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Analysis of Seawater a Guide for the Analytical and Environmental Chemist T.R Analysis of Seawater A Guide for the Analytical and Environmental Chemist T.R. Crompton Analysis of Seawater A Guide for the Analytical and Environmental Chemist With 48 Figures and 45 Tables 123 T.R. Crompton Hill Cottage (Bwthyn Yr Allt) Anglesey, Gwynedd United Kingdom Library of Congress Control Number: 2005929412 ISBN-10 3-540-26762-X Springer Berlin Heidelberg New York ISBN-13 978-3-540-26762-1 Springer Berlin Heidelberg New York DOI 10.1007/b95901 This work is subject to copyright. All rights 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. Violations are liable for prosecution under the German Copyright Law. Springer is a part of Springer Science+Business Media springer.com © Springer-Verlag Berlin Heidelberg 2006 Printed in Germany 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. Product liability: The publishers cannot guarantee the accuracy of any information about dosage and application contained in this book. In every individual case the user must check such information by consulting the relevant literature. Cover design: design & production GmbH, Heidelberg Typesetting and production: LE-TEX Jelonek, Schmidt & Vöckler GbR, Leipzig, Germany Printed on acid-free paper 2/3141/YL - 5 4 3 2 1 0 Preface This book covers all aspects of the analysis of seawater using both classical and the most advanced recently introduced physical techniques. Until fairly recently, the analysis of seawater was limited to a number of major constituents such as chloride and alkalinity. It was generally agreed that any determinations of trace metals carried out on seawater prior to about 1975 are questionable, principally due to the adverse effects of contamination during sampling, which were then little understood and lead to artificially high results. It is only in the past few years that meth- ods of adequate sensitivity have become available for true ultra-trace metal determinations in water. Similar comments apply in the case of organics in seawater, because it has now become possible to resolve the complex mixtures of organics in seawater and achieve the required very low detection limits. Only since the advent of sample preconcentration and mass spectrometry coupled with gas chromatog- raphy and high-performance liquid chromatography, and possibly derivatisa- tion of the original sample constituents to convert them into a form suitable for chromatography, has this become possible. Fortunately, our interest in micro-constituents in the seawater both from the environmental and the nutrient balance points of view has coincided with the availability of advanced instrumentation capable of meeting the analytical needs. Chapter 1 discusses a very important aspect of seawater analysis, namely sampling. If the sample is not taken correctly, the final result is invalidated, no matter how sophisticated the final analytical procedure. Recent important work on sampling is discussed in detail. Chapters 2 and 3 discuss the determination of anions. Direct application of many of the classical procedures for anions fail for seawater owing to interfering effects of the simple matrix. Suitable modifications are discussed that are amenable to seawater. Dissolved gases in seawater are of interest in certain contexts and their determination is discussed in Chap. 4. Chapters 5 and 6 discuss the application of new techniques such as atomic absorption spectrometry with and without graphite furnace and Zeeman back- ground correction, inductively coupled plasma mass spectrometry,X-ray fluo- VI Preface rescence spectrometry, neutron activation analysis, voltammetric techniques, and others. In the first part of the chapter elements are discussed singly in al- phabetical order, then as the groups of elements, because the newer techniques often cover ranges of elements. Finally, there is a section on metal preconcen- tration techniques. By concentrating all the metals present in a large volume of sample into a few millilitres, dramatic improvements in detection limited can be achieved, and it is this that enables the techniques to be applicable at the low basal concentrations at which many metals exist in seawater. In- creasingly, owing to fallout and the introduction of nuclear power stations and processing plants, it is necessary to monitor the levels of radioactive elements in the seawater, and this is discussed in Chap. 7. Chapters 8 and 9 cover the determination of a wide range of organics in seawater, whilst Chap. 10 covers organometallic compounds. An increasingly long list of organometallics can be detected in seawater, many of these being produced by biologically induced metal methylation processes occurring in sediment and fish tissues. Finally, in Chap. 11, is discussed the present state of knowledge on the de- termination of various oxygen demand parameters and non-metallic elements in seawater. Amongst others these include total, dissolved, and volatile organic carbon, and total inorganic carbon, as well as recent work on the older oxygen demand parameters such as chemical oxygen demand and biochemical oxygen demand. The confusion that formerly existed regarding these methodologies in now being resolved to the point that meaningful measurements can now be reported. The determination of other non-metallic elements is also discussed in this chapter. Whilst the book will be of obvious interest to anyone concerned with sea- water environmental protection, it is believed that it will also be of interest to othergroupsofworkers,includingRiverAuthoritieswhohavetoimplement legal requirements regarding seawater pollution, oceanographers, fisheries experts and politicians who create and implement environmental policies, and the news media, who are responsible for making the general public aware of environmental matters. The book will also be of interest to practising analysts and, not least, to the scientists and environmentalists of the future who are currently passing through the university system and on whom, more than even previously, will rest the responsibility of ensuring that our oceans are protected in the future. Anglesey, UK, 2006 T. R. Crompton Contents 1 Sampling and Storage ....................... 1 1.1 Sampling............................. 1 1.2 SamplingDevices........................ 3 1.2.1 Intercomparison of Seawater Sampling for Trace Metals . 7 1.2.2 Intercomparison of Sampling Devices andAnalyticalTechniquesUsingSeawaterfromaCEPEX (Controlled, Ecosystem Pollution Experiment) Enclosure . 12 1.3 SamplePreservationandStorage................ 17 1.3.1 Losses of Silver, Arsenic, Cadmium, Selenium, and Zinc from Seawater by Sorption on Various Container Surfaces [54] ............... 19 1.3.2 Losses of Phthalic Acid Esters and Polychlorinated Biphenyls fromSeawaterSamplesDuringStorage............ 26 1.4 SampleContaminationDuringAnalysis............ 27 References............................ 34 2 Determination of Anions ..................... 39 2.1 Acetate.............................. 39 2.1.1 IonChromatography...................... 39 2.2 Acrylate............................. 39 2.2.1 IonChromatography...................... 39 2.3 Alkalinity............................ 39 2.3.1 TitrationMethod........................ 39 2.3.2 Spectrophotometric Methods .................. 40 2.4 Arsenate/Arsenite........................ 41 2.4.1 Spectrophotometric Method . ................. 41 2.5 Benzoate............................. 41 2.5.1 IonChromatography...................... 41 2.6 Butyrate............................. 41 2.6.1 IonChromatography...................... 41 2.7 Borate.............................. 42 2.7.1 Spectrophotometric Method . ................. 42 2.8 Bromate............................. 42 2.8.1 Spectrophotometric Titration and Differential Pulse Polarography........................... 42 VIII Contents 2.9 Bromide............................. 45 2.9.1 TitrationMethod........................ 45 2.9.2 X-rayEmissionSpectrometry.................. 45 2.9.3 SegmentedFlowAnalysis.................... 46 2.9.4 SolidStateMembraneElectrodes................ 46 2.9.5 X-rayFluorescenceSpectroscopy................ 46 2.9.6 Isotachoelectrophoresis..................... 46 2.10 Chloride............................. 47 2.10.1 TitrationMethod........................ 47 2.10.2 IonSelectiveElectrodes..................... 47 2.10.3 Chronopotentiometry...................... 48 2.10.4 Miscellaneous.......................... 48 2.11 ChromateandDichromate................... 48 2.11.1 AtomicAbsorptionSpectrometry............... 48 2.11.2 OrganicFormsofChromium.................. 49 2.12 Fluoride............................. 53 2.12.1 Spectrophotometric Method . ................. 53 2.12.2 IonSelectiveElectrodes..................... 53 2.12.3 PhotoactivationAnalysis.................... 56 2.12.4 AtomicAbsorptionSpectrometry............... 56 2.13 Formate............................. 57 2.13.1 HighPerformanceLiquidChromatography(HPLC)..... 57
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