Handbook.of.Water.analysis.third.edition

THIRD EDITION

2014 by Taylor & Francis Group, LLC


THIRD EDITION

EDITED BY

Leo M. L. NolletL e e n S . P. D e G e l d e r

Boca Raton London New York

CRC Press is an imprint of theTaylor & Francis Group, an informa business


CRC PressTaylor & Francis Group6000 Broken Sound Parkway NW, Suite 300Boca Raton, FL 33487-2742 2014 by Taylor & Francis Group, LLCCRC Press is an imprint of Taylor & Francis Group, an Informa businessNo claim to original U.S. Government worksVersion Date: 20130614International 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 beenmade to publish reliable data and information, but the author and publisher cannot assume responsibility for the validity of all materials or the consequences of their use. The authors and publishers have attempted to trace the copyrightholders of all material reproduced in this publication and apologize to copyright holders if permission to publish in thisform has not been obtained. If any copyright material has not been acknowledged please write and let us know so we mayrectify in any future reprint.Except as permitted under U.S. Copyright Law, no part of this book may be reprinted, reproduced, transmitted, or utilized in any form by any electronic, mechanical, or other means, now known or hereafter invented, including photocopying, microfilming, and recording, or in any information storage or retrieval system, without written permission from thepublishers.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. Fororganizations 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 foridentification and explanation without intent to infringe.Visit the Taylor & Francis Web site athttp://www.taylorandfrancis.comand the CRC Press Web site athttp://www.crcpress.com

ContentsPreface....................................................................................................................................................... ixEditors........................................................................................................................................................ xiContributors.............................................................................................................................................xiii

Section I Sampling and Data Treatment Methods 1. Sampling Methods in Surface Waters............................................................................................. 3Munro Mortimer, Jochen F. Mller, and Matthias Liess 2. Methods of Treatment of Data....................................................................................................... 47Riccardo Leardi

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

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

Section IV Analysis of Biological Parameters 5. Bacteriological Analysis of Water.................................................................................................115Paulinus Chigbu and Salina Parveen 6. Marine Toxins Analysis.................................................................................................................153Luis M. Botana, A. Alfonso, M. R. Vieytes, N. Vilario, A. M. Botana, C.Louzao,andC.Vale 7. Algal Analysis.................................................................................................................................163Leonardo Rubi Rrig

Section V Halogens, N-Compounds, and Phosphates 8. Halogens..........................................................................................................................................189Gza Nagy and Livia Nagy 9. Analysis of Sulfur Compounds in Water.................................................................................... 233Leo M. L. Nolletv 2014 by Taylor & Francis Group, LLC

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Contents

10. Determination of Ammonia in Water Samples.......................................................................... 249Juliana Antunes Galvo, Alexandre Matthiensen, Marlia Oetterer, Y. Moliner-Martnez,R.A.Gonzalez-Fuenzalida, M. Muoz-Ortuo, R. Herrez-Hernndez, J. Verd-Andrs,C.Molins-Legua, and P. Campns Falc11. Nitrites and Nitrates...................................................................................................................... 283Adnan Aydn12. Phosphates in Aquatic Systems.................................................................................................... 327Alexandre Matthiensen, Juliana Antunes Galvo, and Marlia Oetterer

Section VI Cyanides, Asbestos, Metals, and Si-Compounds13. Cyanides......................................................................................................................................... 365Leo M. L. Nollet14. Asbestos in Water.......................................................................................................................... 379James S. Webber15. Heavy Metals, Major Metals, Trace Elements........................................................................... 385Jorge E. Marcovecchio, Sandra E. Bott, Claudia E. Domini, and Rubn H. Freije16. Determination of Silicon and Silicates.........................................................................................435Salah M. Sultan

Section VII Organic Parameters17. Main Parameters and Assays Involved with the Organic Pollution of Water........................ 459Lorena Vidal, Claudia E. Domini, and Antonio Canals18. Determination of Organic Nitrogen in the AquaticEnvironment........................................... 493Juliana Antunes Galvo, Alexandre Matthiensen, and Marlia Oetterer19. Determination of Urea in Aquatic Samples.................................................................................511Juliana Antunes Galvo, Alexandre Matthiensen, and Marlia Oetterer20. Organic Acids.................................................................................................................................521Mercedes Gallego Fernndez, Evaristo Ballesteros Tribaldo, and Beatriz Jurado Snchez21. Determination of Volatile Organic Compounds inWater........................................................ 549Ivn P. Romn Falc and Marta Nogueroles Moya

Section VIII Phenolic and Humic Compounds22. Determination of Phenolic Compounds in Water.......................................................................613Leo M. L. Nollet23. Characterization of Humic Matter.............................................................................................. 647Leo M. L. Nollet


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Section IX Residues of Pesticides24. Determination of Pesticides in Water.......................................................................................... 665Evaristo Ballesteros Tribaldo25. Analysis of Herbicide and Fungicide Residues in Waters......................................................... 697N. Sridhara Chary, Maria Jose Gmez Ramos, and Amadeo R. Fernndez-Alba

Section X Residues of PCBs, PCDDs, PCDFS, and PAHs26. Analysis of PCBs in Waters.......................................................................................................... 765L. Bartolom, O. Zuloaga, and N. Etxebarria27. PCDDs and PCDFs....................................................................................................................... 789Luigi Turrio-Baldassarri, Paola Pettine, and Laura Achene28. Polynuclear Aromatic Hydrocarbons.......................................................................................... 807Chimezie Anyakora

Section XI Surfactants and Petroleum Hydrocarbon Analysis29. Surfactants..................................................................................................................................... 825Eva Pocurull and Rosa Maria Marc30. Petroleum Hydrocarbon Analysis............................................................................................... 845Ivn P. Romn Falc

Section XII EDCs and Residues of Plastics31. Endocrine-Disrupting Chemicals, Pharmaceuticals, and Personal Care Products............... 871Dimitra A. Lambropoulou and Eleni Evgenidou32. Residues of Plastics........................................................................................................................917Dimitra A. Lambropoulou and Eleni EvgenidouIndex....................................................................................................................................................... 943



PrefaceThe Handbook of Water Analysis, Third Edition, strives to provide the most comprehensive texta vailable in terms of the physicochemical and biological properties and analysis techniques of all typesof water.Organized in sections, most chapters cover the physical, chemical, and other relevant properties ofa 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 stillfrequently in use are compared to recently developed protocols, and an outlook is provided on futuretrends. Figures are incorporated to provide procedure flow charts and schematics concerning samplingor analytical devices. Numerous tables categorizing methods according to type of component, origin ofthe water sample, parameters and procedures used, and application range, facilitate the search for furtherreferences.Section I of the book lays out two crucial aspects besides the actual analysis procedures. Sound scientific investigation starts with a sampling strategy designed to capture the real-world situation as closelyas 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 presentsnew techniques for their determination.Section III regarding organoleptical analysis of water acknowledges that ultimately the consumers ofdrinking 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 marinetoxins.Sections V through XII encompass harmful or toxic components originating from domestic, agricultural, 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. Organiccompounds comprise organic nitrogen and acids, volatile and phenolic compounds, and humic matter. 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 micropollutants, such as endocrine disrupting compounds, pharmaceutical and personal care products and plasticresidues.This book aims to be a reference work for anybody learning about or carrying out water analysis, fromundergraduate and graduate students to scientific researchers and technicians in academic, governmental, industrial, or nonprofit sectors.All contributors are international experts in their field of water analysis, whom we would like to thankcordially for all their efforts.This book is dedicated to three granddaughters, Fara, Fleur, and Kato, and two grandsons Naut andRoel and two daughters, Hanne and Mona, for whom we wish that they can always enjoy fresh, cleanwater 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


EditorsLeo M. L. Nollet received an MS (1973) and a PhD (1978) in biology from the Katholieke UniversiteitLeuven, Belgium. Dr. Nollet is the editor and associate editor of numerous books. He edited for MarcelDekker, New Yorknow CRC Press of Taylor & Francis Groupthe first, second, and third editions ofFood Analysis by HPLC and Handbook of Food Analysis. The last edition is a three-volume book. Healso edited the Handbook of Water Analysis (first and second editions) and Chromatographic Analysisof the Environment, third edition (CRC Press).With F. Toldr he coedited two books published in 2006 and 2007: Advanced Technologies for MeatProcessing (CRC Press) and Advances in Food Diagnostics (Blackwell Publishingnow Wiley). WithM. Poschl he coedited Radionuclide Concentrations in Foods and the Environment also published in2006 (CRC Press).Dr. Nollet coedited several books with Y. H. Hui and other colleagues such as the Handbook ofFood Product Manufacturing (Wiley, 2007), Handbook of Food Science, Technology and Engineering(CRC Press, 2005), Food Biochemistry and Food Processing, first and second editions (BlackwellPublishingWiley, 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 (BlackwellPublishingWiley, 2007 and 2012).From 2008 to 2011 he published five volumes with F. Toldr in animal productsrelated books:Handbook of Muscle Foods Analysis, Handbook of Processed Meats and Poultry Analysis, Handbook ofSeafood and Seafood Products Analysis, Handbook of Dairy Foods Analysis, and Handbook ofAnalysisofEdibleAnimal By-Products. Also in 2011 with F. Toldr he coedited two volumes for CRC Press:Safety Analysis of Foods of Animal Origin and Sensory Analysis of Foods of Animal Origin. In 2012Nollet and Toldr published the Handbook of Analysis of Active Compounds in Functional Foods.Coediting with Hamir Rathore, the book Handbook of Pesticides: Methods of Pesticides ResiduesAnalysis 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 biotechnology at the Faculty of Bioscience Engineering of Ghent University, Belgium. Her main researchinterests include applied microbiology, microbial ecology, biodegradation and biological waste watertreatment. She received her MS in bioengineering (2002) from the University of Ghent, Ghent, Belgiumand her PhD in biology (2006) from the University of Idaho, Moscow, USA, and is the author or coauthorof several peer-reviewed articles and conference abstracts.

xi 2014 by Taylor & Francis Group, LLC


Contributors

Laura AcheneIstituto Superiore di SanitRome, ItalyA. AlfonsoDepartment of PharmacologyCampus de Lugo, USCLugo, Spain

Antonio CanalsDepartamento de Qumica AnalticaNutricin y Bromatologa e InstitutoUniversitario de MaterialesUniversidad de AlicanteAlicante, Spain

Jorge S. AlvaradoEnvironmental Science DivisionArgonne National LaboratoryArgonne, Illinois

N. Sridhara CharyIMDEA-Water (Madrid Institute for AdvancedStudies-Water)Cientifico de la Universidad de AlcalaAlcal de HenaresMadrid, Spain

Chimezie AnyakoraDepartment of Pharmaceutical ChemistryUniversity of LagosLagos, Nigeria

Paulinus ChigbuDepartment of Natural SciencesUniversity of Maryland Eastern ShorePrincess Anne, Maryland

Adnan AydnDepartment of ChemistryMarmara UniversityIstanbul, Turkey

Claudia E. DominiDepartamento de QumicaUniversidad Nacional del SurBaha Blanca, Argentina

L. BartolomGeneral Research ServiceUniversity of the Basque Country (UPV/EHU)Bizkaia, Spain

N. EtxebarriaDepartment of Analytical ChemistryUniversity of the Basque Country(UPV/EHU)Biscay (Basque Country), Spain

A. M. BotanaDepartment of Analytical ChemistryCampus de Lugo, USCLugo, SpainLuis M. BotanaDepartment of PharmacologyCampus de Lugo, USCLugo, SpainSandra E. BottArea de Oceanografia QuimicaInstituto Argentino de Oceanografia(IADO-CONICET/UNS)Casilla de CorreoBahia Blanca, Argentina

Eleni EvgenidouDepartment of ChemistryAristotle University of ThessalonikiThessaloniki, GreeceIvn P. Romn FalcDepartment of Analytical Chemistry andFoodSciencesUniversity of AlicanteAlicante, SpainP. Campns FalcDepartamento de Qumica AnalticaUniversitat de ValenciaValencia, Spainxiii


xivMercedes Gallego FernndezDepartment of Analytical ChemistryUniversity of CrdobaCrdoba, SpainAmadeo R. Fernndez-AlbaIMDEA-Water (Madrid Institute forAdvancedStudies-Water)Cientifico de la Universidad de AlcalaAlcal de HenaresMadrid, SpainandPesticide Residue Research GroupUniversity of AlmeraAlmera, SpainRubn H. FreijeArea de Oceanografia QuimicaInstituto Argentino de Oceanografia(IADO-CONICET/UNS)Casilla de CorreoBahia Blanca, ArgentinaJuliana Antunes GalvoDepartment of Agri-Food IndustryUniversity of So PauloSo Paulo, Brazil

ContributorsMatthias LiessDepartment of System-EcotoxicologyUFZ-Helmholtz-Zentrum fr UmweltforschungGmbHLeipzig, DeutschlandC. LouzaoDepartment of PharmacologyCampus de Lugo, USCLugo, SpainRosa Maria MarcDepartment of Analytical Chemistry andOrganic ChemistryUniversitat Rovira i VirgiliTarragona, SpainJorge E. MarcovecchioArea de Oceanografia QuimicaInstituto Argentino de Oceanografia(IADO-CONICET/UNS)Casilla de CorreoBahia Blanca, Argentina

R. A. Gonzalez-FuenzalidaDepartamento de Qumica AnalticaUniversitat de ValenciaValencia, Spain

Alexandre MatthiensenDepartment of Agri-Food IndustryUniversity of So PauloSo Paulo, BrazilandEmbrapa-Brazilian Agricultural ResearchCorporationEmbrapa Swine and PoultrySanta Catarina, Brazil

R. Herrez-HernndezDepartamento de Qumica AnalticaUniversitat de ValenciaValencia, Spain

Abdul MohemanDepartment of ChemistryAligarh Muslim UniversityAligarh, India

Musawwer KhanDepartment of ChemistryAligarh Muslim UniversityAligarh, IndiaDimitra A. LambropoulouDepartment of ChemistryAristotle University of ThessalonikiThessaloniki, GreeceRiccardo LeardiDepartment of PharmacyUniversity of GenovaGenova, Italy


Y. Moliner-MartnezDepartamento de Qumica AnalticaUniversitat de ValenciaValencia, SpainC. Molins-LeguaDepartamento de Qumica AnalticaUniversitat de ValenciaValencia, SpainMunro MortimerNational Research Centre for EnvironmentalToxicologyThe University of QueenslandBrisbane, Australia

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ContributorsMarta Nogueroles MoyaDepartment of Analytical Chemistry and FoodSciencesUniversity of AlicanteAlicante, SpainJochen F. MllerNational Research Centre for EnvironmentalToxicologyThe University of QueenslandBrisbane, AustraliaM. Muoz-OrtuoDepartamento de Qumica AnalticaUniversitat de ValenciaValencia, Spain

Maria Jose Gmez RamosIMDEA-Water (Madrid Institute forAdvancedStudies-Water)Cientifico de la Universidad de AlcalaAlcal de HenaresMadrid, SpainandPesticide Residue Research GroupUniversity of AlmeraAlmera, SpainLeonardo Rubi RrigDepartment of BotanyFederal University of Santa CatarinaSanta Catarina, Brazil

Gza NagyDepartment of General and PhysicalChemistryUniversity of PcsPcs, Hungary

Beatriz Jurado SnchezDepartment of Analytical ChemistryUniversity of CrdobaCrdoba, Spain

Livia NagyDepartment of General and PhysicalChemistryUniversity of PcsPcs, Hungary

K. S. SiddiqiDepartment of ChemistryAligarh Muslim UniversityAligarh, India

Leo M. L. Nollet (Retired)University College GhentGent, Belgium

Salah M. SultanSamf Pharmaceutical Co, WLLTubli, Bahrain

Marlia OettererDepartment of Agri-Food IndustryUniversity of So PauloSo Paulo, Brazil

Evaristo Ballesteros TribaldoDepartment of Physical and AnalyticalChemistryUniversity of JanJan, Spain

Salina ParveenDepartment of Agriculture, Food and ResourceSciencesUniversity of Maryland Eastern ShorePrincess Anne, Maryland

Luigi Turrio-BaldassarriIstituto Superiore di SanitRome, Italy

Paola PettineIstituto Superiore di SanitRome, Italy

C. ValeDepartment of PharmacologyCampus de Lugo, USCLugo, Spain

Eva PocurullDepartment of Analytical Chemistry andOrganic ChemistryUniversitat Rovira i VirgiliTarragona, Spain 2014 by Taylor & Francis Group, LLC

J. Verd-AndrsDepartamento de Qumica AnalticaUniversitat de ValenciaValencia, Spain

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Contributors

Lorena VidalDepartamento de Qumica AnalticaUniversidad de AlicanteAlicante, Spain

James S. WebberWadworth CenterNew York State Department of HealthAlbany, New York

M. R. VieytesDepartment of PhysiologyCampus de Lugo, USCLugo, Spain

O. ZuloagaDepartment of Analytical ChemistryUniversity of the Basque Country(UPV/EHU)Biscay (Basque Country), Spain

N. VilarioDepartment of PharmacologyCampus de Lugo, USCLugo, Spain


Section I

Sampling and Data TreatmentMethods


1Sampling Methods in Surface WatersMunro Mortimer, Jochen F. Mller, and Matthias LiessContents1.1 Introduction....................................................................................................................................... 41.2 General Aspects of Sampling and Sample Handling....................................................................... 51.2.1 Initial Considerations........................................................................................................... 51.2.2 Spatial Aspects..................................................................................................................... 61.2.3 Temporal Aspects................................................................................................................. 61.2.4 Number of Samples.............................................................................................................. 71.2.5 Sample Volume..................................................................................................................... 71.2.6 Storage and Conservation..................................................................................................... 71.2.6.1 Contamination...................................................................................................... 71.2.6.2 Loss....................................................................................................................... 81.2.6.3 Sorption................................................................................................................. 81.2.6.4 Recommended Storage......................................................................................... 91.2.6.5 Quality Control in Water Sampling.....................................................................161.3 Sampling Strategies for Different Ecosystems................................................................................161.3.1 Lakes and Reservoirs..........................................................................................................161.3.2 Streams and Rivers..............................................................................................................171.3.2.1 Location of Sampling within the Stream.............................................................171.3.2.2 Description of the Longitudinal Gradient...........................................................181.3.2.3 Temporal Changes of Water Quality...................................................................181.3.2.4 Using Sediments to Integrate over Time............................................................ 191.3.3 Estuarine and Marine Environments................................................................................. 191.3.4 Urban Areas........................................................................................................................ 201.3.5 Wastewater Systems........................................................................................................... 211.4 Sampling Equipment....................................................................................................................... 221.4.1 General Comments............................................................................................................. 221.4.2 Manual Sampling Systems................................................................................................. 221.4.2.1 Simple Sampler for Shallow Water..................................................................... 221.4.2.2 Sampler for Large Quantities in Shallow Water................................................. 221.4.2.3 Simple Sampler for Deepwater........................................................................... 221.4.2.4 Deepwater Sampler (Not Adding Air to the Sample)......................................... 231.4.2.5 Deepwater Sampler for Trace Elements (Allowing Air to MixwiththeSample)................................................................................................. 231.4.3 Systems for Sampling the Benthic Boundary Layer at Different Depths.......................... 261.4.3.1 Deepwater (>50m).............................................................................................. 261.4.3.2 Shallow Water (

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Handbook.of.Water.analysis.third.edition