems that can be baked.
Traps 7.4 |
389 |
the various traps and their effectiveness against various vacuum system contamination.
5.Mist traps limit the amount of the aerosols of mechanical pump oils from leaving the pump and drifting into the room containing the pump. These traps are different from the other traps in that they go on the exhaust of the mechanical pump and do not protect the pump or the system, only the operators.
Cold traps use either water, dry ice slush baths, or liquid nitrogen as a coolant. The low temperatures of a cold trap cause condensable vapors to change their state of matter into a liquid or a solid depending on the temperature and the vapor. As temperature decreases, there is an increase in price and an increase in performance.
Water-based cold traps have limited efficiency, although they are the most costeffective. They can liquefy water vapor and many hydrocarbon solvents, but they can't entrap these materials. Thus, they are capable (and likely) to revaporize back into the system. The cost of running tap water through the cooler and down the sink can be eliminated by running a recirculating pump in a large plastic bucket. The effectiveness can be enhanced by periodically dumping crushed ice into the bucket, but this does take constant maintenance of placing more ice as necessary and removing excess water as necessary (a drain placed on the top can decrease that concern).
Slush baths (see Sec. 6.2.7) are effective for a greater range of vapors and can entrap many vapors by freezing. These types of cold traps require a lot of maintenance.
The most efficient type of cold trap is one that uses liquid nitrogen. This is because it is so cold that once captured, water, hydrocarbon solvents, and most other vapors will not be released into the system. Liquid nitrogen cold traps also enhance pumping within the system due to their cryogenic capabilities. Unfortunately, they are not without problems or complications. Probably the biggest handicap is that they require constant attention to maintain filling levels. Every time the coolant level goes below the level of frozen vapors, the pressure in the system will increase (see Fig. 7.32). Additionally, liquid nitrogen and its equipment are expensive.
Molecular sieve traps (and Micromaze traps from the Kurt J. Lesker Co.) have low maintenance and low long-term costs. Their main advantage is that, once bound, vapors are trapped till they are released by heating their active materials. Thus they do not have the periodic pressure fluctuations that cold traps have. Their main disadvantage is that they require regeneration of the sieve by baking at 150300°C about every 300 hours (or less) of use, and the regeneration requires many hours. The vacuum section must be closed off during the bakeout; otherwise, already-trapped hydrocarbons are dumped right back into the system. Because it is recommended that any valve between the trap and the system be baked as well as the trap,* this whole section cannot be made out of glass. There is no problem
390 Vacuum Systems
with a glass-to-metal connection of some type (except a polymer based o-ring seal) placed a sufficient distance away from the valve and the glass system. One can also have removable cartridges on the trap allowing one to remove the cartridge for regeneration away from the vacuum system. The advantage of this approach is that one sieve can be baked and ready to go, limiting downtime. Otherwise, this type of trap requires a long downtime during the bake-out period; thus this design may not be acceptable to all users. Some molecular sieves allow for easy removal of charging material, whereas others do not. Roepke and Pung devised a simple homemade molecular sieve with a removable charge unit.
Backstreaming can be one of the main limitations for mechanical pumps to achieve a better vacuum. Because molecular sieve and Micromaze traps are so efficient at capturing (and not releasing) vapors, Strattman37 experimented with a Micromaze foreline trap to trap the hydrocarbon oils from a mechanical pump. After proper baking and cooling, he was able to achieve pressures of 10"5 torr consistently with only a mechanical vacuum pump.
Participate traps are simply physical barriers, or screens, that catch particulate matter just as the screens in clothes dryers catch lint. If your processes create particulate matter, it is very important to prevent it from getting into a mechanical pump of any kind. These traps can slow the pumping speed to some degree, but that is a small price to pay to prevent damage to the pump. Only particulate traps can stop particulate matter; no other trap can do so in an effective manner and should not be expected to perform this function.
Coaxial (or assimilation) traps utilize an adsorbing material drawn out to a fine fiber to provide as much surface area as possible. The various different materials available provide varying capabilities. For example, copper provides the best absorption capabilities (particularly to hydrocarbon oils), but is not very durable and needs to be replaced often. Stainless steel (particularly good for acid environments) and bronze will survive better in tougher environments, and activated alumina is great when organics or pump oils need to be trapped. Like molecular sieves, these traps work at room temperature. Unlike molecular sieves, not all can be baked out for regeneration and typically must be replaced with the old one discarded in an environmentally safe manner because it is likely to contain a variety of harmful materials.
Mist traps trap oil aerosols (> 0.3 microns) from the exhaust port of mechanical pumps to minimize exposure to workers in the area. Since they cannot trap gases, vent tubes going to fume hoods are still recommended (see Fig. 7.14).
All traps designs require proper use and maintenance. Mistakes, or improper use, can at a minimum backfill your system with the hydrocarbon oils you are trying to prevent from getting in there to the condensable vapors you are trying to remove. All trap designs should have a valve between the trap and the system to
* The coolness of a nonheated valve will become a condensation point for any hydrocarbons that are baked out of the trap. This forces contamination into a region next to the system that the trap is trying to prevent.