Antarctic Environmental Monitoring Handbook Council of Managers of Scientific Committee on National Antarctic Programs Antarctic Research Antarctic Environmental Monitoring Handbook Standard techniques for monitoring in Antarctica May 2000 Prepared by the Geochemical and Environmental Research Group (GERG) Texas A&M University College Station Texas USA on behalf of COMNAP and SCAR Published by the Council of Managers of National Antarctic Programs (COMNAP) and the Scientific Committee on Antarctic Research (SCAR) Copyright © COMNAP Secretariat 2000 COMNAP Secretariat GPO Box 824 Hobart Tasmania 7001 AUSTRALIA Tel: +61 (0)3 6233 5498 Fax: +61 (0)3 6233 5497 TABLE OF CONTENTS Page Foreword................................................................................................................... xi List of Acronyms....................................................................................................... xiii List of Figures........................................................................................................... xvii List of Tables............................................................................................................. xix SECTION A - ADMINISTRATIVE AND PRE-ANALYSIS ASPECTS OF ENVIRONMENTAL MONITORING Chapter 1. Introduction 1.1 Purpose...................................................................................................................... 1-1 1.2 Handbook Preparation............................................................................................... 1-2 1.3 Choice of Indicators.................................................................................................. 1-3 Chapter 2. Quality Assurance/Quality Control (QA/QC) 2.1 Standard Operating Procedures................................................................................. 2-1 2.2 Standard Reference Materials................................................................................... 2-2 Chapter 3. Data Management 3.1 Data Administration.................................................................................................. 3-2 3.2 Data Control.............................................................................................................. 3-6 3.3 Data Utilization......................................................................................................... 3-7 3.4 Data Archive............................................................................................................. 3-8 3.5 Geographic Information Systems.............................................................................. 3-9 Chapter 4. Sample Collection, Handling, and Preservation 4.1 Wastewater................................................................................................................ 4-2 4.2 Marine and Freshwater.............................................................................................. 4-6 4.2.1 Discrete Water Sample Collection................................................................ 4-6 4.2.2 In Situ Sensors............................................................................................... 4-7 4.2.3 Ice and Through-Ice Sampling...................................................................... 4-8 4.3 Snow.......................................................................................................................... 4-8 4.3.1 Sampling Procedures..................................................................................... 4-9 4.3.2 Snowpits........................................................................................................ 4-10 4.3.3 Snowpit Sampling......................................................................................... 4-10 4.3.4 Stratigraphy and Physical Studies................................................................. 4-11 v 4.3.5 Snow Pack Depth.......................................................................................... 4-12 4.4 Sediments and Soils.................................................................................................. 4-12 Chapter 5. Station Performance 5.1 Station Performance.................................................................................................. 5-1 5.2 Aerial Photography................................................................................................... 5-2 SECTION B - ANALYTICAL TECHNIQUES Chapter 6. Wastewater/Seawater/Freshwater 6.1 Total Suspended Solids (TSS).................................................................................. 6-1 6.1.1 Sample Preparation....................................................................................... 6-3 6.1.2 Sample Processing......................................................................................... 6-3 6.1.3 Calculations................................................................................................... 6-4 6.2 Dissolved Oxygen(DO)............................................................................................. 6-4 6.2.1 Modified Winkler Method............................................................................ 6-5 6.2.1.1 Sample Preparation........................................................................ 6-7 6.2.1.2 Sample Processing.......................................................................... 6-7 6.2.1.3 Calculations.................................................................................... 6-8 6.2.2 Membrane Electrode Method........................................................................ 6-8 6.3 Biological Oxidation Demand (BOD)....................................................................... 6-10 6.3.1 Sample Preparation....................................................................................... 6-11 6.3.2 Sample Processing......................................................................................... 6-11 6.3.2.1 Preparation of Dilution Water........................................................ 6-11 6.3.2.2 Dilution Water Check..................................................................... 6-11 6.3.2.3 Seeding Material............................................................................ 6-12 6.3.2.4 Use of DO Probe or Sensor............................................................ 6-14 6.3.3 Calculations................................................................................................... 6-14 6.4 Chemical Oxidation Demand (COD)........................................................................ 6-16 6.4.1 Open Reflux Method..................................................................................... 6-18 6.4.1.1 Sample Preparation and Processing............................................... 6-18 vi 6.4.1.2 Calculations.................................................................................... 6-19 6.4.2 Closed Reflux Method - #1 - Sample Preparation and Processing............... 6-19 6.4.2.1 Calculations.................................................................................... 6-21 6.4.3 Closed Reflux Method - #2 - Sample Preparation and Processing............... 6-21 6.4.3.1 Calculations.................................................................................... 6-22 6.5 Acidity....................................................................................................................... 6-22 6.5.1 Sample Preparation and Processing.............................................................. 6-23 6.5.2 Calculations................................................................................................... 6-23 6.6 pH.............................................................................................................................. 6-24 6.6.1 Sample Preparation and Processing.............................................................. 6-25 6.6.2 Calculations................................................................................................... 6-25 6.7 Conductivity.............................................................................................................. 6-26 6.7.1 Sample Preparation and Processing.............................................................. 6-27 6.7.2 Calculations................................................................................................... 6-28 6.8 Nitrate/Nitrite............................................................................................................ 6-29 6.8.1 Spectrophotometric, Cadmium Reduction Method....................................... 6-29 6.8.1.1 Sample Preparation........................................................................ 6-31 6.8.1.2 Sample Processing.......................................................................... 6-31 6.8.1.3 Calculations.................................................................................... 6-32 6.8.2 Autoanalyzer Method.................................................................................... 6-32 6.8.2.1 Sample Preparation........................................................................ 6-32 6.8.2.2 Sample Processing.......................................................................... 6-34 6.8.2.3 Calculations.................................................................................... 6-36 6.8.3 Portable Test Kits.......................................................................................... 6-36 6.8.4 Ion Selective Electrodes................................................................................ 6-37 6.8.5 Test Strips...................................................................................................... 6-38 6.9 Phosphate.................................................................................................................. 6-39 6.9.1 Sample Preparation....................................................................................... 6-40 vii 6.9.2 Sample Processing......................................................................................... 6-41 6.9.3 Calculations................................................................................................... 6-41 6.10 Temperature (T)........................................................................................................ 6-41 6.11 Coliform Bacteria...................................................................................................... 6-42 6.11.1 Sample Preparation and Processing.............................................................. 6-42 6.11.2 Calculations................................................................................................... 6-45 6.12 Phytoplankton............................................................................................................ 6-46 6.12.1 Sample Preparation....................................................................................... 6-46 6.12.2 Sample Processing and Calculations............................................................. 6-47 6.12.3 Modified Method for Chlorophylls and Carotenoids.................................... 6-49 6.12.3.1 Sample Preparation........................................................................ 6-49 6.12.3.2 Sample Processing.......................................................................... 6-50 6.12.3.3 Calculations.................................................................................... 6-50 Chapter 7. Snow 7.1 Metals........................................................................................................................ 7-1 7.1.1 Sample Preparation....................................................................................... 7-2 7.1.1.1 Acid Digestion Procedure for Furnace Atomic Absorption (FAA) Analysis.............................................................................. 7-3 7.1.1.2 Acid Digestion Procedure for ICP and Flame AA Analyses......... 7-3 7.1.1.3 Total Metals Sample Preparation Using Microwave Digestion..... 7-3 7.2 Total Petroleum Hydrocarbons................................................................................. 7-5 7.2.1 Sample Preparation....................................................................................... 7-6 7.2.2 Sample Processing......................................................................................... 7-6 7.2.3 Calculations................................................................................................... 7-7 7.3 Particulates................................................................................................................ 7-8 7.3.1 Sample Preparation and Processing.............................................................. 7-8 Chapter 8. Soils/Sediments 8.1 Grain Size.................................................................................................................. 8-1 8.1.1 Sample Preparation....................................................................................... 8-2 8.1.2 Sample Processing......................................................................................... 8-2 viii 8.1.3 Calculations................................................................................................... 8-4 8.2 Carbon Content ........................................................................................................ 8-4 8.2.1 Total Carbon (TC) ........................................................................................ 8-6 8.2.2 Total Organic Carbon (TOC)........................................................................ 8-7 8.2.3 Total Inorganic Carbon (TIC)....................................................................... 8-8 8.2.4 Calculations................................................................................................... 8-8 8.3 Metals........................................................................................................................ 8-9 8.3.1 Sample Preparation....................................................................................... 8-10 8.3.1.1 Acid Digestion Procedure for ICP, Flame AA, and Furnace AA Analyses......................................................................................... 8-10 8.3.1.2 Total Metals Sample Preparation Using Microwave Digestion..... 8-12 8.3.1.3 Total Digestion of Sediment with Hydrofluric Acid for Trace Metal Analyses..................................................................... 8-15 8.3.2 Graphite Furnace Atomic Absorption Spetrophotometry (GFAAS)............ 8-16 8.3.3 Inductively Coupled Plasma Emission Spectroscopy (ICP)......................... 8-22 8.3.4 Cold Vapor Atomic Absoprtion Spectroscopy-Mercury (Hg)...................... 8-34 8.3.4.1 Sample Preparation........................................................................ 8-36 8.3.4.2 Instrument Analysis........................................................................ 8-36 8.3.5 Calculations................................................................................................... 8-36 8.4 Total Petroleum Hydrocarbons (TPH)...................................................................... 8-40 8.4.1 Sample Preparation....................................................................................... 8-40 8.4.2 Gravimetry.................................................................................................... 8-41 8.4.3 Infrared Spectrophotometry.......................................................................... 8-41 8.4.4 Gas Chromatography..................................................................................... 8-42 8.5 Polycyclic Aromatic Hydrocarbons (PAH)............................................................... 8-46 8.5.1 Sample Preparation....................................................................................... 8-46 8.5.2 Spectrophotometry........................................................................................ 8-48 8.5.3 High Performance Liquid Chromatography (HPLC).................................... 8-56 8.5.4 Gas Chromatography/Mass Spectrometry (GC/MS).................................... 8-62 Chapter 9. Bibliography - Glossary of Terms ix
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