THIRD EDITION

© 2014 by Taylor & Francis Group, LLC

 Downloaded by [103.225.208.1] at 23:01 12 February 2015

© 2014 by Taylor & Francis Group, LLC

 THIRD EDITION
Downloaded by [103.225.208.1] at 23:01 12 February 2015

EDITED BY
Leo M. L. Nollet
L e e n S . P. D e G e l d e r

Boca Raton London New York

CRC Press is an imprint of the

Taylor & Francis Group, an informa business

© 2014 by Taylor & Francis Group, LLC

Downloaded by [103.225.208.1] at 23:01 12 February 2015

CRC Press
Taylor & Francis Group
6000 Broken Sound Parkway NW, Suite 300
Boca Raton, FL 33487-2742
© 2014 by Taylor & Francis Group, LLC
CRC Press is an imprint of Taylor & Francis Group, an Informa business

No claim to original U.S. Government works

Version Date: 20130614

International Standard Book Number-13: 978-1-4398-8966-4 (eBook - PDF)

This book contains information obtained from authentic and highly regarded sources. Reasonable efforts have been
made to publish reliable data and information, but the author and publisher cannot assume responsibility for the valid-
ity of all materials or the consequences of their use. The authors and publishers have attempted to trace the copyright
holders of all material reproduced in this publication and apologize to copyright holders if permission to publish in this
form has not been obtained. If any copyright material has not been acknowledged please write and let us know so we may
rectify in any future reprint.

Except as permitted under U.S. Copyright Law, no part of this book may be reprinted, reproduced, transmitted, or uti-
lized in any form by any electronic, mechanical, or other means, now known or hereafter invented, including photocopy-
ing, microfilming, and recording, or in any information storage or retrieval system, without written permission from the
publishers.

For permission to photocopy or use material electronically from this work, please access www.copyright.com (http://
www.copyright.com/) or contact the Copyright Clearance Center, Inc. (CCC), 222 Rosewood Drive, Danvers, MA 01923,
978-750-8400. CCC is a not-for-profit organization that provides licenses and registration for a variety of users. For
organizations that have been granted a photocopy license by the CCC, a separate system of payment has been arranged.

Trademark Notice: Product or corporate names may be trademarks or registered trademarks, and are used only for
identification and explanation without intent to infringe.
Visit the Taylor & Francis Web site at
http://www.taylorandfrancis.com
and the CRC Press Web site at
http://www.crcpress.com
 Contents

Preface....................................................................................................................................................... ix
Editors........................................................................................................................................................ xi
Contributors.............................................................................................................................................xiii

Section I  Sampling and Data Treatment Methods

1. Sampling Methods in Surface Waters............................................................................................. 3
Munro Mortimer, Jochen F. Müller, and Matthias Liess
Downloaded by [103.225.208.1] at 23:01 12 February 2015

2. Methods of Treatment of Data....................................................................................................... 47

Riccardo Leardi

Section II  Radioanalytical Analysis

3. Radioanalytical Methodology for Water Analysis....................................................................... 79
Jorge S. Alvarado

Section III  Organoleptical Analysis

4. Organoleptical Methodology.........................................................................................................101
Abdul Moheman, Md. Musawwer Khan, and K. S. Siddiqi

Section IV  Analysis of Biological Parameters

5. Bacteriological Analysis of Water.................................................................................................115
Paulinus Chigbu and Salina Parveen

6. Marine Toxins Analysis.................................................................................................................153

Luis M. Botana, A. Alfonso, M. R. Vieytes, N. Vilariño, A. M. Botana, C. Louzao,
and C. Vale

7. Algal Analysis.................................................................................................................................163
Leonardo Rubi Rörig

Section V  Halogens, N-Compounds, and Phosphates

8. Halogens..........................................................................................................................................189
Géza Nagy and Livia Nagy

9. Analysis of Sulfur Compounds in Water.................................................................................... 233

Leo M. L. Nollet

v
© 2014 by Taylor & Francis Group, LLC
 vi Contents

10. Determination of Ammonia in Water Samples.......................................................................... 249

Juliana Antunes Galvão, Alexandre Matthiensen, Marília Oetterer, Y. Moliner-Martínez,
R. A. Gonzalez-Fuenzalida, M. Muñoz-Ortuño, R. Herráez-Hernández, J. Verdú-Andrés,
C. Molins-Legua, and P. Campíns Falcó

11. Nitrites and Nitrates...................................................................................................................... 283

Adnan Aydın

12. Phosphates in Aquatic Systems.................................................................................................... 327

Alexandre Matthiensen, Juliana Antunes Galvão, and Marília Oetterer

Section VI  Cyanides, Asbestos, Metals, and Si-Compounds

13. Cyanides......................................................................................................................................... 365
Downloaded by [103.225.208.1] at 23:01 12 February 2015

Leo M. L. Nollet

14. Asbestos in Water.......................................................................................................................... 379

James S. Webber

15. Heavy Metals, Major Metals, Trace Elements........................................................................... 385

Jorge E. Marcovecchio, Sandra E. Botté, Claudia E. Domini, and Rubén H. Freije

16. Determination of Silicon and Silicates.........................................................................................435

Salah M. Sultan

Section VII  Organic Parameters

17. Main Parameters and Assays Involved with the Organic Pollution of Water........................ 459
Lorena Vidal, Claudia E. Domini, and Antonio Canals

18. Determination of Organic Nitrogen in the Aquatic Environment........................................... 493

Juliana Antunes Galvão, Alexandre Matthiensen, and Marília Oetterer

19. Determination of Urea in Aquatic Samples.................................................................................511

Juliana Antunes Galvão, Alexandre Matthiensen, and Marília Oetterer

20. Organic Acids.................................................................................................................................521

Mercedes Gallego Fernández, Evaristo Ballesteros Tribaldo, and Beatriz Jurado Sánchez

21. Determination of Volatile Organic Compounds in Water........................................................ 549

Iván P. Román Falcó and Marta Nogueroles Moya

Section VIII  Phenolic and Humic Compounds

22. Determination of Phenolic Compounds in Water.......................................................................613
Leo M. L. Nollet

23. Characterization of Humic Matter.............................................................................................. 647

Leo M. L. Nollet

© 2014 by Taylor & Francis Group, LLC

 Contents vii

Section IX  Residues of Pesticides

24. Determination of Pesticides in Water.......................................................................................... 665
Evaristo Ballesteros Tribaldo

25. Analysis of Herbicide and Fungicide Residues in Waters......................................................... 697

N. Sridhara Chary, Maria Jose Gómez Ramos, and Amadeo R. Fernández-Alba

Section X  Residues of PCBs, PCDDs, PCDFS, and PAHs

26. Analysis of PCBs in Waters.......................................................................................................... 765
L. Bartolomé, O. Zuloaga, and N. Etxebarria

27. PCDDs and PCDFs....................................................................................................................... 789

Downloaded by [103.225.208.1] at 23:01 12 February 2015

Luigi Turrio-Baldassarri, Paola Pettine, and Laura Achene

28. Polynuclear Aromatic Hydrocarbons.......................................................................................... 807

Chimezie Anyakora

Section XI  Surfactants and Petroleum Hydrocarbon Analysis

29. Surfactants..................................................................................................................................... 825
Eva Pocurull and Rosa Maria Marcé

30. Petroleum Hydrocarbon Analysis............................................................................................... 845

Iván P. Román Falcó

Section XII  EDCs and Residues of Plastics

31. Endocrine-Disrupting Chemicals, Pharmaceuticals, and Personal Care Products............... 871
Dimitra A. Lambropoulou and Eleni Evgenidou

32. Residues of Plastics........................................................................................................................917

Dimitra A. Lambropoulou and Eleni Evgenidou

Index....................................................................................................................................................... 943

© 2014 by Taylor & Francis Group, LLC

 Downloaded by [103.225.208.1] at 23:01 12 February 2015

© 2014 by Taylor & Francis Group, LLC

 Preface

The Handbook of Water Analysis, Third Edition, strives to provide the most comprehensive text
a­ vailable in terms of the physicochemical and biological properties and analysis techniques of all types
of water.
Organized in sections, most chapters cover the physical, chemical, and other relevant properties of
a particular subset of water components, followed by a description of sampling, cleanup, extraction,
and derivatization procedures, and concluding with detection methods. Earlier techniques that are still
frequently in use are compared to recently developed protocols, and an outlook is provided on future
trends. Figures are incorporated to provide procedure flow charts and schematics concerning sampling
or analytical devices. Numerous tables categorizing methods according to type of component, origin of
Downloaded by [103.225.208.1] at 23:01 12 February 2015

the water sample, parameters and procedures used, and application range, facilitate the search for further
references.
Section I of the book lays out two crucial aspects besides the actual analysis procedures. Sound scien-
tific investigation starts with a sampling strategy designed to capture the real-world situation as closely
as possible, and ends with an adequate chemometrical and statistical treatment of the acquired data.
Section II summarizes health and environmental problems due to radionuclides in water and presents
new techniques for their determination.
Section III regarding organoleptical analysis of water acknowledges that ultimately the consumers of
drinking water have the final vote over its quality regarding odor, flavor, and color.
Water houses many organisms, of which the smallest may cause illness and produce toxic substances.
Section IV discusses bacteriological and algal analysis, as well as the occurrence and detection of marine
toxins.
Sections V through XII encompass harmful or toxic components originating from domestic, agricul-
tural, or industrial sources that can be found in different waters. Inorganic substances include nitrogen,
sulfur, phosphate, silica, and halogenated compounds, cyanides, (heavy) metals, and asbestos. Organic
compounds comprise organic nitrogen and acids, volatile and phenolic compounds, and humic mat-
ter. The main groups of anthropogenic polluting compounds are discussed: pesticides, PCBs, PCDDs,
PCDFS, PAHs, petroleum hydrocarbons, and surfactants.
Specific chapters in these sections are also dedicated to the challenging category of micropollut-
ants, such as endocrine disrupting compounds, pharmaceutical and personal care products and plastic
residues.
This book aims to be a reference work for anybody learning about or carrying out water analysis, from
undergraduate and graduate students to scientific researchers and technicians in academic, governmen-
tal, industrial, or nonprofit sectors.
All contributors are international experts in their field of water analysis, whom we would like to thank
cordially for all their efforts.
This book is dedicated to three granddaughters, Fara, Fleur, and Kato, and two grandsons Naut and
Roel and two daughters, Hanne and Mona, for whom we wish that they can always enjoy fresh, clean
water in their lifetime.

It is far more impressive when others discover your good qualities without your help.
— Judith Martin

ix
© 2014 by Taylor & Francis Group, LLC
 Downloaded by [103.225.208.1] at 23:01 12 February 2015

© 2014 by Taylor & Francis Group, LLC

 Editors

Leo M. L. Nollet received an MS (1973) and a PhD (1978) in biology from the Katholieke Universiteit
Leuven, Belgium. Dr. Nollet is the editor and associate editor of numerous books. He edited for Marcel
Dekker, New York—now CRC Press of Taylor & Francis Group—the first, second, and third editions of
Food Analysis by HPLC and Handbook of Food Analysis. The last edition is a three-volume book. He
also edited the Handbook of Water Analysis (first and second editions) and Chromatographic Analysis
of the Environment, third edition (CRC Press).
With F. Toldrá he coedited two books published in 2006 and 2007: Advanced Technologies for Meat
Processing (CRC Press) and Advances in Food Diagnostics (Blackwell Publishing—now Wiley). With
M. Poschl he coedited Radionuclide Concentrations in Foods and the Environment also published in
Downloaded by [103.225.208.1] at 23:01 12 February 2015

2006 (CRC Press).

Dr. Nollet coedited several books with Y. H. Hui and other colleagues such as the Handbook of
Food Product Manufacturing (Wiley, 2007), Handbook of Food Science, Technology and Engineering
(CRC Press, 2005), Food Biochemistry and Food Processing, first and second editions (Blackwell
Publishing—Wiley, 2006 and 2012), and Handbook of Fruits and Vegetable Flavors (Wiley, 2010).
He edited the Handbook of Meat, Poultry and Seafood Quality, first and second editions (Blackwell
Publishing—Wiley, 2007 and 2012).
From 2008 to 2011 he published five volumes with F. Toldrá in animal products–related books:
Handbook of Muscle Foods Analysis, Handbook of Processed Meats and Poultry Analysis, Handbook of
Seafood and Seafood Products Analysis, Handbook of Dairy Foods Analysis, and Handbook of Analysis
of Edible Animal By-Products. Also in 2011 with F. Toldrá he coedited two volumes for CRC Press:
Safety Analysis of Foods of Animal Origin and Sensory Analysis of Foods of Animal Origin. In 2012
Nollet and Toldrá published the Handbook of Analysis of Active Compounds in Functional Foods.
Coediting with Hamir Rathore, the book Handbook of Pesticides: Methods of Pesticides Residues
Analysis was marketed in 2009 and Pesticides: Evaluation of Environmental Pollution in 2012.
Other completed book projects are Food Allergens: Analysis, Instrumentation, and Methods with A.
van Hengel (CRC Press, 2011) and Analysis of Endocrine Compounds in Food (Wiley-Blackwell, 2011).

Leen S. P. De Gelder is a professor of microbiology, biochemical technology, and environmental bio-

technology at the Faculty of Bioscience Engineering of Ghent University, Belgium. Her main research
interests include applied microbiology, microbial ecology, biodegradation and biological waste water
treatment. She received her MS in bioengineering (2002) from the University of Ghent, Ghent, Belgium
and her PhD in biology (2006) from the University of Idaho, Moscow, USA, and is the author or coauthor
of several peer-reviewed articles and conference abstracts.

xi
© 2014 by Taylor & Francis Group, LLC
 Downloaded by [103.225.208.1] at 23:01 12 February 2015

© 2014 by Taylor & Francis Group, LLC

 Contributors

Laura Achene Antonio Canals

Istituto Superiore di Sanità Departamento de Química Analítica
Rome, Italy Nutrición y Bromatología e Instituto
Universitario de Materiales
A. Alfonso Universidad de Alicante
Department of Pharmacology Alicante, Spain
Campus de Lugo, USC
Lugo, Spain N. Sridhara Chary
Downloaded by [103.225.208.1] at 23:01 12 February 2015

IMDEA-Water (Madrid Institute for Advanced

Jorge S. Alvarado Studies-Water)
Environmental Science Division Cientifico de la Universidad de Alcala
Argonne National Laboratory Alcalá de Henares
Argonne, Illinois Madrid, Spain

Chimezie Anyakora Paulinus Chigbu

Department of Pharmaceutical Chemistry Department of Natural Sciences
University of Lagos University of Maryland Eastern Shore
Lagos, Nigeria Princess Anne, Maryland

Adnan Aydın Claudia E. Domini

Department of Chemistry Departamento de Química
Marmara University Universidad Nacional del Sur
Istanbul, Turkey Bahía Blanca, Argentina

L. Bartolomé N. Etxebarria
General Research Service Department of Analytical Chemistry
University of the Basque Country (UPV/EHU) University of the Basque Country
Bizkaia, Spain (UPV/EHU)
Biscay (Basque Country), Spain
A. M. Botana
Department of Analytical Chemistry Eleni Evgenidou
Campus de Lugo, USC Department of Chemistry
Lugo, Spain Aristotle University of Thessaloniki
Thessaloniki, Greece
Luis M. Botana
Department of Pharmacology Iván P. Román Falcó
Campus de Lugo, USC Department of Analytical Chemistry and
Lugo, Spain Food Sciences
University of Alicante
Sandra E. Botté Alicante, Spain
Area de Oceanografia Quimica
Instituto Argentino de Oceanografia P. Campíns Falcó
(IADO-CONICET/UNS) Departamento de Química Analítica
Casilla de Correo Universitat de Valencia
Bahia Blanca, Argentina Valencia, Spain

xiii
© 2014 by Taylor & Francis Group, LLC
 xiv Contributors

Mercedes Gallego Fernández Matthias Liess

Department of Analytical Chemistry Department of System-Ecotoxicology
University of Córdoba UFZ-Helmholtz-Zentrum für Umweltforschung
Córdoba, Spain GmbH
Leipzig, Deutschland
Amadeo R. Fernández-Alba
IMDEA-Water (Madrid Institute forAdvanced C. Louzao
Studies-Water) Department of Pharmacology
Cientifico de la Universidad de Alcala Campus de Lugo, USC
Alcalá de Henares Lugo, Spain
Madrid, Spain
and Rosa Maria Marcé
Pesticide Residue Research Group Department of Analytical Chemistry and
University of Almería Organic Chemistry
Almería, Spain Universitat Rovira i Virgili
Tarragona, Spain
Downloaded by [103.225.208.1] at 23:01 12 February 2015

Rubén H. Freije
Jorge E. Marcovecchio
Area de Oceanografia Quimica
Area de Oceanografia Quimica
Instituto Argentino de Oceanografia
Instituto Argentino de Oceanografia
(IADO-CONICET/UNS)
(IADO-CONICET/UNS)
Casilla de Correo
Casilla de Correo
Bahia Blanca, Argentina
Bahia Blanca, Argentina

Juliana Antunes Galvão Alexandre Matthiensen

Department of Agri-Food Industry
University of São Paulo
São Paulo, Brazil
R. A. Gonzalez-Fuenzalida
Departamento de Química Analítica
Universitat de Valencia
Valencia, Spain
Department of Agri-Food Industry
University of São Paulo
São Paulo, Brazil
and
Embrapa-Brazilian Agricultural Research
Corporation
Embrapa Swine and Poultry
Santa Catarina, Brazil

R. Herráez-Hernández Abdul Moheman

Departamento de Química Analítica Department of Chemistry
Universitat de Valencia Aligarh Muslim University
Valencia, Spain Aligarh, India

Y. Moliner-Martínez
Musawwer Khan
Departamento de Química Analítica
Department of Chemistry
Universitat de Valencia
Aligarh Muslim University
Valencia, Spain
Aligarh, India
C. Molins-Legua
Dimitra A. Lambropoulou Departamento de Química Analítica
Department of Chemistry Universitat de Valencia
Aristotle University of Thessaloniki Valencia, Spain
Thessaloniki, Greece
Munro Mortimer
Riccardo Leardi National Research Centre for Environmental
Department of Pharmacy Toxicology
University of Genova The University of Queensland
Genova, Italy Brisbane, Australia

© 2014 by Taylor & Francis Group, LLC

 Contributors xv

Marta Nogueroles Moya Maria Jose Gómez Ramos

Department of Analytical Chemistry and Food IMDEA-Water (Madrid Institute forAdvanced
Sciences Studies-Water)
University of Alicante Cientifico de la Universidad de Alcala
Alicante, Spain Alcalá de Henares
Madrid, Spain
Jochen F. Müller and
National Research Centre for Environmental Pesticide Residue Research Group
Toxicology University of Almería
The University of Queensland Almería, Spain
Brisbane, Australia
Leonardo Rubi Rörig
M. Muñoz-Ortuño
Department of Botany
Departamento de Química Analítica
Federal University of Santa Catarina
Universitat de Valencia
Santa Catarina, Brazil
Valencia, Spain
Downloaded by [103.225.208.1] at 23:01 12 February 2015

Géza Nagy Beatriz Jurado Sánchez

Department of General and Physical Department of Analytical Chemistry
Chemistry University of Córdoba
University of Pécs Córdoba, Spain
Pécs, Hungary

Livia Nagy K. S. Siddiqi

Department of General and Physical Department of Chemistry
Chemistry Aligarh Muslim University
University of Pécs Aligarh, India
Pécs, Hungary
Salah M. Sultan
Leo M. L. Nollet (Retired) Samf Pharmaceutical Co, WLL
University College Ghent Tubli, Bahrain
Gent, Belgium
Evaristo Ballesteros Tribaldo
Marília Oetterer
Department of Physical and Analytical
Department of Agri-Food Industry
Chemistry
University of São Paulo
University of Jaén
São Paulo, Brazil
Jaén, Spain
Salina Parveen
Department of Agriculture, Food and Resource Luigi Turrio-Baldassarri
Sciences Istituto Superiore di Sanità
University of Maryland Eastern Shore Rome, Italy
Princess Anne, Maryland
C. Vale
Paola Pettine
Department of Pharmacology
Istituto Superiore di Sanità
Campus de Lugo, USC
Rome, Italy
Lugo, Spain
Eva Pocurull
Department of Analytical Chemistry and J. Verdú-Andrés
Organic Chemistry Departamento de Química Analítica
Universitat Rovira i Virgili Universitat de Valencia
Tarragona, Spain Valencia, Spain

© 2014 by Taylor & Francis Group, LLC

 xvi Contributors

Lorena Vidal James S. Webber

Departamento de Química Analítica Wadworth Center
Universidad de Alicante New York State Department of Health
Alicante, Spain Albany, New York

M. R. Vieytes O. Zuloaga
Department of Physiology Department of Analytical Chemistry
Campus de Lugo, USC University of the Basque Country
Lugo, Spain (UPV/EHU)
Biscay (Basque Country), Spain
N. Vilariño
Department of Pharmacology
Campus de Lugo, USC
Lugo, Spain
Downloaded by [103.225.208.1] at 23:01 12 February 2015

© 2014 by Taylor & Francis Group, LLC