
- •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
208 |
Joints, Stopcocks, and Glass Tubing |
Tap the outer member with a sharp light blow at a glancing angle.
Fig. 3.35 Lightly tapping stuck (ungreased) joint or stopcock members with wood can sometimes separate the pieces.
very difficult. Trying to grab onto remaining glass with a pair of pliers often is futile as the glass breaks and chips off. If there is access to the opposite end, it may be possible to tap, or push, the piece out. Alternatively, if the plug or joint is hollow and is closed like a cup, it may be possible to pour melted lead or melted electrical solder into the item like a screwdriver tip. Then when the melted metal hardens, you have a good handle with which to remove the remaining portion of the plug. The solder may then be removed and reused.7
WARNING: Although the materials used in these unsticking techniques are, for the most part, inert or nonreactive, practice safe chemistry. If you have a chemical (that is trapped by a stuck stopcock or joint) that may react with one of the materials or solutions mentioned in this subsection, select a different approach.
3.3.8 Leaking Stopcocks and Joints
There are three reasons that a joint or stopcock might leak: Either the item is not being used in the conditions, or manner, for which it was designed, the stopcock or joint is worn, or the item was poorly manufactured. Although extra grease may be used for short-term emergency situations, it is not a solution because extra grease is not fixing the problem. Similarly, adding extra stopcock grease to a regular stopcock will neither make it act like a high-vacuum stopcock nor help a defective stopcock or joint.
Surprisingly, many assumed defects of a joint or stopcock are caused by using an item improperly. By trying to "make do" with what you have, you either may jeopardize the quality of your work or may subject yourself and others around you to potential dangers. Thus, adding extra grease onto a standard stopcock to that it can be used for vacuum work will be a losing battle.
Assuming that the joint or stopcock selected is proper for the application and there is evidence of leakage, you should look for potential human errors:
1.Did you apply the stopcock grease properly, or is the current grease old?
2.Did you properly clean the items before assembly? Paniculate matter
left in a joint or stopcock can not only cause a leak, but can also cause the stopcock to jam.
3. Are the pieces of a Teflon stopcock assembled in the correct order? For example, on a Teflon stopcock, if the black O-ring is placed next to
Maintenance and Care of Joints, Stopcocks, and Glassware 3.3 |
209 |
the stopcock barrel, counterclockwise rotation may cause the plug to loosen.
4. If you have a vacuum system with glass stopcocks, do the numbers on the plugs and barrels match (see Sec. 3.3.1 and Fig. 3.30)?
Even if failure to prevent the above errors has not caused a leak outright, prolonged misuse eventually causes wear on a joint or stopcock, which can then cause permanent damage. Not all defects caused by wear can be distinguished from manufacturing defects by appearance alone. However, if a new item leaks from structural defects, it probably is a manufacturing imperfection.
Although the quality of joint and stopcock construction from the glass manufacturing industry is generally excellent, mistakes do happen. It is possible to have received hundreds, or thousands, of excellent joints and stopcocks from the same manufacturer, plus one that leaks. Fortunately, manufacturers will promptly replace defective materials.
The Rock or Jiggle Test. It is possible for a joint or stopcock to be so badly made that a mated pair can rock, or jiggle, when a little lateral motion is applied. This test should be done without any stopcock grease on the pair to prevent artificial damping of the motion. Do not force or twist any joint without grease as it is likely to jam. The biggest problem with this test is that it is impossible to know which of the pair is the bad one. To use a pair with this problem will only make both pieces bad as the bad one will wear the good one unevenly, thus making it unusable.
The Pencil Test. Before performing the pencil test, completely clean the entire apparatus in question. Remove all traces of any oil or grease (if the grease is hydrocarbon-based, you can heat the glass item in an oven to approximately 400°C to burn off any remaining grease). Next, take a standard no. 2 pencil and scribble a line all over the inside surface of the outer piece and the outside surface of the inner piece, as shown at the left of Fig. 3.36. Then, wet the joint (or stopcock) members with water (for lubrication) and rotate back and forth five to ten times (do not bear down, let the water be a lubricant). If the ground sections of both faces of the joint (or stopcock) are perfectly flat, the pencil will have been
Before grind. |
After grind. |
Fig. 3.36 Sample of using the pencil test to examine the quality of a joint.
210 |
Joints, Stopcocks, and Glass Tubing |
removed while the two faces ground against each other. If there are any depressions or raised areas on either surface, pencil lines will remain or be selectively ground away as seen at the right of Fig. 3.36.
This technique works well with both regular stopcocks and joints, but the surfaces on vacuum stopcocks are ground so smooth that they are unable to grind off the pencil. However, by adding a very small amount of an optical finishing powder (i.e., aluminum oxide #50) you will be adding sufficient roughness without doing any damage to the stopcock. If there is too much of the optical finishing compound, the slurry will grind all the pencil off regardless of the quality of the stopcock. Use plenty of water for lubrication; a joint that becomes stuck with grinding compound is almost impossible to separate. Once you have finished using the grinding compound, be sure to thoroughly rinse it out. Grinding compound left on a joint or stopcock is likely to destroy the item over time.
As previously mentioned, it is important that all oil and grease be removed before trying the pencil test. This point becomes even more critical if any optical finishing compound or grinding compound is used because it is likely to stick to any remaining oil or grease. If the stopcock is used with any particulate matter mixed in with the grease, it will grind into the glass and destroy the stopcock or joint.
The Merthiolate or Prussian Blue Test. The pencil test will not work on a Teflon stopcock because there is no rough surface with which to rub a pencil mark off. Grinding compound cannot be used because it will destroy the surface of the Teflon, thus destroying the plug. Rather than using a rough material to grind off a pencil line, this test uses either Prussian Blue or Merthiolate to collect in the depressed surface of the member. The item is cleaned as before, but this time several drops of Prussian Blue or Merthiolate are placed on the inner piece before assembly with the outer member. As seen in Fig. 3.37, any dark spots signify a thicker film of the indicating solution, which implies a concave impression on one or the other piece. A perfect joint shows clear with no dark areas. This test can
Depression
Fig. 3.37 Sample of using the Prussian Blue (or Merthiolate) test to examine the quality of a joint.
Maintenance and Care of Joints, Stopcocks, and Glassware 3.3 |
211 |
also be used on glass stopcocks or joints. By rotating the two pieces you can note with which member the dark spot travels. If you hold the outer piece still, rotate the inner piece, and the spot travels, you know the depression is on the inner piece. Similar logic is used to identify depressions on the nonrotated piece.
3.3.9 What to Do About Leaks in Stopcocks and Joints
Unfortunately, there are not many options available when you have a defective stopcock or joint. The best solution is to replace the defective part of the apparatus, or the entire apparatus if necessary. If the item is new, return it to your supplier and have it replaced.
If the defective part is the plug of a Teflon stopcock, you can try to simply replace the plug. If the plug was damaged by abrasion (or other abuse), replacement offers a simple resolution. The possibility that a distorted Teflon plug is causing a leak is very unlikely. If the glass barrel of a Teflon stopcock is distorted (showing the problems seen in Fig. 3.37), you have no recourse but replacement.
If the item is all glass, it may be reground. However, do not regrind a glass stopcock if:
1.You have any other recourse (see Point 5).
2.You are not experienced in grinding stopcocks or joints.
3.You are unable to completely remove all traces of oil or grease from the item. Any oil or grease will retain grinding compound onto the part, and subsequent use of the item with the grinding compound on it will cause it to jam or wear unevenly, leaving you back where you started. The best technique for removing organic greases is to burn them off in a high-heat oven.
4.If the item is a stopcock and the overlap of the holes on the plug and barrel are such that any grinding will close the hole passageway (see Fig. 3.17).
5.You can accept that the piece in question is expendable.
Grinding should be done with 120-grit Carborundum and plenty of available water. Adding a little dishwater soap will help lubricate of the pieces as they are ground.
After removing all grease, wet both glass members with water and place a small bit of grinding compound on one of the members. Insert the inner member into the outer member and, while applying a light amount of pressure, rotate the members around and around, not back and forth (this point is very important because back and forth rotation with grinding compound will cause uneven wear). Remember, incomplete rotation will mean that you are making a depression in only one region