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LASER EXPERIMENTS FOR CHEMISTRY AND PHYSICS
Laser Experiments for Chemistry and Physics

Robert N. Compton
and
Michael A. Duncan

3
 3
Great Clarendon Street, Oxford, OX2 6DP,
United Kingdom
Oxford University Press is a department of the University of Oxford.
It furthers the University's objective of excellence in research, scholarship,
and education by publishing worldwide. Oxford is a registered trade mark of
Oxford University Press in the UK and in certain other countries
© Robert N. Compton and Michael A. Duncan 2016
The moral rights of the authors have been asserted
First Edition published in 2016
Impression: 1
All rights reserved. No part of this publication may be reproduced, stored in
a retrieval system, or transmitted, in any form or by any means, without the
prior permission in writing of Oxford University Press, or as expressly permitted
by law, by licence or under terms agreed with the appropriate reprographics
rights organization. Enquiries concerning reproduction outside the scope of the
above should be sent to the Rights Department, Oxford University Press, at the
address above
You must not circulate this work in any other form
and you must impose this same condition on any acquirer
Published in the United States of America by Oxford University Press
198 Madison Avenue, New York, NY 10016, United States of America
British Library Cataloguing in Publication Data
Data available
Library of Congress Control Number: 2015939606
ISBN 978–0–19–874297–5 (hbk.)
ISBN 978–0–19–874298–2 (pbk.)
Printed and bound by
CPI Group (UK) Ltd, Croydon, CR0 4YY
Links to third party websites are provided by Oxford in good faith and
for information only. Oxford disclaims any responsibility for the materials
contained in any third party website referenced in this work.
Preface

Like most scientists, the authors of this textbook have been greatly influenced by
their academic backgrounds and mentors. Duncan and Compton were both un-
dergraduate students in small liberal arts colleges (Furman University and Berea
College, respectively) in which student research was a vital part of their educa-
tional experience. Performing undergraduate research was of equal importance
to course work. Both authors began their research careers at the time of the
development of the laser and were witness to many incredible advances in the
development and applications of this new technology.
In graduate school, Compton was particularly influenced by the first year ex-
perimental research course required of every incoming graduate student (theory
or experiment) in the Department of Physics at the University of Florida. In ad-
dition to experiments, Professor Alex Green included glass blowing and machine
shop fundamentals in this course. Although it is not a required course, a similar
experience is offered to the physics and chemistry graduate students at the Uni-
versity of Tennessee (UT) by Compton. Some of these experiments are included
in this book. In a few instances, the laboratory experiments resulted in an area of
research. For example, in the undergraduate laboratories students were required
to record and analyze a Raman spectrum of CCl4 at room temperature. Due to
the thermal rovibrational population, the Stokes lines are very broad at room tem-
perature. To resolve the isotope lines of CCl4 , one of the students in the advanced
physics laboratory (Darrin Ellis) recorded a Raman spectrum of CCl4 submerged
under liquid nitrogen in a Styrofoam cup. Due to rovibrational cooling, the spec-
trum of CCl4 under liquid nitrogen shows fully resolved isotopic contributions
due to the 35 Cl and 37 Cl isotopes (see Chapter 18, Figure 18.3). A number of
papers have appeared illustrating the advantages and utility of Raman Under Ni-
trogen (RUN). As a graduate student in 1962 working under G. S. Hurst at the
Oak Ridge National Laboratory, Compton was privileged to purchase and use
one of the first commercial (Bendix Corporation) time-of-flight mass spectrom-
eters (TOF-MS). His thesis employed electron impact ionization, but after the
development of the pulsed laser Compton integrated many home-built TOF-MS
instruments into laser ionization experiments at ORNL and UT. In 1979, col-
leagues J. A. D. Stockdale and Compton formed a scientific instruments company
in Oak Ridge known as Comstock, which manufactured and sold TOFs as well as
electrostatic energy analyzers (ESAs). Many of these instruments have been used
by researchers around the world to record multiphoton ionization mass and pho-
toelectron spectra. This company has employed a number scientists, engineers,
and machinists, which has enriched their lives as well as science in general.
vi Preface

As an undergraduate at Furman, Duncan learned to solder from Professor Lon

Knight and together they built a vacuum system for matrix isolation experiments
and EPR studies of unusual radicals. At Rice University in the group of Richard
Smalley, he was given the task of designing and building their first time-of-flight
mass spectrometer. With virtually no electronics background, Duncan was guided
by the electronics shop to the classic paper by Wiley and McLaren (Rev. Sci.
Instrum. 26, 1150 (1955)). After many design pitfalls and burned-out circuits, he
eventually made a working instrument and incorporated it into their supersonic
molecular beam machine. Other experiments and a misaligned Nd:YAG laser led
inadvertently to the discovery of the laser vaporization method used to produce
gas-phase clusters of metal atoms and other refractory elements. It was this laser
vaporization method and the same mass spectrometer that were later employed
by Jim Heath and Sean O'Brien in the Smalley group to discover C60 . At Georgia,
Duncan has continued to design and implement new versions of time-of-flight
mass spectrometers into his research, and has also developed new experiments
for the undergraduate labs using these instruments, many of which are included
in this book.
The authors have employed many kinds of modern lasers and laser techniques
in their research and teaching laboratories. Compton was one of the first to study
and employ nonlinear optical processes in atomic and molecular research and
some of this early work is found in the chapters describing multiphoton ionization,
stimulated electronic Raman scattering (SERS), and third harmonic generation
(THG). Duncan has employed photoionization, laser desorption analysis of ma-
terials, and mass-selected ion photodissociation measurements throughout his
research. Both authors have developed advanced physical chemistry laboratories
at their respective universities and are deeply indebted to the numerous students
who have passed through these laboratories, many of whom are now directing
their own physical chemistry or physics laboratories at other universities.
This book is designed to introduce researchers to the breadth of available ex-
periments in chemical physics that can be integrated into physics and chemistry
laboratories. The authors have tried to include chapters that are fundamental to
lasers and spectroscopy and provide theoretical background to the experiments
described. For example, the chapters on properties of light, diffraction, etc., and
rovibrational spectroscopy should be read before considering the experiments
describing IR and Raman spectroscopy, optical activity, and other laser-based
experiments. We hope that the enjoyment of laser experiments and their role
in advancing chemistry and physics can be appreciated by a new generation of
scientists through the experiments presented here.
Robert N. Compton, Knoxville, TN
Michael A. Duncan, Athens, GA
Acknowledgments

The authors are grateful to the many graduate and undergraduate students who
have worked in their labs over the years and have contributed to the experiments
described here. Special recognition is due to the many Teaching Assistants who
implemented these experiments in the undergraduate and graduate laboratories
at the University of Tennessee and the University of Georgia. MAD would like to
thank Professors Lionnel Carreira and Allen King, who shared ideas and provided
feedback for lab experiments early in his career at Georgia. RNC is indebted to
Professor Charles Feigerle for collaborations on the study of MPI of molecu-
lar iodine, to Dr. Donald Armstrong, Dr. Stewart Hager, and Dr. Jeffery Steill
(Sandia Laboratory) for assisting with recording the numerous FTIR spectra,
and to Dr. James Parks for sharing an experiment from the advanced physics
laboratories at UT. Special thanks are also due to former masters degree student
Darren Ellis for performing the first RUN spectrum in our laboratories at UT.
We would also like to acknowledge the special help in preparing this manu-
script from Mr. Jonathan Maner (proofreading), Ms. Alex Orlowsky (figure prep-
aration), Mr. Joshua Marks (photography), Mr. Timothy Ward and Mr. David
McDonald (computational work), and Mr. Ivan Geigerman (figure preparation).
We are also grateful to Drs. Sharani Roy and Jay Agarwal for a critical assessment
of Chapter 15 on quantum chemistry calculations. Dr. Paul Siders is gratefully
acknowledged for contributions to Chapter 22 on Fermi resonances.
Table of Contents

Part I Introduction to Light, Lasers, and Optics

1 Elementary Properties of Light 3

2 Basic Optics 28

3 General Characteristics of Lasers 53

4 Laboratory Lasers 63

5 Nonlinear Optics 88

6 Laser Safety 102

Part II Laser Experiments for Thermodynamics

7 The Speed of Light 115

8 The Speed of Sound in Gases, Liquids, and Solids 122

9 Thermal Lens Calorimetry 144

10 Laser Refractometry 152

Part III Laser Experiments for Chemical Analysis

11 Laser-Induced Breakdown Spectroscopy 159

12 Laser Desorption Time-of-Flight Mass Spectrometry 167

13 Multiphoton Ionization Mass Spectrometry of Metal Carbonyls 198

Part IV Laser Experiments for Quantum Chemistry and Spectroscopy

14 Optical Spectroscopy 207

15 Quantum Chemistry Calculations 243

16 Multiphoton Ionization and Third Harmonic Generation in Alkali Atoms 259

17 Electronic Absorption Spectroscopy of Molecular Iodine 273

18 Electronic Spectroscopy of Iodine Using REMPI 280

19 Raman Spectroscopy Under Liquid Nitrogen 288

x Table of Contents

20 Optical Rotary Dispersion of a Chiral Liquid (α-pinene) 299

21 Faraday Rotation 306

22 Fermi Resonance in CO2 316

23 Photoacoustic Spectroscopy of Methane 322

24 Optogalvanic Spectroscopy 329

25 Diode Laser Atomic Spectroscopy 334

26 Vacuum Ultraviolet Spectroscopy using THG in Rare Gases 343

27 Raman Shifting and Stimulated Electronic Raman Scattering (SERS) 350

Part V Laser Experiments for Kinetics

28 Fluorescence Lifetime of Iodine Vapor 365

29 Raman Spectroscopy Applied to Molecular Conformational Analysis 372

30 Diffraction of Light from Blood Cells 379

31 Inversion of Sucrose by Acid-Catalyzed Hydrolysis 388

Appendix I: Recommended Components and Equipment 393

Appendix II: Fast Signal Measurements 398
Index 401
Part I
Introduction to Light,
Lasers, and Optics
Elementary Properties
of Light
1
Introduction 3
Introduction Maxwell's Equations 6
Speed of light 7
The experiments described in this book involve the use of laser light in a wide
Light as a particle 8
range of applications. The present chapter is an elementary introduction to the
Photon energies and molecular
properties of light that will serve to make these experiments more understandable.
properties 14
This chapter, along with Chapter 2, is certainly not intended to replace a rigorous
Photon sources and detectors 18
course in physical or geometrical optics; rather it is a summary of some of the
References 26
important concepts and formulae in optics applied to the use of lasers in chemical
physics research.
All electromagnetic (E&M) waves propagate with the same velocity in free
space (which is defined as c) and differ only in frequency, ν, and wavelength, λ,
through the relationship c = λν. There is one report of E&M waves having a wave-
length of 1.9 × 107 miles.[1] At the other extreme, the Compton Gamma Ray
Observatory (GRO), a NASA satellite, has been used to detect gamma rays with
wavelengths as small as 40 femtometers (40 × 10–15 meters), approximately the
size of a proton.
The description of electromagnetic radiation is carried out using a classi-
cal/quantum mechanical wave/particle treatment. Certain phenomena are best
described using waves and others can only be explained by treating light as par-
ticles called photons. All light phenomena can be explained by treating light as
photons; however, in most cases the wave picture is easier to employ. The en-
ergy of a photon is Planck's constant h times the frequency, ν (E = hν). Photons
have momentum (p = h/λ) but no mass. In 1890 Heinrich Hertz first produced
radiowaves ("Maxwellian waves") in the laboratory and it was many more years
before Marconi put them to good use in communications. We now know that any
material object (gas, liquid, or solid) having a temperature above absolute zero
(0 K) will emit photons. For so-called "black-body" radiators the temperature is
related to the photon energy hν and emitted light intensity I(ν,T) by the Planck
Black-body radiation formula:

2hν3 1
I(ν, T) =  hν  (1.1)
c2 e kT –1

The Planck radiation law represents the power per unit area per unit solid
angle per unit frequency emitted from a black body in thermal equilibrium.

Laser Experiments for Chemistry and Physics. First Edition. Robert N. Compton and Michael A. Duncan.
© Robert N. Compton and Michael A. Duncan 2016. Published in 2016 by Oxford University Press.
4 Elementary Properties of Light

This function has a maximum (i.e., setting the derivative dI(ν,T)/dν = 0 and
solving for νmax from equation (1.1)) corresponding to hνmax = 2.82 kT. Al-
ternately one can write this in the form of the Wien's Displacement Law as
λmax T = 2.8977685(51)×10–3 m · K.
The Planck radiation law is known to accurately describe the emission from
stars, the heater eye on an electric stove, and even the cosmic background
radiation left over from the Big Bang creation of the universe. The Cosmic Mi-
crowave Background (CMB) consists of photons left over from the Big Bang,
which through multiple collisions have established a thermal "cosmic black-body"
equilibrium. In Figure 1.1 the microwave cosmic background radiation data is
fitted to a Planck radiation law prediction (equation 1.1) giving a temperature
of 2.725 K. The data were recorded using the Far-Infrared Absolute Spectro-
photometer (FIRAS) onboard NASA's Cosmic Background Explorer (COBE)
satellite. [2] It is remarkable that the experimental data points lie within the line
(theory) in Figure 1.1.
The black-body temperature for the data in Figure 1.1 was determined from a
fit to equation (1.1), but this can also be estimated using Wien's displacement law
hνmax = 2.82 kT or alternately νmax = 58.79 (GHz/K)T. Using T = 2.725 K gives
νmax = 160.2 GHz.
It is impossible to make a representation of the full wavelength range of E&M
waves. There are regions of the spectrum yet to be explored at both the long and
short wavelength regions. Figure 1.2 is an attempt to show on one scale the range
of the spectrum that science has presently explored.

Spectrum of the cosmic microwave

background
Frequency (GHz)
100 200 300 400 500
400

T = 2.725 ± 0.001 ºK

300
Intensity (MJy/sr)

200
Figure 1.1 Cosmic microwave back-
ground spectrum fit to a Planck radia-
tion law function (equation 1). The data
points are smaller than the line drawn 100
using the Planck law. The deviations
are less than 0.30% of the peak bright-
ness, with an rms value of 0.01%. (This 0
COBE/FIRAS image was kindly pro- 1 0.2 0.1 0.07 0.05
vided by COBE Science Team/NASA.) Wavelength (cm)
 Introduction 5

Radiowave Microwave IR UV X-ray Gamma ray

Figure 1.2 Illustration of the known

100 1 10–2 10–4 10–6 10–8 10–10 10–12 full electromagnetic spectrum of light
Wavelength (meters) from radiowaves to gamma rays.

Table 1.1 Approximate wavelength, frequency, energy, and temperature corresponding to Figure 1.2.

E&M Wavelength cm, Frequency Energy eV Energy cm–1 Energy kcal/mol Temp. K
except as noted Hz

Radiowave > 10 ~ 109 < 10–5 < 0.1 cm–1 < 2.9 × 10–4 < 0.03
Microwave 10 – 0.01 ~ 1012 10–5 – 0.01 0.1 – 100 3 × 10–4 – 3 × 10–1 0.03 – 30
Infrared 0.01 – 7 × 10 –5
~ 10 14
0.01 – 1 2
10 – 10 4
3 × 10 – 29 –1
30 – 4100
Visible 7 × 10 – 4 × 10
–5 –5
~ 10 15
~1–3 (1.0 – 2.5) × 10 4
29 – 71 4100 – 7300
700 – 400 nm
Ultraviolet 4 × 10–5 – 10–7 ~ 1016 ~ 3 – 103 2.5×104 – 107 71 – 2.9 × 104 7300 – 3 × 106
400 – 1 nm
X-ray 10–7 – 10–9 ~ 1018 103 – 105 107 – 109 104 – 106 3 × 106 – 3 × 108
Gamma ray < 10–9 > 3 × 1019 > 105 > 109 > 3 × 108

Maxwell was the first to show that visible light represents but a narrow compo-
1600
nent of the entire electromagnetic spectrum. From this figure we see that visible
light represents only one octave out of almost 60 octaves of the known electro-
Lumens/watt

1200
magnetic spectrum. This wavelength range is further described in Table 1.1 in
terms of wavelength, frequency, energy, and temperature. 800
The visible spectrum ranges in wavelength from approximately 400 to 700 nm.
The sensitivity of the human eye to visible light depends upon the observer and 400
the time of day. Figure 1.3 shows the relative sensitivity curves for the standard
observer as defined by the International Commission on Illumination. The Inter- 0
380

480

580

680

national Commission on Illumination, which was established in 1913 and based 780
in Vienna, Austria, is the international authority on light, illumination, and color. Wavelength (nm)
A complete description of the sensitivity of the eye can be found in the book
by Williamson and Cummins.[3] As mentioned before, visible light is but a nar- Figure 1.3 Relative sensitivity of the
row and somewhat ill-defined region of the spectrum. The curves in Figure 1.3 human eye of a standard observer as a
are ill-defined in the sense that the relative sensitivity of the eye for humans can function of wavelength under conditions
only be considered for a standard observer. The standard curve also varies under of daylight vision (photopic, dashed line)
different light levels because of the sensitivity difference of the rods and cones and night vision (scotopic, solid line).
covering the retina. The rod system is about 1000 times more sensitive than the
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