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Compendium of Thermophysical Property Measurement Methods Volume 2 Reeommended Measurement Teehniques and Practiees

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Page 1: Compendium of Thermophysical Property Measurement Methods978-1-4615-3286-6/1.pdf · Therll10physical Property MeasureITIent Methods Volume 2 Recommended Measurement Techniques and

Compendium of Thermophysical Property Measurement Methods

Volume 2

Reeommended Measurement Teehniques and Practiees

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COITIpendiull1 of Therll10physical Property MeasureITIent Methods Volume 2

Recommended Measurement Techniques and Practices

Edited by

K. D. Maglic Boris Kidric Institute of Nuclear Sciences Belgrade, Yugoslavia

A. Cezairliyan National Institute of Standards and Technology Gaithersburg, Maryland, USA

and

V. E. Peletsky Institute for High Temperatures Moscow, Russian Federation

Springer Science+Business Media, LLC

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Library of Congress Cataloging in Publicat ion Data

(Revised for voI. 2) Compendium of thermophysical property measurement methods: recommended mea­surement techniques and practices

Includes bibliographical references and indexes. Contents: v. 1. Survey of measurement techniques-v. 2. Recommended measurement

techniques and practices. 1. Solids - Thermal properties - Measurement - Handbooks, manuals, etc. 1. Maglic,

K. D. (Kosta D.) II. Cezairliyan, A. III. Peletsky, V. E. QCI76.8.T4C66 1984 530.4'12 84-3268 ISBN 978-1-4613-6445-0 ISBN 978-1-4615-3286-6 (eBook) DOI 10.1007/978-1-4615-3286-6 . .

ISBN 978-1-4613-6445-0

© 1992 Springer Science+Business Media New York Originally published by Plenum Press, New York in 1992 Softcover reprint of the hardcover 1 st edition 1992

All rights reserved

No part of this book may be reproduced, stored in a retrieval system, or transmitted in any form or by any means, electronic, mechanical, photocopying, microfilming, recording, or otherwise, without written permission from the Publisher

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Contributors

PIERRE ABELARO, Ecole Nationale Superieure de Ceramiques Industrielles, Limoges Cedex, France

BERNARD CALES, Ceramiques Techniques Desmarquest, Evreux Cedex, France

ARE D CEZAIRLIYAN, Thermophysics Division, National Institute of Stan­dards and Technology, Gaithersburg, Maryland, USA

VITALlY YA. CHEKHOVSKOI, Institute for High Temperatures, USSR Academy of Sciences, Moscow, USSR

J.W. COOKE, Energy Programs Division, Oak Ridge Field Offiee, Department of Energy, Oak Ridge, Tennessee

JOHN M. CORSAN, Division of Quantum Metrology, National Physical Laboratory, Teddington, Middlesex, England

W.R DAVIS, 28 Joseph Crescent, Alsager, Stoke-on-Trent, England RUDOLF DE CONINCK, Materials Science Department, SCKjCEN, Mol,

Belgium FRANCESCO DE PONTE, Istituto di Fisica Teenica, Universita di Padova,

Padova, Italy DAVID A. DITMARS, National Institute of Standards and Technology,

Gaithersburg, Maryland, USA DANIEL R FLYNN, National Institute of Standards and Technology,

Gaithersburg, Maryland, USA RK. KIRBY, Retired from National Institute of Standards and Technology,

Gaithersburg, Maryland, USA SORIN KLARSFELD, Saint-Gobain Recherche, Aubervilliers, France Y A.A. KRAFTMAKHER, Institute of Inorganic Chemistry, USSR Academy

of Sciences, Novosibirsk, USSR S.N. KRA VCHUN, Physics Department, Moscow State University, Moscow,

USSR CATHERINE LANGLAIS, Isover Saint-Gobain, Centre de Recherches I~dus­

trielles, Rantigny, France K.D. MAGLIC, Boris Kidric Institute of Nuclear Sciences, Institute ofThermal

Engineering and Energy Research, Belgrade, Yugoslavia

v

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vi CONTRIBUTORS

A.G. MOZGOVOI, Institute for High Temperatures, USSR Academy of Sciences, Moscow, USSR

V.E. PELETSKY, Institute for High Temperatures, USSR Academy of Sciences, Moscow, USSR

L.P. PHYLIPPOV, Physics Department, Moscow State University, Moscow, USSR

E.S. PLATUNOV, Physics Department, Leningrad Technological Institute of the Refrigerating Industry, Leningrad, USSR

MICHAEL J. RICHARDSON, Division of Materials Metrology, National Physical Laboratory, Teddington, Middlesex, England

G. RUFFINO, Mechanieal Engineering Department, Second University of Rome Tor Vergata, Rome, Italy

E.E. SHPIL'RAIN, Institute for High Temperatures, USSR Academy of Sciences, Moscow, USSR

RA YM 0 ND E. TA YLO R, Thermophysical Properties Research Laboratory, Purdue University, West Lafayette, Indiana, USA

A.S. TLEUBAEV, Physics Department, Moscow State University, Moscow, USSR

RONALD P. TYE, Consultant, Sinku Riko Inc., Cohasset, Massachusetts, USA ALFRED E. WECHSLER, Arthur D. Little, Inc., Cambridge, Massachusetts,

USA K.A. Y AKIMOVICH, Institute for High Temperatures, USSR Academy of

Sciences, Moscow, USSR

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Preface

The two-volume reference work Compendium of Thermophysical Property Measurement Methods was intended to systematize and record the knowledge accumulated in the past, especially du ring the last three decades of intensive studies of thermophysical property me asu rem ent methods, and to serve as a guide in selecting the best technique to be employed in measuring the required property of a material. The first volume, Survey of Measurement Techniques, published in 1984, provided an exhaustive compilation of the currently used methods for the measurement of thermal and electrical conductivity, thermal diffusivity, specific heat, thermal expansion, and thermal radiative properties of solid materials, from room temperature to very high temperatures. The first volume also served as the basis for the second phase of the work, namely, the description of recommended practice s for the determination of transport and thermodynamic properties of selected groups of materials.

This second volume, Recommended Measurement Techniques and Prac­tiees, presents the results of work in the second phase, with detailed coverage of selected recommended techniques and relevant information. Contributing authors were selected to represent various measurement methods developed and used in different parts of the world, keeping in mind that only techniques which have reached a mature state of development should be ineluded in the first place. Contributions in this volume inelude information at a sufficient level of detail to permit potential users of the method to be guided in the construction of the equipment and its subsequent use. Particular attention was paid to the fundamental aspect ofthe measurements, Le., the mismatch between the physical model and the actual measurement conditions, which is usually the principal source of error in thermophysical experiments.

The intention in composing this second volume was to record all significant aspects of thermophysical property measurements resulting from many years of dedicated studies and a high degree of specialization. There is little doubt that the experimental methods will continue to be developed particularly in the areas related to data acquisition and their computerized processing. The area related to the physics of the measurements and the sources of error arising from the deviations of real measurement conditions from those considered for

vii

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viii PREFACE

the modeis are very actual, gaining importanee with automation of the measure­ment processes. The increasing availability and use of automated apparatus enhance the importanee of such a source book in assessing the nature and magnitude of errors resulting from the measurements and computational techniques.

The main portions of the chapters in this volume refer to a description of the individual apparatus and measurement procedures, written by authors who have designed and developed such instruments. While most of the apparatus described is for measuring solid materials, a few methods for molten metals or ftuids have also been included to bridge the gap between measurement techniques us ed for the two aggregate states of matter. Two chapters have been devoted to an assessment of the state-of-the-art in electrical resistivity and thermaI expansion measurements. The last chapter summarizes thermo­physical property reference materials, being an update of the list provided in the first volume of the Compendium.

The present volume is composed of six major sections, with twenty two chapters in all. The first section presents eight chapters on methods for measuring thermaI conductivity: the methods for metaIs, from room to very high temperatures, for loose fill, insulating, building and refractory material s, and a method appropriate for ftuids. The second section is devoted to a review of methods for measuring electrical resistivity, applicable to medium and good conductors. The third section covers three methods for measuring thermaI diffusivity of solid materials: the laser pulse technique, the modulated electron beam and thermaI radiation method, and a group of methods for measuring both thermaI diffusivity and thermaI conductivity in the monotonic heating regime. The last chapter within this section deals with a method for measuring several properties of liquids and compressed gases. The fourth section contains five chapters describing equipment and measurement procedures for measuring specific heat; they include the method of mixtures, and its high-temperature variant, levitation calorimetry, modulation calorimetry, the subsecond pulse heating calorimetry, as well as instructions for the use of differential seanning calorimetry in specific heat measurements. The fifth section contains three chapters dealing with methods for the measurement of thermaI expansion. The first is an overview of approaches for measuring thermaI expansion. The other two describe an apparatus for interferometric measurement of thermaI expansion of solids and an apparatus for the continuous measurement of thermaI expansion and density of materials in the condensed phase at high temperatures and pressures. The sixth section contains an updated list of certified thermophysical property standard reference materials.

K.D. Magiit A. Cezairliyan

v.E. Peletsky

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Acknowledgments

The editors are indebted to many people who helped in the preparation of this book. Special thanks, however, must go to the individuals who contributed most, the authors of chapters.

In addition, thanks must be also extended to the referees of individual chapters, whose reviews contributed to the final form and quality of the manuscripts in this book. These are, in the order of appearance of particular chapters in the main section of the book:

For the section on thermaI conductivity:

R.P. Tye, Holometrix, Inc. Cambridge, Massachusetts, USA (two chapters)

J .P. Moore, Martin Marietta Energy Systems, Oak Ridge, Tennessee, USA W. Neumann, Austrian Research Centre, Seibersdorf, Austria M.L. Laubitz, National Research Couneil, Ottawa, Canada D.R. Smith, National Institute of Standards and Technology, Boulder,

Colorado, USA A.E. Wechsler, Arthur D. Little, Inc., Cambridge, Massachusetts, USA D.L. McElroy, Oak Ridge National Laboratory, Oak Ridge, Tennessee,

USA

For the section on electrical resistivity:

F. Cabannes, Centre de Recherches sur la Physique des Hautes Tem­peratures, Orleans, France

For the section on thermaI diffusivity:

R.V. Acton, Sandia National Laboratories, Albuquerque, New Mexico, USA

V.E. Zinov'ev, Mining Institute, Ura/' s Polytechnical Institute, Sverdlovsk, USSR

K.D. Maglic, Boris Kidric Institute, Vinca, Belgrade, Yugoslavia S.e. Saxena, University of Illinois at Chicago Circ/e, Chicago, Illinois,

USA

ix

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x ACKNOWLEDGMENTS

For the section on specific heat:

E. Hanitzsch, Physikalisch-Technische Bundesanstalt, Braunschweig, Germany

V.Ya. Chekhovskoi, Institute for High Temperatures, Moscow, USSR J.L. Margrave, Rice University, Houston, Texas, USA F. Righini, Istituto di Metrologia "0. Colonnetti," Turin, Italy R.E. Taylor, Thermophysical Properties Research Laboratory, West

Lafayette, Indiana, USA

For the section on thermal expansion:

G. Ruffino, Second University of Rome, Rome, Italy T.A. Hahn, Naval Researt;:h Laboratory, Washington, D.C., USA R. Ohse, European Institute for Transuranium Elements, Karlsruhe,

Germany

For the section on standard referenee materials:

L.L. Sparks, National Institute of Standards and Technology, Boulder, Colorado, USA

The editors wish to express grateful appreciation to referees: T.A. Hahn and J.L. Margrave for voluntary leetorial editing of the refereed manuseripts of non-English origin.

Thanks are extended to all organization s represented by the authors and referees throughout the world. The eontributions of the U.S.-Yugoslav Joint Board for Seientifie and Teehnologieal Cooperation and the Soviet Organizing Committee for International Thermophysical Properties Conferenees to the eoordination of work on this volume are also gratefully aeknowledged.

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Contents

I. THERMAL CONDUCTIVITY

CHAPTER 1. AXIAL HEAT FLOW METHODS OF THERMAL CONDUCTIVITY MEASUREMENT FOR GOOD CONDUCTING MATERIALS J.M. Corsan

1. Introduction ................................................ 3 2. GeneraI-Purpose Apparatus . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . . . . 4 3. Low-Temperature Apparatus .. ........ .. .. .... . . . . . . .. . . . . . . . . 16 4. Long-Bar Apparatus ......................................... 20 5. Deterrnination of TherrnaI Conductivity from EIectricaI Resistivity 27 References .................................................... 30

CHAPTER 2. THERMAL CONDUCTIVITY OF LOOSE-FILL MATERIALS BY A RADIAL-HEAT-FLOW METHOD Daniel R. Flynn

1. Introduction ................................................ 33 2. Method and MathematicaI Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36 3. ThermaI Conductivity Apparatus (1963) ........................ 39 4. Improved LongitudinaI-Heat-Flow Correction . . . . . . . . . . . . . . . . . . . 48 5. ThermaI Conductance Apparatus (1969) . . . . . . . . . . . . . . . . . . . . . . . . 52 6. Recommendations for Future Designs . . . . . . . . . . . . . . . . . . . . . . . . . . 63 References .................................................... 74

CHAPTER 3. THE MEASUREMENT OF THERMAL CONDUCTIVITY BY THE COMPARATIVE METHOD Ronald P. Tye

1. Introduction ................................................ 77 2. TerminoIogy ................................................ 79 3. Apparatus .................................................. 80

xi

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xii CONTENTS

4. Procedure................................................... 91 5. Calculation ................................................. 92 6. Calibration and Verification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93 7. Preeision and Bias . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94 Notation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95 References .................................................... 96

CHAPTER 4. REFERENCE GUARDED HOT PLATE APPARATUS FOR THE DETERMINATION OF STEADY-STATE THERMAL TRANSMISSION PROPERTIES Franceseo De Ponte, Catherine Langlais, and Sorin Klarsfeld

1. Introduction ................................................ 99 2. Choice of Technical Characteristics and Performance Specifications 100 3. Apparatus Description. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 101 4. Apparatus Design. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 103 5. Measurement Results and Performance Check . . . . . . . . . . . . . . . . . .. 115 6. Conclusions................................................. 121 Appendix A . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 122 Appendix B ................................................... 124 Appendix C ................................................... 124 References .................................................... 131

CHAPTER 5. APPARATUS FOR TESTING HIGH-TEMPERATURE THERMAL-CONDUCTIVITY STANDARD REFERENCE MATERIALS WITH CONDUCTIVITIES ABOVE 1 Wm- I K- 1 IN THE TEMPERATURE RANGE 400 TO 2500 K V,E. Peletsky

1. Introduction ................................................ 133 2. Schematic Outline of the Method and the Basic Mathematical Model 134 3. Experimental Setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 139 4. Pre-Starting and Measurement Procedures ...................... 149 5. Processing of Experimental Results and Error Evaluation . . . . . . . .. 152 6. Functional Potentialities and Limitations of the Apparatus . . . . . . .. 156 7. Examples of Application... . .. . . . . . . . . . . . . . . . . . . . . . .. . . . .... .. 157 References .................................................... 159

CHAPTER 6. THE PROBE METHOD FOR MEASUREMENT OF THERMAL CONDUCTIVITY Alfred E. Wechsler

1. Introduction ................................................ 161 2. Measurement Theory and Analyses ............................ 162

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CONTENTS xiii

3. Description of Apparatus and Instrumentation. . . . . . . . . . . . . . . . . .. 170 4. Measurement Methods ....................................... 178 5. Practical Considerations in the Use of the Probe and Line Heat

Source Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 182 Notation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 184 References .................................................... 184

CHAPTER 7. B.S.1902 PANEL TEST METHOD FOR THE MEASUREMENT OF THE THERMAL CONDUCTIVITY OF REFRACTORY MATERIALS WR. Davis

1. General Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 187 2. General OutIine of the Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 191 3. Error Analysis. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 196 Notation ...................................................... ·200 References .................................................... 200

CHAPTER 8. THE V ARIABLE-GAP TECHNIQUE FOR MEASURING THERMAL CONDUCTIVITY OF FLUID SPECIMENS J. W Cooke

1. Introduction ................................................ 201 2. Principle of Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 201 3. Experimental Apparatus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 214 4. Experimental Procedures ..................................... 223 5. Experimental Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 225 6. Discussion of the Results .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 230 7. Conelusions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 234 References

II. ELECTRICAL RESISTIVITY

CHAPTER 9. METHODS FOR ELECTRICAL RESISTIVITY MEASUREMENT APPLICABLE TO MEDIUM AND GOOD ELECTRICAL CONDUCTORS B. Cales and P. Abelard

234

1. Introduction ................................................ 239 2. Direct-Current Measurements of Total Conductivity . . . . . . . . . . . . .. 240 3. Alternating-Current Measurements . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 254 4. Measurements of Parti al Conductivities . . . . . . . . . . . . . . . . . . . . . . . .. 265 References .................................................... 276

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xiv CONTENTS

III. THERMAL DIFFUSIVITY

CHAPTER 10. THE APPARATUS FOR THERMAL DIFFUSIVITY MEASUREMENT BY THE LASER PULSE METHOD K.D. Magiit and R.E. Taylor

1. Introduction ................................................ 281 2. Physical Model and Mathematical Interpretation. . . . . . . .. . . .... .. 281 3. Measurement System. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 284 4. Measurement Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 293 5. Estimate of Errors and Corrections. . . . . . . . . . . . . . . . . . . . . . . . . . . .. 299 6. Extension of the Method to Nonideal Materials ................. 307 7. Front-Face Methods ......................................... 311 References .................................................... 311

CHAPTER 11. MODULATED ELECTRON BEAM THERMAL DIFFUSIVITY EQUIPMENT R. De Coninck

1. Introduction................................................ 315 2. Principle of the Method ...................................... 315 3. Measurement Range Capacities . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 316 4. Description and Experimental Design Features . . . . . . . . . . . . . . . . .. 316 5. Mathematical Treatment of the Data .......... . . . . . . . . . . . . . . . .. 337 6. Practical Operation Techniques . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 342 7. Closing Remarks-Further Improvements . . . . . . . . . . . . . . . . . . . . . .. 343 N otation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 345 References .................................................... 346

CHAPTER 12. INSTRUMENTS FOR MEASURING THERMAL CONDUCTIVITY, THERMAL DIFFUSIVITY, AND SPECIFIC HEAT UNDER MONOTONIC HEATING E.S. Platunov

1. Introduction ................................................ 347 2. Theory of a Monotonic Regime . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 347 3. Theory of Measurement Techniques . . . . . . . . . . . . . . . . . . . . . . . . . . .. 349 4. Structural Features of Calorimeters ............................ 352 5. Accessories ................................................. 370 Notation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 372 References .................................................... 373

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CONTENTS xv

CHAPTER 13. APPARATUS FOR MEASURING THERMOPHYSICAL PROPERTlES OF LIQUIDS BY AC HOT-WIRE TECHNIQUES L.P. Phylippov, S.N. Kravchun, and A.S. Tleubaev

1. Introduction ............................................... 375 2. The Theory of the Method . . . . ... . .. . .. . . .... . . . . . . . . . . . . . . .. 376 3. Absolute and Relative Variants of the Method . . . . . . . . . . . . . . . . .. 380 4. The Effect of Radiation Heat Transfer. . . . . . . . . . . . . . . . . . . . . . . .. 381 5. The Effect of Convective Heat Transfer. . . . . . . . . . . . . . . . . . . . . . .. 384 6. The Effect of Diffusive Heat Conduction in Mixtures . . . . . . . . . . .. 385 7. The Limitations of the Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 386 8. The Apparatus Circuit. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 388 9. The Relation between Electrical Quantities Being Measured and

the Amplitude and Phase of Probe Temperature Oscillations ..... 389 10. Cireuit Adjustment, Control and Proeessing Program . . . . . . . . . . .. 393 11. Probe Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 397 12. Measurement Errors ........................................ 400 13. Hardware of Set and Microeomputer Input/Output Interface . . . .. 401 14. Measuring CelI Design .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 402 15. Conclusion....... . . . . . . . . . . . . . . . . . . .. . . . ... . . . . . . . . . . . . . . .. 404 References .................................................... 404

IV. SPECIFIC HEAT

CHAPTER 14. PRACTlCAL MODULATION CALORIMETRY Ya. A. Kraftmakher

1. Introduction ................................................ 409 2. Measurement of Specific Heat by the Equivalent-Impedance Method 412 3. Determination of Temperature Oscillations by Oseillations of

Sample Brightness ........................................... 418 4. Measuring the Specific Heat of Nonconducting Materials . . . . . . . .. 421 5. Modulation Dilatometer with Interferometric Recording . . . . . . . . .. 426 6. Electronic Equipment for Modulation Measurements . . . . . . . . . . . .. 428 7. Conclusion.................................................. 433 Notation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 433 Referenees .................................................... 434

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CHAPTER 15. PHASE-CHANGE CALORIMETER FOR MEASURING RELA TIVE ENTHALPY IN THE TEMPERA TURE RANGE 273.15 TO 1200 K David A. Ditmars

1. Introduction ................................................ 437 2. Schematic Overview of Apparatus. . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 438 3. Furnace for Temperatures to 1200 K ........................... 441 4. Phase-Change Calorimeter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 443 5. Operating the Calorimeter .................................... 451 6. General Observations and Recommended Operating Procedures ... 455 References .................................................... 456

CHAPTER 16. APPARATUS FOR INVESTIGATION OF THERMODYNAMIC PROPERTIES OF METALS BY LEVITATION CALORIMETRY Vitaliy Ya. Chekhovskoi

1. Introduction ................................................ 457 2. Major Units of Experimental Apparatus . . . . . . . . . . . . . . . . . . . . . . .. 459 3. Hermetically Sealed Chamber . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 461 4. Thermostat.................................................. 464 5. Jacket of the Calorimetric System. . . . . . . . . . . . . . . . . . . . . . . .. . . . .. 466 6. Calorimetric System. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 467 7. Resistance Thermometers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 470 8. Calorimeter Calibration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 473 9. Sequence of Experimental Steps. . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 476 Notation ................................................... ,. .. 479 References .................................................... 479

CHAPTER 17. A MILLISECOND-RESOLUTION PULSE HEATING SYSTEM FOR SPECIFIC-HEAT MEASUREMENTS AT HIGH TEMPERATURES Ared Cezairliyan

1. Introduction ................................................ 483 2. Measurement System. .... . .. . . . . . . . . . . . . . . . . . . . . . . . .. ... .. . .. 484 3. Measurement Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . .. 492 4. Consideration of Various Phenomena .......................... 499 5. Estimate of Errors .............. . . . . . . . . . . . . . . . . . . . . . . .. . . . .. 508 6. Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 516 References .................................................... 517

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CONTENTS xvii

CHAPTER 18. THE APPLlCATION OF DIFFERENTIAL SCANNING CALORIMETRY TO THE MEASUREMENT OF SPECIFIC HEAT M.J. Richardson

1. Differential Seanning Calorimetry . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 519 2. Specific Heat. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 520 3. Baseline Balancing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 524 4. Calibration.................................................. 526 5. Containment and Samples .................................... 536 6. Operation and Sources of Error ............................... 539 7. Instrumental Performance. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 542 Bibliography . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 544

V. THERMAL EXPANSION

CHAPTER 19. METHODS OF MEASURING THERMAL EXPANSION R.K. Kirby

1. Introduction ................................................ 549 2. Methods for Measuring ThermaI Expansion. . . . . . . . . . . . . . . . . . . .. 552 3. X-Ray Methods ............................................. 553 4. Capacitance Methods ........................................ 555 5. Pushrod Dilatometry . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 557 Notation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 565 References .................................................... 566

CHAPTER 20. RECENT THERMAL EXPANSION INTERFEROMETRIC MEASURING INSTRUMENTS G. Ruffino

1. Introduction ................................................ 569 2. Sample . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 569 3. Interferometers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 574 4. Light Sources ............................................... 582 5. Detector and Fringe Counter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 583 6. ThermaI System ............................................. 586 7. Temperature Measurement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 589 8. Data Acquisition and Treatment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 591 9. Error Analysis. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 597 References .................................................... 599

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xviii CONTENTS

CHAPTER 21. APPARATUS FOR CONTINUOUS MEASUREMENT OF TEMPERATURE DEPENDENCE OF DENSITY OF MOLTEN METALS BY THE METHOD OF A SUSPENDED PYCNOMETER AT HIGH TEMPERATURES AND PRESSURES E.E. Shpil'rain, K.A. Yakimovich, and A.G. Mozgovoi

1. Deseription of the Suspended Pyenometer Method . . . . . . . . . . . . . .. 601 2. Basie Components of the Experimental Setup ................... 604 3. The Experimental Setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . .. 613 4. Experiment: Preparations and Proeedure. . . . . . . . . . . . . . . . . . . . . . .. 616 5. Aeeuraey of the Measurement Results . . . . . . . . . . . . . . . . . . . . . . . . .. 622 6. Summary ..................... . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 623 Referenees .................................................... 624

VI. REVIEW OF CERTIFIED THERMOPHYSICAL PROPERTY STANDARD REFERENCE MATERIALS

CHAPTER 22. REFERENCE MATERIALS FOR THERMOPHYSICAL PROPERTIES .............. 627 R.K. Kirby

INDEX ....................................................... 635