Microweighing in Vacuum and Controlled Environments - 1st Edition - ISBN: 9780444418685, 9780444596468

Microweighing in Vacuum and Controlled Environments, Volume 4

1st Edition

Editors: A.W. Czanderna S.P. Wolsky
Hardcover ISBN: 9780444418685
eBook ISBN: 9780444596468
Imprint: North Holland
Published Date: 1st January 1980
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Table of Contents


Chapter 1. Introduction and Microbalance Review

I. Introduction

II. History

III. Definitions

IV. Classifications of Various Types of Microbalance

A. Introduction: The Ideal Microbalance

B. Types of Instruments

C. Methods of Monitoring Mass Changes

D. Methods for Automatic Sensing of Movement from the Null Point

E. Materials for Microbalance Fabrication

F. Conclusion: The Ultimate Microbalance

V. Calibration Techniques

VI. Auxiliary Equipment for Operation of a Vacuum Microbalance

A. Introduction

B. Vacuum Operation

C. Vibrational Mounts

D. Thermostatic Operation

E. Automatic Operation

F. Manual Operation

G. High Temperature Operation

H. Low Temperature Operation

VII. Undesirable Disturbances or Forces

A. Adsorption and Desorption Effects

B. Temperature Fluctuations

C. Static Charge Forces

D. Convection Currents

E. Buoyancy Forces

F. Radiometric Forces that Result from the Thermomolecular Flow of Gases

G. Water Vapor Effects

VIII. Applications

A. Classic Operation

B. Simultaneous Measurement of Mass and Other Physical Parameters

C. Future

D. Thermogravimetry



Chapter 2. Beam Microbalance Design, Construction and Operation

I. Introduction

II. Some General Theoretical Considerations in Beam Microbalance Design

III. Microbalance Selection Considerations

A. Environmental and Experimental Considerations

B. Advantages and Disadvantages of Various Beam Microbalances

IV. Microbalance Construction

A. Materials Considerations

B. Beam and Suspension Construction

V. Microbalance Operation

A. Deflection Detectors

B. Compensation and Null Techniques

C. Automatic Damping and Nulling Systems

D. System Sensibility or Resolution

E. Microbalance Calibration

VI. Summary


Chapter 3. Sources of Error in Micro Weighing in Controlled Environments

I. Introduction

II. Brownian Motion

A. The Undamped Balance Without Feedback

B. The Critically Damped Balance without Feedback

C. The Automated Balance

III. Knudsen Forces

IV. Cavity Forces

V. Armlength Effect

VI. Radiation Pressure

VII. Gravitational Forces

VIII. Electrostatic Forces

IX. Magnetostatic Forces

X. Building Vibrations


Chapter 4. Physical Adsorption Studies with the Vacuum Microbalance

I. Introduction

II. Instrumentation

A. Sorption Balances

B. Instruments for Pressure Measurement and Control

C. Instruments for Temperature Measurement and Control

D. Determination of the Saturation Vapor Pressure

E. Gravimetric Sorption Measuring Instruments

III. Measuring Techniques

A. Measuring Procedure

B. Pretreatment of the Materials

C. Pretreatment of the Instrument

D. Special Recommendations for the Measurements

E. Reducing the Measuring Time

IV. Examples of Physisorption Measurements and their Evaluation

A. Evaluation of Adsorption Isotherms

B. Determination of Specific Surface Area, Particle Size and Roughness

C. Isotherms of Porous Materials

D. Mesopore Analysis

E. Micropore Analysis

F. Determination of the Isosteric Heat


Chapter 5. Chemisorption Studies with the Vacuum Microbalance

I. Introduction

II. Probing the Surface Phase

III. Quantitative Information from Adsorption and Desorption

A. Adsorption Parameters

B. Isosteric Heat of Adsorption

C. Activation Energy of Adsorption

D. Desorption Kinetics

IV. Experimental

A. Overview

B. Apparatus

C. Technique

V. Chemisorption Results Obtained on Silver Powders

A. The Effectiveness of Outgassing, Oxygen Adsorption, and Chemical Reduction for Cleaning the Surface and Producing Reproducible Chemisorptive Behavior

B. Adsorption and Desorption of Oxygen on Silver

C. Adsorption of Carbon Dioxide on Oxygen Covered Silver

VI. Chemisorption Results Obtained on Other Solids

VII. Concluding Remarks



Chapter 6. Simultaneous Microgravimetric and Residual Gas Analyzer Measurements

I. Introduction

II. Instrumentation

A. Mass Spectrometers

III. Experimental

A. System Design

B. Methods

IV. Applications

A. Review

B. Future Applications



Chapter 7. The Simultaneous Measurement of Mass Change and Infrared Spectra

I. Introduction

II. Experimental

III. Results

IV. Conclusion


Chapter 8. Microgravimetric Studies of Catalysts and Catalytic Processes

I. Introduction

II. Vacuum Microbalances

A. Equipment and Apparatus

B. Assembly and Operation

III. Selected Examples

A. Surface Area Determination: Variation with Pretreatment

B. Surface Area Determination: Mixed Physical and Chemical Adsorption

C. Chemisorption: Rehydration

D. Support Information: Heat of Adsorption from Heat of Wetting

E. Sorption Energetics and Mechanism: Lunar Soils

IV. Areas of Additional Research

V. Conclusions



Chapter 9. High Temperature Reaction Studies

I. Introduction

A. Types of Chemical Reactions

B. Purpose of Chapter

C. Preliminary Thermochemical Analyses

D. Extent of Reaction

E. Units

II. Empirical and Theoretical Rate Laws

A. General

III. Apparatus and Methods

A. Static Reaction Systems

B. Flow Reaction Systems

C. Special Problems

IV. Applications

A. Vapor Pressure of Silicon

B. Oxidation of Graphite Using the Static Reaction System

C. Oxidation of Graphite Using the Flow Reaction System

D. Oxidation of Molybdenum-Static Reaction System

E. Oxidation of Tungsten

V. General Comments

VI. Appendix 1: Theory of Surface Interface Reactions with no Oxides Present

A. Processes

B. Kinetic Theory

C. Absolute Reaction Rate Theory

VII. Appendix 2: Furnaces for Temperatures Up to 1650°C

A. Mechanical and Physical Properties of Molybdenum Disilicide Elements

B. Electrical Supply Equipment

C. Useful Life

D. Atmospheric Effects

E. Furnace Design: Refractories

VIII. Appendix 3: Furnace Tubes and Reaction Systems

A. Criteria of Furnace Tube Performance

B. Types of Furnace Tubes

C. Specimen Supporting Wires


Chapter 10. Unusual Applications of the Vacuum Microbalance

I. Introduction

II. Permeation of Water Vapor through Plastic Membranes

A. Theory of Permeation

B. Measurement of Permeation

III. Measurement of Dust Concentration

A. The Basic Concept of the Dust Balance

B. Combination of Electrostatic Precipitation and Electromagnetic Weighing

C. Mass Determination by Vibrations of a Very Thin Band

IV. Determination of Grain Size Distributions by Weighing

A. Theory of Sedimentation Analysis

B. Grain Size Distribution by Sedimentation in Liquids

C. Grain Size Distribution by Sedimentation in Air

D. Grain Size Distribution by Sedimentation in Partial Vacuum

E. General Considerations

V. Measurement of Surface Tension

A. Basic Facts

B. Measurement of Surface Tension with the Aid of Wire Loops and Rings

C. Measurement of Surface Tension with the Aid of an Immersed Solid Plate

D. Measurement of Surface Tension with the Aid of a Cylinder or of a Solid Plate Touching the Surface

E. Adaptation of the Vacuum Microbalance to Measurement of Surface Tension

VI. Measurement of Permittivity and Dielectric Loss Factor

A. Theory of Electrostatic Forces on Dielectric Bodies

B. Measurement of Dielectric Permittivity

C. Measurement of the Dielectric Loss Factor

VII. Precision Measurement of Pressure Using the Principle of Automatic Compensation

A. Objective of the Development

B. A Self Compensating Bodenstein Manometer

VIII. Simultaneous Measurement of Components of Force and Combinations of Force and Torque

A. Measurement of Lift and Drag in a Gas Stream by a Two Component Microbalance

B. Simultaneous Determination of Mass Flow and Reaction Force of a Vapor Stream from a Heated Sample

C. Simultaneous Measurement of Weight and Torque by Magnetic Suspension

IX. Conclusion




Methods and Phenomena, 4: Their Applications in Science and Technology: Microweighing in Vacuum and Controlled Environments focuses on the principles, methodologies, and approaches involved in micro mass measurements.

The selection first elaborates on introduction and microbalance review, beam microbalance design, construction and operation, and sources of error in microweighing in controlled environments. Discussions focus on Brownian motion, Knudsen forces, gravitational forces, microbalance construction and operation, auxiliary equipment for operation of a vacuum microbalance, undesirable disturbances or forces, calibration techniques, and classification of various types of microbalances.

The text then takes a look at physical adsorption studies and chemisorption studies with the vacuum microbalance, simultaneous microgravimetric and residual gas analyzer measurements, and simultaneous measurement of mass change and infrared spectra. Topics include chemisorption results obtained on other solids and silver powders, probing the surface phase, quantitative information from adsorption and desorption, measuring techniques, and examples of physisorption measurements and their evaluation. The manuscript examines unusual applications of the vacuum microbalance and high temperature reaction studies, as well as empirical and theoretical rate laws, permeation of water vapor through plastic membranes, and measurement of permittivity and dielectric loss factor.

The selection is a valuable source of data for researchers wanting to explore microweighing in vacuum and controlled environments.


© North Holland 1980
North Holland
eBook ISBN:


@qu:This compendium of discussions of the application of the beam microbalance is a valuable source of information for all who wish to apply these techniques to current and future problems. Excellent reviews of many aspects of microweighing are presented by internationally renowned authorities in the areas of theoretical analyses, design, fabrication, and application... an excellent volume which should be considered required reading for analysts and physical scientists... @source:Journal of Colloid & Interface Science

About the Editors

A.W. Czanderna Editor

S.P. Wolsky Editor

Affiliations and Expertise

1900 Cocoanut Road, Boca Raton, Florida, FL 33432, USA