Instrumental Multi Element Chemical Analysis
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Instrumental Multi Element Chemical Analysis


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Instrumental Multi-Element Chemical Analysis 
Instrumental Multi-Element 
Chemical Analysis 
Edited by 
Z.B. ALF ASSI 
Department of Nuclear Engineering 
Ben-Gurion University of the Negev 
Beer-Sheeva 
Israel 
SPRINGER-SCIENCE+BUSINESS MEDIA, B.V. 
Library of Congress Catalog Card number: 98-66852 
ISBN 978-94-010-6078-3 ISBN 978-94-011-4952-5 (eBook) 
DOI 10.1007/978-94-011-4952-5 
Printed an acid-free paper 
AII Rights Reserved 
© 1998 Springer Science+Business Media Dordrecht 
Originally pubIished by Kluwer Academic PubIishers in 1998 
No part of the material protected by this copyright notice may be reproduced or 
utilized in any form or by any means, electronic or mechanical, 
incIuding photocopying, recording, or by any information storage and 
retrieval system, without prior permis sion from the copyright owner. 
Typeset in 10/12pt Times by AFS Image Setters Ltd, Glasgow 
to Sabina 
with love 
Contents 
List of contributors 
Preface 
1 
2 
3 
4 
Preparation of samples 
Z.B. Alfassi and S. Felix 
1.1 Introduction 
1.2 Dissolution of geological and environmental inorganic samples 
1.3 Dissolution of biological (organic) material 
1.4 Contamination from reagents and equipment 
References 
Separation and preconcentration of trace inorganic elements 
Z.B. Alfassi 
2.1 Introduction 
2.2 Precipitation 
2.3 Separation and preconcentration of trace elements by columns 
(ion exchange and sorption) 
2.4 Preconcentration of trace elements by solvent extraction 
2.5 Preconcentration by formation of volatile compounds 
2.6 Electrochemical preconcentration 
References 
Quality assurance, control and assessment 
Z.B. Alfassi 
3.1 Introduction 
3.2 Quality assessment 
3.3 Statistical methods 
3.4 Significance tests 
3.5 Errors in instrumental analysis - calibration lines 
References 
Activation analysis 
M.D. Glascock 
4.1 Introduction 
4.2 Nuclear structure 
4.3 Nuclear reactions 
4.4 Decay rates 
4.5 Irradiation sources 
4.6 Detection and measurement of radiation 
4.7 Activation analysis techniques 
4.8 Special activation analysis methods 
4.9 Exercises and solutions 
References 
xi 
xiii 
1 
I 
2 
5 
15 
17 
19 
19 
20 
30 
43 
49 
51 
53 
55 
55 
56 
56 
62 
81 
92 
93 
93 
94 
98 
105 
112 
115 
127 
141 
146 
149 
Vlll CONTENTS 
5 Inductively coupled plasma optical emission and mass spectrometry 151 
N. De Silva and D.C. Gregoire 
6 
7 
8 
9 
5.1 Inductively coupled plasma as an analytical source 
5.2 Inductively coupled plasma optical emission spectrometry 
5.3 Inductively coupled plasma mass spectrometry 
5.4 Sample introduction 
References 
Electroanalytical methods 
P.e. Hauser 
6.1 Introduction 
6.2 Fundamentals 
6.3 Potentiometry 
6.4 Conductometry 
6.5 Electrogravimetry and coulometry 
6.6 Voltammetry and amperometry 
References 
Atomic absorption spectrometry 
I.Z. Pelly 
7.1 Introduction 
7.2 Theory 
7.3 Major components and instrument types 
7.4 Atomization 
7.5 Hydride generation 
7.6 Interferences 
7.7 Instrumental background corrections 
7.8 Modifiers, standards and chemicals 
7.9 Sample preparation and automation 
References 
X-ray fluorescence analysis 
P. Wobrauschek, P. Kregsamer and M. Mantler 
8.1 Introduction 
8.2 Wavelength- and energy-dispersive XRF 
8.3 X-ray tubes and radioisotope sources 
8.4 Methods of quantitative analysis 
8.5 Scattered radiation 
8.6 Electron probe micro-analysis 
8.7 Other XRF techniques 
8.8 Examples 
8.9 Appendix 
References 
Analysis of ions using high-performance liquid chromatography 
S. Levin 
9.1 What is ion chromatography? 
9.2 Fundamentals of the chromatographic process 
9.3 Principles of the separation 
9.4 Types of stationary phases 
9.5 Properties of mobile phases 
9.6 Ion suppression in ion chromatography 
9.7 Detection in ion chromatography 
9.8 Applications - summary 
References 
151 
156 
168 
192 
199 
201 
201 
203 
214 
233 
236 
239 
250 
251 
251 
256 
257 
269 
282 
283 
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348 
351 
352 
357 
359 
369 
375 
376 
10 Scattering methods 
E. Rauhala 
10.1 Introduction 
CONTENTS 
10.2 Theoretical considerations 
10.3 The experimental arrangement 
10.4 Spectrum analysis 
10.5 Numerical methods 
10.6 Applications to elemental analysis 
References 
11 Elemental analysis of surfaces 
M. Polak 
IX 
379 
379 
382 
404 
407 
426 
427 
435 
438 
11.1 Introduction: overview of surface phenomena and major techniques 438 
11.2 Auger electron spectroscopy and X-ray photoelectron spectroscopy 441 
11.3 Secondary-ion mass spectrometry 471 
11.4 Comparative evaluation of the performance of the three techniques 484 
11.5 Summary 489 
References 490 
Index 493 
Contributors 
Prof. Z.B. Alfassi 
Prof. N. De Silva 
S.Felix 
Dr M.D. Glascock 
Dr D.e. Gregoire 
Prof. P.e. Hauser 
Dr P. Kregsamer 
Dr S. Levin 
Prof. M. Mantler 
Prof. I,.Z. Pelly 
Prof. M. Polak 
Department of Nuclear Engineering, Ben-Gurion 
University of the Negev, Beer-Sheeva 84102, 
Israel 
Department of Chemistry, Carleton University, 
Ottawa, Ontario, Canada KIS 5B6 
Unit for Characterization of Materials, Institute 
for Applied Research, Ben-Gurion University of 
the Negev, Beer-Sheeva 84105, Israel 
Research Reactor Center, University of 
Missouri, Columbia, MO 65211, USA 
Geological Survey of Canada, 601 Booth Street, 
Ottawa, Ontario, Canada KIA OE8 
Department of Chemistry, University of Basel, 
Spitalstrasse 51, 5046 Basel, Switzerland 
Atominstitut der Osterreichischen Universitaten, 
Schiittelstrasse 115, A-I020 Wien, Austria 
Medtechnica, Efal St. 5 Kiriat Arie, Petach 
Tikva 49511, Israel 
Institut fUr Angewandte und Technische Physik, 
Technische Universtitat Wien, Wiedner 
Hauptstrasse 8-10, A-I040 Wien, Austria 
Department of Geological and Environmental 
Sciences, Ben-Gurion University of the Negev, 
Beer-Sheeva 84105, Israel 
Department of Materials Engineering, Ben-
Gurion University of the Negev, Beer-Sheeva 
84105, Israel 
xii CONTRIBUTORS 
Prof. E. Rauhala Accelerator Laboratory, Department of Physics, 
PO Box 9, University of Helsinki, 00014 
Helsinki, Finland 
Prof. P. Wobrauschek Atominstitut der Osterreichischen Universitaten, 
Schiittelstrasse 115, A-l020 Vienna, Austria 
Preface 
Classical analytical methods such as gravimetry and absorption of special 
titrimetry complexes remain in use in many laboratories and are still widely 
taught in first-year analytical courses. These courses and particularly the 
laboratory experiments attached to them are excellent for training students 
in the work of an experimental chemist. These methods are also still the main 
ones when very high analysis of the major elements of a matrix is required. 
However, most analyses are now performed by instrumental analysis, and a 
rough estimate is that at least 99% of current analytical measurements are 
done by instrumental techniques such as emission and absorption spec-
trometry, electrochemical methods, mass spectrometry, various methods of 
gas and liquid chromatography or radiochemical methods. Several proper-
ties common to many of these methods are the reason for the shift from 
classical analytical chemistry to modem instrumental methods. 
\u2022 Sensitivity Instrumental methods can reach detection limits undreamed 
of in classical methods. These higher sensitivities completely change 
the range of what is called trace elements. While not so long ago 
trace elements were those at a concentration of parts per thousand 
(permill, 10-3), nowadays instrumental measurements of parts per 
million