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 EXPERIMENTAL METHODS
AND INSTRUMENTATION FOR
CHEMICAL ENGINEERS
SECOND EDITION

GREGORY S. PATIENCE
Experimental Methods and
Instrumentation for Chemical Engineers
This page intentionally left blank
Experimental Methods
and Instrumentation
for Chemical Engineers

Second Edition
Gregory S. Patience
Department of Chemical Engineering, Polytechnique Montréal, Canada
Elsevier
Radarweg 29, PO Box 211, 1000 AE Amsterdam, Netherlands
The Boulevard, Langford Lane, Kidlington, Oxford OX5 1GB, United Kingdom
50 Hampshire Street, 5th Floor, Cambridge, MA 02139, United States
Copyright © 2018 Elsevier B.V. All rights reserved.
No part of this publication may be reproduced or transmitted in any form or by any means, electronic or
mechanical, including photocopying, recording, or any information storage and retrieval system, without
permission in writing from the publisher. Details on how to seek permission, further information about
the Publisher’s permissions policies and our arrangements with organizations such as the Copyright
Clearance Center and the Copyright Licensing Agency, can be found at our website:
www.elsevier.com/permissions.
This book and the individual contributions contained in it are protected under copyright by the Publisher
(other than as may be noted herein).
Notices
Knowledge and best practice in this field are constantly changing. As new research and experience
broaden our understanding, changes in research methods, professional practices, or medical treatment
may become necessary.
Practitioners and researchers must always rely on their own experience and knowledge in evaluating and
using any information, methods, compounds, or experiments described herein. In using such information
or methods they should be mindful of their own safety and the safety of others, including parties for
whom they have a professional responsibility.
To the fullest extent of the law, neither the Publisher nor the authors, contributors, or editors, assume any
liability for any injury and/or damage to persons or property as a matter of products liability, negligence
or otherwise, or from any use or operation of any methods, products, instructions, or ideas contained in
the material herein.

Library of Congress Cataloging-in-Publication Data

A catalog record for this book is available from the Library of Congress

British Library Cataloguing-in-Publication Data

A catalogue record for this book is available from the British Library

ISBN: 978-0-444-64038-3

For information on all Elsevier publications

visit our website at https://www.elsevier.com/books-and-journals

Publisher: John Fedor

Acquisition Editor: Kostas Marinakis
Editorial Project Manager: Amy Clark
Production Project Manager: Maria Bernard
Designer: Miles Hitchen
Typeset by VTeX
Contents

List of Contributors xiii

Preface xv

1. Introduction
G.S. Patience
1.1 Overview 1
1.2 Metrology 3
1.3 Scientific Method 5
1.4 Industrial Quality Control 5
1.5 Units of Physical Quantities 7
1.6 Writing Conventions 8
1.7 Unit Conversion 11
1.8 Exercises 15
References 16

2. Measurement and Analysis

G.S. Patience
2.1 Overview 17
2.2 Significant Figures 18
2.3 Statistical Notions 20
2.3.1 Normal (Gaussian) Distribution 22
2.3.2 Criterion of Chauvenet 27
2.3.3 Uncertainty (Type B) 29
2.3.4 Confidence Intervals and Uncertainty (Type A) 29
2.3.5 Sample Size 33
2.3.6 Uncertainty Propagation 33
2.4 Instrumentation Concepts 37
2.4.1 Interval 37
2.4.2 Range, Span, Full Scale 37
2.4.3 Resolution, Sensitivity, Detection Limit, Threshold 37
2.4.4 Precision 38
2.4.5 Error 39
2.4.6 Accuracy 42

v
vi Contents

2.4.7 Repeatability and Reproducibility 44

2.5 Representing Data Graphically 46
2.5.1 Plotting Pitfalls 52
2.5.2 3-D and Contour Graphs 52
2.5.3 Bar Charts 54
2.6 Fast Fourier Transform (FFT) 54
2.7 Error Bars 55
2.8 Exercises 56
References 62

3. Experimental Planning
G.S. Patience and A. Bérard
3.1 Overview 65
3.2 Data and Experiments 65
3.2.1 Monitoring 66
3.2.2 Qualification 67
3.2.3 Prove-Out 67
3.2.4 Scouting/Process Development 67
3.2.5 Troubleshooting 68
3.3 Data Analysis 68
3.3.1 Data Smoothing 68
3.3.2 Hypothesis Testing 70
3.3.3 Statistical Tests 71
3.3.4 Error Bars 73
3.3.5 Regression Analysis 75
3.3.6 Coefficient of Determination 76
3.3.7 Nonlinear Regression Analysis 78
3.3.8 Errant Model Data 79
3.4 Design of Experiments (DOE) 81
3.5 Statistical Designs 85
3.5.1 Full Factorial Designs 86
3.5.2 Fractional Factorial Designs 88
3.5.3 Plackett–Burman Design 89
3.5.4 Taguchi Design 90
3.5.5 Central Composite Design—CCD 90
3.5.6 Box–Behnken Design 92
3.5.7 Case Study—Saving Organic Apples 92
3.6 Exercises 97
References 106

4. Force and Mass

J. Gostick
4.1 Overview 107
4.2 Electrical Properties of Strained Metals 109
4.3 Strain Gauge 110
 Contents vii

4.3.1 Gauge Factor 110

4.3.2 Strain Gauge Circuit 111
4.3.3 The Impact of Temperature on Resistance 113
4.4 Strain to Measure Force and Mass 114
4.4.1 Load Cells 114
4.4.2 Pressure Sensors 116
4.5 Other Force Sensing Techniques 117
4.5.1 Force Sensing Resistors 117
4.5.2 Electromagnetic Force Compensation 119
4.5.3 Piezoelectric Sensors and Accelerometers 120
4.6 Exercises 121
References 121

5. Pressure
G.S. Patience

5.1 Overview 123

5.2 Units of Pressure 128
5.3 Types of Pressure 128
5.3.1 Atmospheric Pressure 128
5.3.2 Gauge Pressure 129
5.3.3 Differential Pressure 129
5.3.4 Vacuum Pressure 130
5.3.5 Static and Dynamic Pressure 130
5.3.6 Barometric Pressure 132
5.4 Instrumentation 136
5.4.1 Barometer 136
5.4.2 U-Tube Manometer 137
5.4.3 Bourdon Gauge 139
5.4.4 Diaphragm and Bellows 140
5.4.5 Vacuum 142
5.4.6 Capsule Pressure Gauge 143
5.4.7 McLeod Gauge 144
5.4.8 Pirani Gauge 145
5.5 Process Equipment and Safety 146
5.5.1 Pressure Regulator 146
5.5.2 Back Pressure Regulator 147
5.5.3 Relief Valves 147
5.5.4 Rupture Disk 147
5.5.5 Pressure Testing 148
5.5.6 Leak Test 149
5.6 Instrumentation 149
5.7 Exercises 151
References 158
viii Contents

6. Temperature
G.S. Patience and P.A. Patience
6.1 Overview 159
6.2 Temperature Scales 161
6.2.1 Wet-Bulb, Dry-Bulb Temperature, Dew Point 164
6.2.2 Humidex, Heat Index 166
6.2.3 Wind Chill Factor 166
6.3 Mechanical Instruments 167
6.3.1 Gas Thermometers 167
6.3.2 Liquid Thermometers 171
6.3.3 Bimetallic Thermometers 175
6.4 Electrical Instruments 178
6.4.1 Thermistors 179
6.4.2 Resistance Temperature Devices (RTDs) 180
6.4.3 Thermocouples 182
6.4.4 Thermopile 191
6.5 Radiation 194
6.6 Pyrometry 194
6.6.1 Thermal Radiation 194
6.6.2 Pyrometers 195
6.7 Exercises 197
References 199

7. Fluid Metering
G.S. Patience
7.1 Overview 201
7.2 Fluid Dynamics 202
7.3 Flow Meter Selection 206
7.4 Positive Displacement 209
7.5 Differential Pressure 212
7.5.1 Obstruction Meters—Orifice 212
7.5.2 Obstruction Meters—Venturi 214
7.5.3 Compressible Flow 215
7.5.4 Restriction Orifice 216
7.5.5 Pitot Tube 217
7.6 Rotameters 219
7.7 Thermal Mass Flow Meters—MFC 222
7.7.1 Hot Wire Anemometry 223
7.8 Coriolis 223
7.9 Inferential—Turbine 224
7.10 Oscillatory—Vortex 224
7.11 Flow Meters in an Industrial Setting 225
Exercises 229
References 232
 Contents ix

8. Physicochemical Analysis
G.S. Patience
8.1 Overview 233
8.2 Thermal Conductivity 233
8.2.1 Pressure, Temperature Effects 237
8.2.2 Insulation Design 237
8.3 Viscosity 242
8.3.1 Single Phase Flow 244
8.3.2 Reynolds Number 245
8.3.3 Prandtl Number 246
8.3.4 Viscosity Instrumentation 248
8.3.4.1 Newtonian Fluids 248
8.3.4.2 The Saybolt Viscometer 250
8.3.4.3 Non-Newtonian Fluids 251
8.3.4.4 The Rotational Rheometer 251
8.3.5 Influence of Temperature and Pressure on Viscosity 252
8.4 Binary Gas Diffusion 252
8.4.1 Schmidt Number 254
8.4.2 Measuring Diffusion 255
8.4.2.1 Water Vapor Diffusion through Permeable
Materials 256
8.5 Exercises 258
References 262

9. Gas and Liquid Concentration

D. Béland, S. Lucini, C. Neagoe, P. Perreault, F. Galli, and
G.S. Patience
9.1 Overview 263
9.2 Chromatography Theory 263
9.2.1 The Distribution Coefficient 265
9.2.2 The Capacity Factor 266
9.2.3 The Selectivity Factor 267
9.2.4 The Number of Theoretical Plates 268
9.2.5 Eddy Diffusion 269
9.2.6 Longitudinal Diffusion 270
9.2.7 Resistance to Mass Transfer 270
9.2.8 Resolution 271
9.3 Gas Chromatography 273
9.3.1 Columns 273
9.3.2 Injectors 275
9.3.3 Detectors 276
9.4 High-Performance Liquid Chromatography 278
9.5 Method Development 278
9.6 Troubleshooting 280
9.6.1 The Flat Line 281
x Contents

9.6.2 Changing Peak Retention Times 282

9.6.3 Varying Peak Heights 283
9.7 Mass Spectrometry 284
9.8 Exercises 286
References 292

10. Analysis of Solids and Powders

G.S. Patience, M.G. Rigamonti, and H. Li
10.1 Overview 293
10.2 Density 294
10.2.1 Bulk Density 295
10.2.2 Particle Density 298
10.2.3 Skeletal Density 300
10.3 Diameter and Shape 302
10.3.1 Equivalent Diameter 304
10.3.2 Shape Factors—Sphericity 304
10.3.3 Particle Terminal Velocity 307
10.3.4 Reactor Pressure Drop (Fixed/Packed Beds) 308
10.3.5 Fluidization 311
10.4 Particle Size Distribution 314
10.4.1 Population of Particles 314
10.5 Sampling 319
10.6 Particle Size Distribution (PSD) Analytical Techniques 322
10.6.1 Sieve Analysis 323
10.6.2 Laser Diffraction 325
10.7 Microscopy 327
10.7.1 Electrical Sensing Instruments 327
10.7.2 SEM: Scanning Electron Microscopy 328
10.7.2.1 EDS: Energy-Dispersive X-ray Spectroscopy 329
10.7.3 TEM: Transmission electron microscopy 329
10.7.3.1 EDS for TEM 330
10.8 Surface Area 331
10.9 Exercises 333
References 337

11. Spectroscopy
D.C. Boffito, C. Neagoe, G. Cerrato, C. Boffito, G.L. Chiarello,
C.L. Bianchi, M.G. Rigamonti, A. Benamer, and G.S. Patience
11.1 Overview 339
11.2 Infrared Spectroscopy—IR 344
11.3 Ultraviolet/Visible Spectroscopy—UV/Vis 345
11.4 X-ray Diffraction—XRD 350
11.4.1 Crystalline Materials 352
11.4.2 Powder Diffraction 354
11.4.3 Crystal Size 355
 Contents xi

11.5 X-ray Photoelectron Spectroscopy—XPS 357

11.6 Nuclear Magnetic Resonance—NMR 359
11.6.1 1 H and 13 C Liquid NMR Analysis 361
11.6.2 Reading an NMR Spectrum 362
11.7 X-ray Absorption—XAS 366
11.7.1 The Absorption Coefficient (μ) 367
11.7.2 XAS Experimental Setup 368
11.7.3 X-ray Fluorescence—XRF 370
11.7.4 The Near-Edge Structure—XANES 370
11.7.5 Extended X-ray Absorption Fine Structure—EXAFS 371
11.8 Refractometry 376
11.9 Exercises 378
References 382

Solutions 385
Index 401
This page intentionally left blank
List of Contributors

D. Béland, Varian

A. Benamer, Polytechnique Montréal

A. Bérard, Polytechnique Montréal
C.L. Bianchi, Università Degli Studi di Milano
C. Boffito, Università Degli Studi di Milano

D.C. Boffito, Polytechnique Montréal

G. Cerrato, Università Degli Studi di Milano
G.L. Chiarello, Università Degli Studi di Milano
F. Galli, Polytechnique Montréal

J. Gostick, University of Waterloo

H. Li, Polytechnique Montréal
S. Lucini, Shimadzu Scientific Instruments
C. Neagoe, Polytechnique Montréal

G.S. Patience, Polytechnique Montréal

P.A. Patience, Polytechnique Montréal
P. Perreault, Polytechnique Montréal
M.G. Rigamonti, Polytechnique Montréal

xiii
This page intentionally left blank
Preface

Throughout the day, we apply experimental methods to estimate time, mass, vol-
ume, distance, velocity, and temperature—how much to eat (mass), what clothes
to wear (temperature), how long will it take to get somewhere (distance, veloc-
ity, and time). Preparing a meal requires some precision with respect to these
factors, and the kitchen was the first laboratory for chemists and engineers. We
continue to share many concepts related to instrumentation and experimental
design. This book presents the basic principles of measurement particular to
chemical engineering. Redacting this manuscript has been a collaborative effort;
its original inspiration was J.P. Holman’s textbook entitled “Experimental Meth-
ods for Engineers.” In this 2nd edition, we revise the text entirely, correct typos
(and other errors), and add a chapter on mass and distance and spectroscopy.
Each chapter begins with a historical perspective to recognize the work of
early pioneers but also to stimulate the imagination of the students. For example,
10 000 years ago, man created plaster from limestone. Plaster requires temper-
atures nearing 900°C, which is 150°C higher than an open pit fire. It requires
1000 kg of wood (chopped by stone axes), 500 kg of limestone, a pit 2 m in
diameter and 0.7 m deep, rocks to insulate, and two days to burn. Modern man-
ufacturing errors are costly and a nuisance; in prehistoric times, errors would
have been considerably more than just an inconvenience.
In Chapter 1, we list the seven steps of the scientific method and review the
rules of nomenclature—units of physical quantities, abbreviations, conversion
between SI and British Units, writing convention. Chapter 2 introduces signif-
icant figures and what we mean by accuracy, precision, and error analysis. In
this second edition, we report an explicit equation to calculate how many exper-
iments are necessary to achieve a specified confidence interval.
Chapter 3 reviews data analysis including hypothesis testing, data smooth-
ing, and statistical tests. We summarize design of experiments, and we include
more detail in this edition to describe factorial designs, outlining them and other
complementary designs with detailed examples.
Chapter 4 is new and introduces stress, strain, and electrical properties that
relate to manufacturing sensors for mass and force. We apply these concepts in

xv
xvi Preface

Chapters 5 and 6 that deal with pressure and temperature measurements. In each
of these chapters, we first review basic concepts, including thermodynamics.
Then we describe the sensors that rely on mechanical and electrical properties.
Chapters 7 and 8 continue with chemical engineering fundamentals of fluid
flow and physicochemical properties. The former begins with Bernoulli’s equa-
tion and Reynolds number, then lists common flow meters. The three physic-
ochemical properties that Chapter 8 presents include viscosity, thermal con-
ductivity, and diffusion. It demonstrates how these properties are related and
introduces non-dimensional numbers.
Examples throughout the book help the students grasp the mechanics of solv-
ing problems but also to underline pitfalls in solving them.
Measuring gas and liquid concentration by chromatography and mass spec-
trometry is the subject of Chapter 9. In this edition, we dedicate more scope
to troubleshooting the chromatographic instruments. Spectroscopic instruments
we detail in Chapter 11. This summary includes sections written by eminent
chemists. We have selected the most powerful techniques used to character-
ize the physicochemical properties of solids and include infrared spectroscopy,
X-ray diffraction, X-ray photoelectron spectroscopy, nuclear magnetic reso-
nance, UV/Vis, X-ray absorption, and refractometry
Whereas Chapter 11 probes the nature of the solids phases, composition
and morphology, Chapter 10 concentrates on powder properties—particle shape,
size distribution, density, and surface area.
The first edition of this book was a collaborative effort in which Melina
Hamdine early on drafted several chapters in French, including Physicochemical
Properties, Analysis of Powders and Solids, and Design of Experiments. Prof.
Bala Srinivasan contributed to Chapter 3 on experimental design. Katia Senécal
was “instrumental” in gathering the essential elements for the chapters, includ-
ing Measurement Analysis, Pressure, Temperature, and Flow Rate. Prof. Bruno
Detuncq collaborated in the revision of these chapters. Danielle Béland led the
redaction of the chapter on chromatography to determine concentration, with
some assistance from Cristian Neagoe. He also wrote the section concerning
spectroscopy. Amina Benamer contributed extensively to this project, including
preparing solutions to the problems after each chapter, writing sections related
to refractometry and X-ray, and translating. Second-year students from the De-
partment also participated by proposing original problems that were added at
the end of each chapter (together with the name of the author of the problem).
I would particularly like to recognize Paul Patience for his tremendous contribu-
tion throughout the creative process of preparing this manuscript. The depth of
his reflection has been appreciated tremendously (LATEX). He also co-authored
the section on pyrometry. Christian Patience prepared many of the drawings and
 Preface xvii

Nicolas Patience helped with translating from French to English, as did Nadine
Aboussouan.
This second edition is no less a collaborative effort. Ariane Bérard expanded
Chapter 3 with examples of experimental designs. Prof. J. Gostick contributed
the chapter on Mass and Force instrumentation. Stefano Lucini wrote the section
on troubleshooting GC and HPLC instruments, while F. Galli contributed to
the section on mass spectrometry with Patrice Perreault, who was devout at
identifying errors and proposing additional problems. Marco Rigamonti and He
Li wrote sections of Chapter 10. Collaborators on Chapter 11 included Daria
C. Boffito, Cristian Neagoe, Giuseppina Cerrato, Claudio Boffito, Gian Luca
Chiarello, Claudia L. Bianchi, Marco G. Rigamonti, and Amina Benamer. This
chapter is a tremendous contribution to the book because it details simply which
instruments measure which physicochemical property and then describes how
they work.
This page intentionally left blank
Chapter 1

Introduction
G.S. Patience
Polytechnique Montréal

1.1 OVERVIEW
Experimental methods and instrumentation—for the purpose of systematic,
quantifiable measurements—have been a driving force for human development
and civilization. Anthropologists recognize tool making, together with language
and complex social organizations, as a prime distinguishing feature of Homo
sapiens from primates and other animals. However, the animal kingdom shares
many practices characteristic of experimentation, instrumentation and innova-
tion. Animals measure distance, height, size, estimate probabilities and adapt
objects for tasks: cheetahs, for example, gauge distance between themselves
and their prey before giving chase. Several species devise tools: branches are
levers for large arboreal primates that travel through the forest from tree to tree;
chimpanzees modify sticks as implements to extract grubs from logs; beavers
cut down trees and use mud and stones to build dams and lodges; and, Betty
the crow bends a wire to make a hook to get food out of a narrow tube. If
the act of modifying a twig to extract grubs is considered “tool making” then
we need a more specific definition to differentiate humans from other species.
Man uses tools to make tools and adopts a methodology to improve an out-
come or function. One of the earliest examples of applying methodology is
when early hominids manufactured chopping and core tools—axes and fist
hatchets—before the Lower Paleolithic period (from 650 000 to 170 000 BC):
they produced blades and implements by cleaving rocks with a certain force at
a specific angle to produce sharp edges. The raw material—a rock—is modified
through the use of an implement—a different rock—to produce an object with
an unrelated function (cutting, scraping, digging, piercing, etc.). Striking rocks
(flint) together led to sparks and the discovery of how to make fire.
Throughout the day, we measure mass, size, time, temperature and use in-
struments. The clothes that we wear, the food that we eat, the objects that we
manipulate have all been developed and optimized with standardized procedures
and advanced instrumentation. Sensors have increased the efficiency and safety
of automobiles: gauges in the car assess gasoline/air ratio, rain on the wind-
Experimental Methods and Instrumentation for Chemical Engineers
http://dx.doi.org/10.1016/B978-0-44-463782-6.00001-X 1
Copyright © 2018 Elsevier B.V. All rights reserved.
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