Problems of Instrumental Analytical Chemistry: A Hands-On Guide

478 Pages·2017·41.969 MB·English

by  JM Andrade-Garda, A Carlosena-Zubieta, MP Gómez-Carracedo, MA Maestro-Saavedra, MC Prieto-Blanco, RM Soto-Ferreiro

Problems of
Instrumental
Analytical Chemistry

A Hands-On Guide
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Problems of Instrumental Analytical Chemistry: A Hands-On Guide
by JM Andrade-Garda, A Carlosena-Zubieta, MP Gómez-Carracedo,
MA Maestro-Saavedra, MC Prieto-Blanco and RM Soto-Ferreiro
Essential Textbooks in Chemistry
Problems of
Instrumental
Analytical Chemistry

A Hands-On Guide
JM Andrade-Garda • A Carlosena-Zubieta
MP Gómez-Carracedo • MA Maestro-Saavedra
MC Prieto-Blanco • RM Soto-Ferreiro
University of A Coruña, Spain
World Scientific
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Library of Congress Cataloging-in-Publication Data
Names: Andrade-Garda, José Manuel.
Title: Problems of instrumental analytical chemistry : a hands-on guide / by J.M. Andrade-Garda
(University of A Coruña, Spain) [and five others].
Description: New Jersey : World Scientific, 2016. | Series: Essential textbooks in chemistry
Identifiers: LCCN 2016036786| ISBN 9781786341792 (hc : alk. paper) |
ISBN 9781786341808 (pbk : alk. paper)
Subjects: LCSH: Chemistry, Analytic. | Spectrum analysis. | Chromatographic analysis.
Classification: LCC QD75.22 .P76 2016 | DDC 543--dc23
LC record available at https://lccn.loc.gov/2016036786
British Library Cataloguing-in-Publication Data
A catalogue record for this book is available from the British Library.
Copyright © 2017 by World Scientific Publishing Europe Ltd.
All rights reserved. This book, or parts thereof, may not be reproduced in any form or by any means,
electronic or mechanical, including photocopying, recording or any information storage and retrieval
system now known or to be invented, without written permission from the Publisher.
For photocopying of material in this volume, please pay a copying fee through the Copyright Clearance
Center, Inc., 222 Rosewood Drive, Danvers, MA 01923, USA. In this case permission to photocopy
is not required from the publisher.
Desk Editors: Herbert Moses/Mary Simpson
Typeset by Stallion Press
Email: [email protected]
Printed in Singapore
PREFACE
Thattheworldischangingveryfastisanunderstatementinthedigi-
talage.Howthisshouldtranslateintohighereducationandteaching,
however, is a subject which is up for much debate. Universities
are responsible for training students in the development of their
professional careers, however without a doubt it is impossible to
teacheveryconceptwithintheshortamountoftimeallocatedtoeach
course.Theincreasingcomplexityofthesciencesmeansthatstudents
need to understand deeper and greater fundamental concepts in
order to have the confidence to face different working environments
in laboratories, hospitals and offices. Their backgrounds and basic
knowledge must be sound and deeply rooted to enable the ability of
applying concepts and ideas to new situations.
The strongest recent effort undertaken by Europe to integrate
higher education has been the so-called European Credit Transfer
and Accumulation System (ECTS). This is a tool of the European
Higher Education Area (EHEA) to make courses more transparent
and thus help to enhance the quality of higher education. From a
pragmatic viewpoint (which, unfortunately, we feel has been the
mainunderlyingreason),itisawaytohomogenizeuniversitydegrees
throughout the European Union in order to get a free exchange of
professionals. In many countries (including Spain, Italy, France, and
Portugal), the ECTS system implied a (dramatic) reduction in the
v
vi Preface
time available for teaching and increased the requirement for the
student to implement individual training and study.
This sounds reasonable in theoretical terms but it is very hard
to achieve in practice. Students need to attend laboratory and
theoretical classes, develop oral presentation skills and find solutions
for numerical exercises for several subjects within the semester — a
difficult task for teachers confronted with less contact time. Teachers
are—somehow —forcedtoreducecontent onfundamentalconcepts
in order to includenew skills and updatedchapters for their subjects
within the time allocated. Impetus for learning therefore lies largely
with the student, a big ask when looking at the complexity and
level of knowledge needed to be able to understand even basic
theories.
Aconstantcommentinalmostevery highereducationconference
is the reference to the low level of background understanding of the
fundamentals of chemistry undergraduates demonstrate daily — this
begsthequestion ofatwhichpointandforwhatreason isthesystem
failing you, the student?
We identified a gap in current literature on analytical chemistry
whereby there was a lack of dedicated exercises for students to apply
what they had learnt. Feedback from you throughout teaching was
thatexamplesandinformationfoundinindividualstudywereuseful,
but did not provide enough opportunity for practice and further
learning. We as teachers attempted to provide in-class examples
and exercises, however time constraints and different learning needs
meant that these were not as useful as they could be outside the
classroom. We decided at that point to create a learning resource
which you could use during individual study to learn the basics of
instrumental analytical study — this book was conceived.
The first problem we faced was to limit its extent — we did not
want an overwhelming textbook full of incomprehensible equations.
The many instrumental techniques and possible content had to
be restricted somehow. We considered two issues: First, we knew
about very good books dealing with numerical exercises on the
electroanalyticalfields.Similarly,classicalmethods(suchastitimetry
or gravimetry) are very well treated in many general textbooks.
Preface vii
Accordingly, we could avoid considering these matters within the
first edition. We then decided to focus on exercises based on typical
instrumental analytical techniques, as they are considered in almost
every fundamentalundergraduatetrainingthroughoutEurope.With
this in mind, we started off on our task to write a clear, cohesive
textbook which is designed to be used in undergraduate study of
chemistry and the chemical sciences.
Thanks must be given here to Merlin Fox and Mary Simpson for
their kind help, their continuous supportand patience. The editorial
staff of World Scientific Publishing are also acknowledged for their
wonderful and professional work.
The chapters are organized so that a general review of the basic
concepts addressed are presented first. Here, general explanations,
equations and guidelines to study separate topics are given. Then, a
set of example questions are shown and solved in detail and, finally,
a set of exercises are presented, designed to test students’ learning.
A recommendation is in order just here. We strongly encourage
you to try to solve the numerical exercises before reading their
solutions.Youwilllearnmuchmoreeffectively. Insomeoccasions,we
know the exercises are particularly difficult, and hints are included
to help you solve them. We hope they are useful.
Last, although far from least, we would like to thank all students
thathavesufferedusthroughoutouryears’teaching.Weareproudto
see many of them in relevant and high profile positions. Sometimes
they visit us (or we visit them to ask for collaboration with the
university) and reflect on education in the sciences, and the learning
of young graduates. Time goes by ... for them as well as us (!)
and they hardly remember themselves as undergraduates in our
classrooms. They complain about the low background of young
graduates and encourage us to be less permissive. Yes, it is true
that university teachers should demand a minimum (unchanging)
backgroundonthedisciplinestheyteach.However,thisismoreeasily
said than done, particularly in this fast-changing environment.
We hope this textbook can help both us and undergraduates
to keep an eye on relevant issues that we should teach/learn. Who
knows, maybe even postgraduates can take advantage of exercises
viii Preface
for enhanced learning and/or on-the-job training of their staff. That
would be a marvelous use of this textbook they helped create.
To close this preface, the authors want to encourage readers of
this book to contact us if they detect errors or if they have a say on
particular sections. If you would like to pose a particular numerical
exercise because you feel it is relevant, or an explanation that would
help students, we would be delighted to include that contribution in
future versions (citing the source of course!)
Thanks to all and good luck!
JM Andrade, A Carlosena, MP Go´mez,
MA Maestro, MC Prieto and RM Soto
ABOUT THE AUTHORS
Jos´e Manuel Andrade-Garda is a full professor at the University
of A Corun˜a (Galicia, Spain) since 2011. He was in charge of
teaching different subjects on analytical chemistry since 1995. His
main interests are quality control and chemometrics, in particular,
multivariate regression and pattern recognition methods (either,
unsupervised and supervised). He works on infrared spectrometry
and atomic spectrometry. There, he applied both optimization
techniquesandmultivariateregressiontoolstocopewithspectraland
chemicalinterferencesinETAAS.Intheinfraredspectrometryarena,
he developed analytical methods for the petrochemical field. He
published around 100 papers in peer-reviewed journals, co-authored
12chapters ofbooksandedited twoeditionsofabookwiththeRSC.
Alatzne Carlosena-Zubieta is an associate professor of analytical
chemistry at the University of A Corun˜a, where she is in charge of
several subjects on analytical chemistry since 1994. She currently
works on atomic spectrometry, particularly quantitation of trace
metals in samples of environmental interest. She published many
papers on slurry-sampling ETAAS. There, robust analytical proto-
cols were developed based on multivariate chemometric optimization
methods (namely, experimental design and simplex optimization).
She published around 60 papers in peer-reviewed journals and
ix