Throughout the day, we apply experimental methods to estimate time, mass, volume, distance, velocity, and temperature—how much to eat (mass), what clothes to wear (temperature), how long will it take to get somewhere (distance, velocity, 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 Methods 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 temperatures 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 manufacturing 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 significant figures and what we mean by accuracy, precision, and error analysis. In this second edition, we report an explicit equation to calculate how many experiments are necessary to achieve a specified confidence interval. Chapter 3 reviews data analysis including hypothesis testing, data smoothing, 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 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 equation and Reynolds number, then lists common flow meters. The three physicochemical properties that Chapter 8 presents include viscosity, thermal conductivity, 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 solving problems but also to underline pitfalls in solving them. Measuring gas and liquid concentration by chromatography and mass spectrometry 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 characterize the physicochemical properties of solids and include infrared spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, nuclear magnetic resonance, 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, including 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 Department 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 contribution 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 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.

Spectroscopy / D.C. Boffito, C. Neagoe, G. Cerrato, C. Boffito, G.L. Chiarello, C.L. Bianchi, M.G. Rigamonti, A. Benamer, G.S. Patience - In: Experimental Methods and Instrumentation for Chemical Engineers / [a cura di] G.S. Patience. - Riedizione. - [s.l] : Elsevier, 2018. - ISBN 9780444640383. - pp. 339-382

### Spectroscopy

#### Abstract

Throughout the day, we apply experimental methods to estimate time, mass, volume, distance, velocity, and temperature—how much to eat (mass), what clothes to wear (temperature), how long will it take to get somewhere (distance, velocity, 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 Methods 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 temperatures 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 manufacturing 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 significant figures and what we mean by accuracy, precision, and error analysis. In this second edition, we report an explicit equation to calculate how many experiments are necessary to achieve a specified confidence interval. Chapter 3 reviews data analysis including hypothesis testing, data smoothing, 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 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 equation and Reynolds number, then lists common flow meters. The three physicochemical properties that Chapter 8 presents include viscosity, thermal conductivity, 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 solving problems but also to underline pitfalls in solving them. Measuring gas and liquid concentration by chromatography and mass spectrometry 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 characterize the physicochemical properties of solids and include infrared spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, nuclear magnetic resonance, 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, including 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 Department 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 contribution 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 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.
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2018
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Utilizza questo identificativo per citare o creare un link a questo documento: `https://hdl.handle.net/2434/525491`