- •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
Joints, Stopcocks, and
Glass Tubing
3.1 Joints and Connections
The ability to assemble and disassemble apparatus components has been a longstanding requirement in laboratories. Theuse of ground joints for this purpose is not new, butstandardizing thetaper sothat onepiece from onelabcanbe attached to another section of apparatus in another lab hasonly been in common use since just after World WarII. Currently, there are many standardized ways to join and separate laboratory glass apparatus.
3.1.1 Standard Taper Joints
Standard Taper Ground Joints. These joints have thesame taper throughout the world. This taper, a 1:10 ratio, provides for the ground section to decrease in size
These male joints show thetwoareas that are measured and which thereby identify any Standard Taper " s " joint. These pairs of numbers arealways given in X,Y coordinates. Thefirst number (X) is the widest part of theground area. Thesecond number (Y) is thevertical length of the ground section.
nid
Mid-length joints differ from full-length joints only in their "Y"dimension. It is asif the short endhadbeen cut off. The example to the left shows a regular and mid-length joint.
Fig. 3.1 Full- andmid-length standard taper joints.
173
174 |
|
|
Joints, Stopcocks, and Glass Tubing |
(a) |
(b) |
(c) |
(d) |
Fig. 3.2 Various types of inner joints.
one unit in width for every 10 units of length. These units are always in "mm" (see Fig. 3.1).
Standard taper joints are used in matching inner and outer (also called male and female) members. They are made in a variety of standardized sizes and shapes. Figures 3.2 and 3.3 illustrate the shape variations available. In general, how a joint will be used determines which joint design should be selected.
Inner Joints. Common varieties of inner joints are shown in Fig. 3.2. Figure 3.2(a) is a standard full-length joint, the one most commonly seen in the lab. Figure 3.2(b) has a small "drip tip" extended from the small end of the joint. This joint is commonly placed on condensers to prevent distillate from coming in contact with, and/or dissolving, stopcock grease. Figure 3.2(c) has an extended drip tip that a glassblower can bend to aim the liquid flow, or seal to other pieces of glass. The manufacturer adds these extensions during initial fabrication, before the joint is ground to the proper taper. If a glassblower were to try to seal such an extension onto a Type (a) joint, the distortion caused by the sealing action would alter the taper of the joint, necessitating regrinding. Manufacturers also provide joints that already have hooks for springs on them, as in (d).
Outer Joints. These joint also have a variety of forms (see Fig. 3.3). Both (a) examples have heavy walls and can receive a moderate amount of physical abuse. Example (b) has thinner walls on the ground joint section. Ribs are placed around the joint for extra strength. Thin walls are important for experiments with large
u
(a) (b) (c) (d) Fig. 3.3 Various types of outer joints.
Joints and Connections 3.1 |
175 |
The "old" style female joint is very good to use with two-finger clamps. It is not neccessary to squeeze the wing nut tightly to securely hold the joint. Rather, the bulb of the joint rests easily on the clamp.
Fig. 3.4 Old style outer joint in a two-finger clamp.
temperature fluctuations that, in turn, might cause glass expansion or contraction. Changes in glass size could cause separation of the inner and outer joints, thus causing leaks. Example (c) is often referred to as an "old style" joint. It can easily be identified by the small bulb just below the ground section. This bulb provides a resting place for the joint on a two-finger clamp without requiring extra pressure (see Fig. 3.4). The squeezing of a column to maintain position (when there is no bulb to support the weight) is the exclusive cause of cracks on the sides of columns. If the joint is not held vertically, the bulb can also cause a minor hold-up of fluids. Example (d) shows outer joints with preattached hooks.
Standard taper joints are formed by a process called "tooling," which establishes the physical form from a simple glass tube. After the joint is made, it is ground using various grades of carborundum grinding compounds to achieve the proper tapered smooth finish. In addition to the standard ground surface joint, Wheaton Scientific Co. also makes a joint with a smooth polished glass surface. These joints are known as Clear-Seal® joints. Instead of being ground, the joint is heated until soft and then suctioned over a mandrel. The suctioning causes the glass to collapse onto and conform to the mandrel shape.
Pool of
mercury
(a) |
(b) |
Outer mercury joint |
Inner mercury joint |
Fig. 3.5 Examples of mercury joint seals.
176 Joints, Stopcocks, and Glass Tubing
Table 3.1 Comparison of ASTM Midand Full-Length
Joint Size to European Joint Size
ASTM |
ASTM |
European Size |
|
Standard Mid- |
Standard Full |
||
Joint |
|||
length |
Length |
||
|
|||
Width/Length |
Width/Length |
Width/Length |
|
7/15 |
7/25 |
7/16 |
|
10/18 |
10/30 |
10/19 |
|
12/18 |
12/30 |
12/21 |
|
14/20 |
14/35 |
14/23 |
|
19/22 |
19/38 |
19/26 |
|
24/25 |
24/40 |
24/29 |
|
29/42 |
29/26 |
29/32 |
|
34/28 |
34/45 |
34/35 |
|
40/35 |
40/50 |
40/38 |
|
|
45/50 |
45/40 |
|
|
50/50 |
50/42 |
|
|
55/50 |
55/44 |
|
|
60/50 |
60/46 |
Wheaton Clear-Seal joints have the unique attribute that they do not need any stopcock grease. However, they require very special handling and storage, because any scratch can destroy their sealing abilities. Additionally, when joint members are joined, special care must be taken to ensure that no paniculate matter lodges between the pieces. Such matter can prevent a proper seal, scratch the sides of the members, and/or cause the members to jam or stick. Because no stopcock grease is used with Clear-Seal joints, it is more difficult to separate stuck members.
Clear-Seal joints are mandatory when using diazomethane (CH2N2) as a methylating reagent for carboxylic acids. Diazomethane is a toxic, irritating gas which has the tendency to self-detonate. This self-detonation can occur when the diazomethane is in either a gaseous or liquid state. It has been proven1 that rough surfaces (such as ground joint surfaces) can initiate such detonations. Thus, only Clear-Seal joints should be used in diazomethane chemistry.
Mercury Seal Joint. This joints is no longer used for its intended purpose because of improvements in joint manufacturing as well as safety concerns about mercury in the lab. The mercury seal joint (see Fig. 3.5) was originally used to provide leak-tight seals so that gases couldn't pass by ground joint seals. After the ground glass joints were in place, a small pool of mercury was poured in the trap to complete the seal.
The outer mercury joint is still commonly used by glassblowers who need to seal tubing onto the ground end of an outer joint (for example, on a water-cooled
Joints and Connections 3.1 |
177 |
Fig. 3.6 Sample of a water-cooled condenser using a mercury seal joint.
condenser where the joint also needs to be water cooled, as in Fig. 3.6). Without the extension of glass, a seal of this type would distort the walls of the joint, making it useless. This outer joint, therefore, provides the same advantage afforded by extended drip tip inner joints (Fig. 3.2(c)).
European Joint Sizes. In Europe a different set of joint lengths are used than what are common in North and South America. The European joints are just a bit longer than the ASTM standardized midlength joints found in North America. See Table 3.1 to see how these joints match up with standard and midlength joints.
Normally, laboratories in the America are not likely to encounter European joints. However, it is possible to encounter a Standard Taper Joint that is neither full nor midlength if one is doing joint research with European labs, or when obtaining laboratory apparatus from European companies.
Because the taper (1:10) and the width are the same, it is easy to insert and use European joints in any ASTM Standard Taper Joint. However, the European joint will extend just beyond the midlength joint, and the full-length joint will extend just beyond the European joint. Because of this mismatch, there is a greater chance for stopcock grease to be exposed to materials within the containers. This can be resolved by either being more judicial when applying the stopcock grease (don't overdo it), using a Teflon sleeve, or changing one or the other joints to
Stoppers (solid or hollow) are all measured on the width of the ground section (X). This measurement (in mm) is the size (number) of the stopper. The length is consistent for any given width.
Fig. 3.7 Stopper plugs.