APPLICATION OF IC-MS AND IC-ICP-MS IN ENVIRONMENTAL RESEARCH

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3 APPLICATION OF IC-MS AND IC-ICP-MS IN ENVIRONMENTAL RESEARCH

5 APPLICATION OF IC-MS AND IC-ICP-MS IN ENVIRONMENTAL RESEARCH Edited by RAJMUND MICHALSKI Institute of Environmental Engineering of Polish Academy of Sciences, Poland

6 Copyright 2016 by John Wiley & Sons, Inc. All rights reserved Published by John Wiley & Sons, Inc., Hoboken, New Jersey Published simultaneously in Canada No part of this publication may be reproduced, stored in a retrieval system, or transmitted in any form or by any means, electronic, mechanical, photocopying, recording, scanning, or otherwise, except as permitted under Section 107 or 108 of the 1976 United States Copyright Act, without either the prior written permission of the Publisher, or authorization through payment of the appropriate per-copy fee to the Copyright Clearance Center, Inc., 222 Rosewood Drive, Danvers, MA 01923, (978) , fax (978) , or on the web at Requests to the Publisher for permission should be addressed to the Permissions Department, John Wiley & Sons, Inc., 111 River Street, Hoboken, NJ 07030, (201) , fax (201) , or online at Limit of Liability/Disclaimer of Warranty: While the publisher and author have used their best efforts in preparing this book, they make no representations or warranties with respect to the accuracy or completeness of the contents of this book and specifically disclaim any implied warranties of merchantability or fitness for a particular purpose. No warranty may be created or extended by sales representatives or written sales materials. The advice and strategies contained herein may not be suitable for your situation. You should consult with a professional where appropriate. Neither the publisher nor author shall be liable for any loss of profit or any other commercial damages, including but not limited to special, incidental, consequential, or other damages. For general information on our other products and services or for technical support, please contact our Customer Care Department within the United States at (800) , outside the United States at (317) or fax (317) Wiley also publishes its books in a variety of electronic formats. Some content that appears in print may not be available in electronic formats. For more information about Wiley products, visit our web site at Library of Congress Cataloging-in-Publication Data: Names: Michalski, Rajmund, editor of compilation. Title: Application of IC-MS and IC-ICP-MS in environmental research / edited by Rajmund Michalski. Description: Hoboken, New Jersey : John Wiley & Sons, Includes bibliographical references and index. Identifiers: LCCN ISBN (cloth) ISBN (epub) Subjects: LCSH: Ion exchange chromatography. Inductively coupled plasma mass spectrometry. Classification: LCC QP519.9.I54 A DDC 543/.82 dc23 LC record available at Typeset in 10/12pt TimesLTStd by SPi Global, Chennai, India Printed in the United States of America

7 CONTENTS List of Contributors Preface ix xi 1 Principles and Applications of Ion Chromatography 1 Rajmund Michalski 1.1 Principles of Ion Chromatography, Introduction, Stationary Phases, Eluents, Suppressors, Detection Methods, Ion Chromatography Applications, Speciation Analysis with the Hyphenated Methods of IC-ICP-MS and IC-MS, Sample Preparation for Ion Chromatography, Selected Methodological Aspects of Ion Determination with Ion Chromatography, Ion Chromatography Development Perspectives, References, 37 2 Mass Spectrometric Detectors for Environmental Studies 47 Maria Balcerzak 2.1 Introduction, 47 v

8 vi CONTENTS 2.2 Mass Spectrometric Detectors, Ionization Methods, Mass Analyzers, 58 Acknowledgments, References, 62 3 High-Performance Liquid Chromatography Coupled to Inductively Coupled Plasma MS/Electrospray Ionization MS 79 Jürgen Mattusch 3.1 Separation Principles, Ion Chromatography (Anion/Cation Exchange, Mixed Mode), High-Performance Liquid Chromatography (Reversed-Phase Mode, HILIC), Size Exclusion Chromatography (SEC) (Gel Filtration Chromatography, GFC), Detection Principles, Common Detection in IC: Conductivity, UV Vis, Electrochemical Detection, Element Specific Detection, Hyphenated Techniques, HPLC(IC) ICP-MS, HPLC(IC) ICP-MS/ESI-MS, Fundamentals, Methodology of Data Evaluation, Technical Requirements, Applications and Conclusion, References, Application of IC-MS in Organic Environmental Geochemistry 109 Klaus Fischer 4.1 Introduction, Carboxylic Acids, Molecular Structure, Molecular Interaction Potential, and Chromatographic Retention, Environmental Analysis of Carboxylic Acids by Ion Exclusion Chromatography Mass Spectrometry (HPICE-MS), Environmental Analysis of Carboxylic Acids by Ion-Exchange Chromatography Mass Spectrometry (HPI-EC-MS), Carbohydrates, Structural Diversity and Ion Chromatographic Behavior, Environmental Analysis of Carbohydrates by Various IC-MS Methods, Amines and Amino Acids, 143

9 CONTENTS vii 4.5 Trends and Perspectives, References, Analysis of Oxyhalides and Haloacetic Acids in Drinking Water Using IC-MS and IC-ICP-MS 152 Koji Kosaka 5.1 Introduction, Source of Oxyhalides and HAAs, Analysis of Oxyhalides and HAAs, Suppressed IC-MS, Nonsuppressed IC-MS and LC-MS, IC-ICP-MS, Application for Monitoring of Oxyhalides and HAAs in Drinking Water, Oxyhalides, HAAs, 171 Summary, References, Analysis of Various Anionic Metabolites in Plant and Animal Material by IC-MS 178 Adam Konrad Jagielski and Michal Usarek 6.1 Introduction, Optimization of HPIC and Ms Settings, HPIC Settings, MS Settings, HPIC-MS Settings, Extraction of Metabolites from Cells and Tissues, Application of the Method in Analysis of Metabolites in Plant and Animal Material, Analysis of Metabolites from Cell Cultures (Primary Cultures as well as Established Cell Lines), Analysis of Metabolites from Solid Tissues, Extraction of Metabolites from Plants, Conclusions, References, Analysis of Perchlorate Ion in Various Matrices Using Ion Chromatography Hyphenated with Mass Spectrometry 199 Jay Gandhi 7.1 Introduction, Precautions Unique to Ion Chromatography Mass Spectrometry, Instrumental and Operating Parameters, 201

10 viii CONTENTS 7.3 Results and Discussion, 204 Acknowledgment, References, Sample Preparation Techniques for Ion Chromatography 210 Wolfgang Frenzel and Rajmund Michalski 8.1 Introduction, When and Why is Sample Preparation Required in Ion Chromatography? Automation of Sample Preparation (IN-LINE Techniques), Sample Preparation Methods, Filtration and Ultrafiltration, Solid-Phase Extraction (SPE), Liquid Liquid Extraction, Gas-Phase Separations, Precipitation, Membrane-Based Separations and Sample Treatment, Trace Analysis and Preconcentration for Ion Chromatographic Analysis, Preconcentration Using SPE, Membrane-Based In-Line Preconcentration, In-Line Preseparations Using Two-Dimensional Ion Chromatography (2D-IC), Sample Preparation of Solid Samples, Dissolution and Aqueous or Acid Extraction, Wet-Chemical Acid Digestions, UV Photolytic Digestion, Fusion Methods, Dry Ashing and Combustion Methods, Air Analysis Using Ion Chromatography Application to Gases and Particulate Matter, Postcolumn Eluent Treatment Prior to Ms Detection, Concluding Remarks, References, 258 Index 267

11 LIST OF CONTRIBUTORS Maria Balcerzak; Department of Analytical Chemistry, Faculty of Chemistry, Warsaw University of Technology, Noakowskiego 3, Warsaw, Poland Klaus Fischer; Faculty VI Regional and Environmental Sciences, Department of Analytical and Ecological Chemistry, University of Trier, Behringstr. 21, Trier, Germany Wolfgang Frenzel; Technische Universität Berlin, Strasse des 17. Juni 135, Berlin, Germany Jay Gandhi; Metrohm USA, 4738 Ten Sleep Lane, Friendswood, TX 77546, USA Adam Konrad Jagielski; Department of Metabolic Regulation, Faculty of Biology, Institute of Biochemistry, University of Warsaw, Miecznikowa 1, Warsaw, Poland Koji Kosaka; Department of Environmental Health, National Institute of Public Health, Minami, Wako, Saitama , Japan Jürgen Mattusch; Department of Analytical Chemistry, Helmholtz Centre for Environmental Research, Permoserstr. 15, Leipzig, Germany Rajmund Michalski; Institute of Environmental Engineering, Polish Academy of Sciences, M. Skłodowskiej-Curie 34, Zabrze, Poland Michal Usarek; Department of Metabolic Regulation, Faculty of Biology, Institute of Biochemistry, University of Warsaw, Miecznikowa 1, Warsaw, Poland ix

13 PREFACE Environmental analytical chemistry can be regarded as the study of a series of factors that affect the distribution and interaction of elements and substances present in the environment, the ways they are transported and transferred, as well as their effects on biological systems. In recent years, the importance of monitoring and controlling environmental pollutants has become apparent in all parts of the world. As a result, analysts have intensified their efforts to identify and determine toxic substances in air, water, wastewaters, food, and other sectors of our environment. The toxicological data analyses involve constant lowering of analyte detection limits to extremely low concentration levels. Speciation analysis, understood as research into various element forms, is gaining importance in environmental protection, biochemistry, geology, medicine, pharmacy, and food quality control. It is popular because what frequently determines the toxicological properties of a compound or element is not its total content, but in many cases, it is the presence of its various forms. Elements occurring in ionic forms are generally believed to be biologically and toxicologically interactive with living organisms. Studying low analytes concentrations, particularly in complex matrix samples, requires meticulous and sophisticated analytical methods and techniques. The latest trends embrace the hyphenated methods combining different separation and detection methods. In the range of ionic compounds, the most important separation technique is ion chromatography. Since its introduction in 1975, ion chromatography has been used in most areas of analytical chemistry and has become a versatile and powerful technique for the analysis of a vast number of inorganic and organic ions present in samples with different matrices. The main advantages of ion chromatography include the short time needed for analyses, possibility of analysis of small volume samples, high sensitivity and selectivity, and a possibility of simultaneous separation xi

14 xii PREFACE and determination of a few ions or ions of the same element at different degrees of oxidation. Mass spectrometry is the most popular detection method in speciation analysis, because it offers information on the quantitative and qualitative sample composition and helps to determine analytes structure and molar masses. The access to the structural data (necessary for the identification of the already known or newly found compounds) poses a challenge for speciation analysis as higher sensitivity of detection methods contributes to the increased number of detected element forms. Couplings of ion chromatography with MS or ICP-MS detectors belong to the most popular and useful hyphenated methods to determine different ion forms of metals and metalloids ions (e.g., Cr(III)/Cr(VI), As(III)/As(V)), as well as others ions (e.g., bromate, perchlorate). IC-MS and IC-ICP-MS create unprecedented opportunities, and their main advantages include extremely low limits of detection and quantification, high precision, and repeatability of determinations. The intent of this book is to introduce anyone interested in the field of ion chromatography, species analysis and hyphenated methods (IC-MS and IC-ICP-MS) the theory and practice. This book should be interesting and useful for analytical chemists engaged in environmental protection and research, with backgrounds in chemistry, biology, toxicology, and analytical chemistry in general. Moreover, employees of laboratories analyzing environmental samples and carrying out species analysis might find general procedures for sample preparation, chromatographic separation, and mass spectrometric analysis. 6 February 2016 Rajmund Michalski Zabrze, Poland

15 1 PRINCIPLES AND APPLICATIONS OF ION CHROMATOGRAPHY Rajmund Michalski Institute of Environmental Engineering, Polish Academy of Sciences, M. Skłodowskiej-Curie 34, Zabrze , Poland 1.1 PRINCIPLES OF ION CHROMATOGRAPHY Introduction The history of chromatography as a separation method began in 1903 when Mikhail Semyonovich Tsvet (a Russian biochemist working at the Department of Chemistry of the Warsaw University) separated plant dyes using adsorption in a column filled with calcium carbonate and other substances [1]. After extraction with the petroleum ether, he obtained clearly separated colorful zones. To describe this method, he used Greek words meaning color (ρωμα) and writing (γραφω) and coined a new word, chromatography, which literally meant writing colors. At present, chromatographic methods are among the most popular instrumental methods in the analytical chemistry as they offer quick separation and determination of substances, including complex matrix samples. Chromatographic methods are used widely on both the preparative and analytical scales. They help to separate and determine polar and nonpolar components; acidic, neutral, and alkaline compounds; organic and inorganic substances; monomers, oligomers, and polymers. It is necessary to use an appropriate chromatography type, which depends on the physicochemical properties of the examined sample and its components. Gas chromatography (GC) and liquid chromatography (LC) Application of IC-MS and IC-ICP-MS in Environmental Research, First Edition. Edited by Rajmund Michalski John Wiley & Sons, Inc. Published 2016 by John Wiley & Sons, Inc. 1

BASICS OF ANALYTICAL CHEMISTRY AND CHEMICAL EQUILIBRIA

BASICS OF ANALYTICAL CHEMISTRY AND CHEMICAL EQUILIBRIA BASICS OF ANALYTICAL CHEMISTRY AND CHEMICAL EQUILIBRIA BRIAN M. TISSUE Virginia Tech Department of Chemistry Blacksburg, VA Cover Design: Wiley Cover