UV-VIS Spectroscopy and Its Applications

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1 SPRINGER LABORATORY

2 Heinz-Helmut Perkampus UV-VIS Spectroscopy and Its Applications Translated by H. Charlotte Grinter and Dr. T. L. Threlfall With 78 Figures and 21 Tables Springer -Ver lag Berlin Heidelberg New York London Paris Tokyo Hong Kong Barcelona Budapest

3 Professor em. Dr. HEINZ-HELMUT PERKAMPUS Heinrich-Heine-Universitat Physikalische Chemie und Elektrochemie I UniversitatsstraBe W-4000 Dusseldorf 1 ISBN-13: e-isbn-13: DOl: / Library of Congress Cataloging-in-Publication Data. Perkampus, Heinz-Helmut. [UV-VIS Spektroskopie und ihre Anwendungen. English] UV-VIS spectroscopy and its applications/ Heinz-Helmut Perkampus; translated by H. Charlotte Grinter and T. L. Threlfall. p. cm. Includes bibliographical references and indexes. lsbn U, (alk. paper): DM ISBN (alk. paper: U.S.) 1. Ultraviolet spectroscopy. I. Title. QD96.U4P ' dc This work is subject to copyright. All rights are reserved, whether the whole or part of the material is concerned, specifically the rights of translation, reprinting, reuse of illustrations, recitation, broadcasting, reproduction on microfilm or in any other way, and storage in data banks. Duplication of this publication or parts thereof is permitted only under the provisions of the German Copyright Law of September 9, 1965, in its current version, and permission for use must always be obtained from Springer-Verlag. Violations are liable for prosecution under the German Copyright Law. Springer-Verlag Berlin Heidelberg 1992 Sotlcover reprint of the hardcover 1st edition 1992 The use of general descriptive names, registered names, trademarks, etc. in this publication does not imply, even in the absence of a specific statement, that such names are exempt from the relevant protective laws and regulations and therefore free for general use. lypesetting: K + V Fotosatz GmbH, Beerfelden 52/ Printed on acid-free paper

4 Preface UV-VIS spectroscopy is one of the oldest methods in molecular spectroscopy. The definitive formulation of the Bouguer-Lambert Beer law in 1852 created the basis for the quantitative evaluation of absorption measurements at an early date. This led firstly to colorimetry, then to photometry and finally to spectrophotometry. This evolution ran parallel with the development of detectors for measuring light intensities, i.e. from the human eye via the photoelement and photocell, to the photomultiplier and from the photographic plate to the present silicon-diode detector both of which allow simultaneous measurement of the complete spectrum. With the development of quantum chemistry, increasing attention was paid to the correlation between light absorption and the structure of matter with the result that in recent decades a number of excellent discussions of the theory of electronic spectroscopy (UV-VIS and luminescence sp,~ctroscopy) have been published. Consequently, this extremely ivteresting aspect of molecular spectroscopy has dominated the teaching of the subject both in my own lectures and those of others. However, it is often overlooked that, in addition to the theory, applications of spectroscopic methods are of particular interest to scientists. For this reason, a lecture series about electronic spectroscopy given in the Institute for Physical Chemistry at the Heinrich-Heine-University in Dusseldorf was supplemented by one about "UV-VIS spectroscopy and its applications". This formed the basis of the present book. UV-VIS spectroscopy owes its importance not least to its varied applications in chemistry, physics and biochemistry. This book aims to show how UV-VIS spectroscopy can be applied to analytical problems, to the investigation of chemical equilibria and to the kinetics of chemical reactions, including photokinetics. The theoretical section has been kept to a minimum since, as mentioned above, excellent discussions of such matters are available in the literature. The details of the equipment are also described very briefly because G. KortUm gave an outstanding discussion of this subject in volume II of the series "Anleitung fur die chemische Laboratoriumspraxis"; and its basic details still apply today. In addition to the applications, a number of UV-VIS spectroscopic techniques are discussed. However, in this case the selection has been influenced by the author's own interests. In order to obtain experimental examples, numerous measurements have been

5 VI Preface made which might also be set as practical work for students of advanced physical chemistry. I would like to thank my colleagues for making these measurements, and drawing the diagrams. The English translation of the second edition of this volume is due to the stimulating interest of the "Ultraviolet Spectrometry Group", London, to whom I am very grateful. Mrs. Charlotte Grinter undertook the translation with great interest and engagement, professionally supported by Dr. T. L. Threlfall and Dr. Grinter. I would like to express my sincere thanks to Mrs. Grinter and the colleagues mentioned above for their hard labors. A few additions have been made to the first edition, i.e. the brief section "Chemometrics" was added by the English colleagues, some figures have been changed, others are new and the cited literature has been updated where necessary. Here also the English colleagues proved to be very helpful for which I would like to express my thanks. Thanks are also due to Dr. Enders of the Springer-Verlag for his interest and support of the publication of the English edition. Dusseldorf, June 1992 HEINZ-HELMUT PERKAMPUS

6 Contents 1 Introduction Principles.... The Bouguer-Lambert-Beer Law and Its Practical Application.... Primary Photophysical Processes.... Vibrational Structure of Electronic Spectra 2.4 Electronic Spectra and Molecular Structure References Photometers and Spectrophotometers Photometers.... Spectrophotometers.... The Stray Light Error.... General Observations.... The Stray Light Error of Transmission and Absorbance and Its Measurement Light Sources for UV-VIS Spectroscopy References Analytical Applications of UV-VIS Spectroscopy Photometric Determination of a Single Substance Photometric Determination of Elements by Means of Complexing Agents.... Photometric Determination of Anions and Ammonia.... Photometric Water Analyses.... Photometric Determination of Organic Compounds.... Enzymatic Analysis and Enzyme Kinetics.... Multicomponent Analysis.... Basic Equations.... An Example of a Multicomponent Analysis.... Identification and Structure Determination

7 VIII.Contents 4.4 Chemometrics 75 References Recent Developments in UV-VIS Spectroscopy Dual-Wavelength Spectroscopy.... Derivative Spectroscopy.... Reflectance Spectroscopy.... Photoacoustic Spectroscopy.... Principles of PAS.... PAS Applications.... Luminescence-Excitation Spectroscopy References Investigation of Equilibria General Protolytic Equilibria; pk-values Complex-Forming Equilibria H-Bond Association EDA Complexes Metal Complexes.... References Investigation of the Kinetics of Chemical Reactions Fundamental Equations of Kinetics Introduction of Absorbance as a Measurement Parameter Classification of Other 'JYpes of Reaction nd Order Reactions rd Order Reactions Pseudo 1 st Order Reactions Consecutive Reactions Parallel Reactions The Number of Linearly Independent Partial Reactions Evaluation of Kinetic Measurements Examples Fast Reactions.... Flow Methods: The Stopped-Flow Technique.... Spectroscopic Relaxation Techniques

8 Contents IX Photo reactions.... Spectrometers for Kinetic Measurements.... Rapid Spectrometers.... FT-UV Spectrometers Diode Array Spectrometers Determination of the Spectra of Intermediates References Evaluation of UV-VIS Spectral Bands Oscillator Strength and Transition Moment Band Analysis Gaussian and Lorentzian Functions Application of Derivative Spectra Vibrational Structure References Index of lliustrated Absorption Spectra.... Subject Index

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