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Lake Michigan Mass Balance
Methods Compendium

June 1997

LMMB ICON

The Lake Michigan Mass Budget/Mass Balance (LMMB) Study was initiated in late 1993 as part of the Lakewide Management Plan (LaMP) for Lake Michigan. The Lake Michigan LaMP and the LMMB Study were developed to meet requirements mandated by Section 118 of the Clean Water Act (CWA); Title III, Section 112(m) of the Clean Air Act Amendments; and Annex 2 of the Great Lakes Water Quality Agreement. Organizations participating in the development of these programs included: EPA Region 5, the EPA Great Lakes National Program Office, the National Oceanic and Atmospheric Administration, the U.S. Geological Survey, the U.S. Fish and Wildlife Service, the Michigan Department of Natural Resources, the Wisconsin Department of Natural Resources, the Illinois Department of Natural Resources, and the Indiana Department of Environmental Management. In general, the primary goal of the LaMP and the LMMB Study is to develop a sound, scientific base of information with which to guide future toxic load reduction efforts at the federal, state, and local levels.

This compendium describes the sampling and analytical methods used in the LMMB Study. For ease of use, the compendium is organized into three volumes. Volume 1 describes sampling procedures used in the study; Volumes 2 and 3 describe analytical procedures used by each PI. Because sampling apparatus and techniques are generally geared towards specific matrices, Volume 1 is organized according to sample matrix (e.g., air, water, sediment, tissue, etc). Volumes 2 and 3 are organized by pollutant type (e.g, organics, metals, biologicals) because laboratories and instrumentation are typically set up to address specific pollutants rather than specific matrices.

Each Principal Investigator (PI) was required to follow specific quality control requirements necessary to meet data quality and measurement quality objectives for the LMMB Study. To assist users of this document, Appendix A provides the measurement quality objectives (MQOs) established by each PI for his/her sampling and analysis program.

Finally, EPA has made no attempt to standardize the procedures submitted by PIs for publication in this compendium. Therefore, the methods provided in this document contain varying levels of detail. Appendix B provides names, addresses and phone numbers for each PI and for each EPA Project Officer (PO). Specific questions about the procedures used in the study should be directed to the appropriate PI or PO listed in Appendix B.

 

Methods

Methods

Volume 1 Volume 2 Volume 3
Sample Collection Techniques

 

Organic and Mercury sample Analysis Techiques Metals, Conventions, Radiochemistry, and Biomonitoring Sample Techniques
Air, Water, Sediment, Plankton, Fish Organic Analysis, Mercury Analysis Metals, Conventionals, Radiochemistry, Biomonitoring, Shipboard Measurements

 

Volume 1
Sample Collection Techniques
Air
Water
Sediment
Plankton
Fish

(back to other methods)

Chapter 1: Air

LMMB 001 Standard Operating Procedure for Air Sampling for Semivolatile Organic Contaminants Using the Organics High-Volume Sampler (Sweet, C.)
LMMB 002 Standard Operating Procedure for Precipitation Sampling Using XAD-2 and MIC Collectors (Sweet, C.)
LMMB 003 Standard Operating Procedure for Air Sampling for Metals Using the Dichotomous Sampler (Sweet, C.)
LMMB 004 Standard Operating Procedure for Sampling Trace Metals in Precipitation Using Modified Aerochem Collectors (Vermette, S. and Sweet, C.)
LMMB 005 Metals Cleaning Procedures for Teflon Bottles and Rigid HDPE (Vermette, S. and Sweet, C.)
LMMB 006 Standard Operating Procedure for Sampling of Vapor Phase Mercury (Keeler, G. and Landis, M.)
LMMB 007 Standard Operating Procedure for Sampling of Mercury in Precipitation (Keeler, G and Landis, M.)
LMMB 008 Standard Operating Procedure for Sampling of Particulate Phase Mercury (Keeler, G. and Landis, M.)
LMMB 009 Standard Operating Procedure for Dry Deposition Sampling: Dry Deposition of Atmospheric Particles (Paode, R. and Holsen, T.)

Chapter 2: Water

LMMB 010 Standard Operating Procedure for Sample Collection of Atrazine and Atrazine Metabolites (Eisenreich, S., Schottler, S., and Hines, N.)
LMMB 011 HOC Sampling Media Preparation and Handling; XAD-2 Resin and GF/F Filters (Crecelius, E. and Lefkovitz, L.)
LMMB 012 Standard Operating Procedure for Site Selection and Sampling for Mercury in Lakewater (Mason, R. and Sullivan, K.)
LMMB 013 Field Sampling Using the Rosette Sampler (Warren, G.)
LMMB 014 Standard Operating Procedure for the Sampling of Particulate-Phase and Dissolved-Phase Organic Carbon in Great Lakes Waters (Grace Analytical Lab)
LMMB 015 Standard Operating Procedure for Chlorophyll-a Sampling Method: Field Procedure (Grace Analytical Lab)
LMMB 016 Standard Operating Procedure for Primary Productivity Using 14C: Field Procedure (Grace Analytical Lab)
LMMB 017 USGS Field Operation Plan: Tributary Monitoring (USGS/Eisenreich, S.)
LMMB 018 Trace Metal and Mercury Sampling Methods for Lake Michigan Tributaries (Shafer, M.)

Chapter 3: Sediment

LMMB 019 Standard Operating Procedure for Collection of Sediment Samples (Edgington, D. and Robbins, J.)
LMMB 020 Trap Sample Splitting (wet): Use of Sediment Traps for the Measurement of Particle and Associated Contaminant Fluxes (Eadie, B.)

Chapter 4: Plankton

LMMB 021 Standard Operating Procedure for Sampling Lake Michigan Lower Pelagic Foodchain for PCBs, Nonachlor, and Mercury (Swackhamer, D., Trowbridge, A., and Nater, E.)
LMMB 022 Sampling Procedure for Collection of Benthic Invertebrates for Contaminant Analysis (Warren, G.)
LMMB023 Standard Operating Procedure for Phytoplankton Sample Collection and Preservation (Grace Analytical Lab)
LMMB 024 Standard Operating Procedure for Zooplankton Sample Collection and Preservation (Grace Analytical Lab)

Chapter 5: Fish

LMMB 025 Fish Processing Method (Hesselberg, R.)
LMMB 026 Quality Assurance Project Plan for Lake Trout and Forage Fish Sampling for Diet Analysis and/or Contaminant Analysis (Brown, E. and Eck, G.)
LMMB 027 Quality Assurance Project Plan for Coho Sampling for Contaminant and Diet Analysis (Holey, M. and Elliott, R.)

 

Volume 2
Organic and Mercury Sample Analysis Techniques
Organic Analysis
Mercury Analysis

(back to other methods)

Chapter 1: Organic Analysis

LMMB 028 Instrumental Analysis and Quantitation of Polycyclic Aromatic Hydrocarbons and Atrazine: IADN Project (Cortes, D. and Brubaker, W.)
LMMB 029 Analysis of PCBs and Pesticides in Air and Precipitation Samples : IADN Project - Gas Chromatography Procedure (Basu, I.)
LMMB 030 Analysis of PCBs, Pesticides, and PAHs in Air and Precipitation Samples: IADN Project - Sample Preparation Procedure (Basu, I.)
LMMB 031 Analysis of PCBs, Pesticides, and PAHs in Air and Precipitation Samples: Sample Preparation Procedures (Harlin, K. and Surratt, K.)
LMMB 032 Standard Operating Procedure for the Analysis of PAHs and Atrazine by GC/Ion Trap MS (Peters, C. and Harlin, K.)
LMMB 033 Standard Operating Procedure for the Analysis of PCBs and Organochlorine Pesticides by GC-ECD (Harlin, K., Surratt, K., and Peters, C.) Appendix C
LMMB 034 Standard Operating Procedure for Isolation, Extraction and Analysis of Atrazine, DEA and DIA (Eisenreich, S., Schottler, S., and Hines, N.)
LMMB 035 Standard Operating Procedures for Semivolatile Organic Compounds in Dry Deposition Samples (Eisenreich, S. and Franz, T.)
LMMB 036 Extraction and Cleanup of XAD-2 Resin Cartridges for Polychlorinated Biphenyls and Trans-Nonachlor (Crecelius, E. and Lefkovitz, L.)
LMMB 037 Extraction and Cleanup of Glass Fiber Filters for Polychlorinated Biphenyls and Trans-Nonachlor (Crecelius, E. and Lefkovitz, L.)
LMMB 038 PCB Congener Analysis of XAD-2 Resins and GFF Filters Using GC/ECD (Crecelius, E. and Lefkovitz, L.)
LMMB 039 PCBs and Pesticides in Surface Water by XAD-2 Resin Extraction (Wisconsin State Lab of Hygiene)
LMMB 040 Extraction and Cleanup of Sediments for Semivolatile Organics Following the Internal Standard Method (Van Hoof, P. and Hsieh, J.)
LMMB 041 Analysis of Polychlorinated Biphenyls and Chlorinated Pesticides by Gas Chromatography with Electron Capture Detection (Van Hoof, P. and Hsieh, J.)
LMMB 042 Standard Operating Procedure for the Analysis of PCB Congeners by GC/ECD and Trans-Nonachlor by GC/MS/ECNI (Swackhamer, D., Trowbridge, A., and Nater, E.)
LMMB 043 Extraction and Lipid Separation of Fish Samples for Contaminant Analysis and Lipid Determination (Schmidt, L.)
LMMB 044 Analysis of Total PCBs and PCB Congeners and Trans-nonachlor in Fish by Gas Chromatography/Negative Chemical Ionization Single Ion Mass Spectrometry (Schmidt, L.)

Chapter 2: Mercury Analysis

LMMB 045 Standard Operating Procedure for Analysis of Vapor Phase Mercury (Keeler, G. and Landis, M.)
LMMB 046 Standard Operating Procedure for Analysis of Mercury in Precipitation (Keeler, G. and Landis, M.)
LMMB 047 Standard Operating Procedure for Analysis of Particulate Phase Mercury (Keeler, G. and Landis, M.)
LMMB 048 Standard Operating Procedure for Mercury Analysis (Mason, R. and Sullivan, K.)
LMMB 049 Total Mercury Analysis in Aqueous Samples (Hurley, J.)
LMMB 050 Standard Operating Procedure for Analysis of Sediment for Total Mercury Using the Cold Vapor Technique with the Leeman Labs, Inc. Automated Mercury System (Uscinowicz, T. and Rossmann, R.)
LMMB 051 Mercury in Plankton (Nater, E. and Cook, B.)
LMMB 052 Versatile Combustion-Amalgamation Technique for the Photometric Determination of Mercury in Fish and Environmental Samples (Willford, W., Hesselberg, R., and Bergman, H.)
LMMB 053 Analysis of Fish for Total Mercury (Nriagu, J.)

NOTE: For “Standard Operating Procedure for Lab Analysis of Coho Salmon Stomachs and Data Entry”, see Volume 1, Chapter 5, LMMB 026, Quality Assurance Project Plan for Coho Sampling for Contaminant and Diet Analysis.

Volume 3
Metals, Conventionals, Radiochemistry, and Biomonitoring Sample Analysis Techniques
Metals
Conventionals
Radiochemistry
Biomonitoring
Shipboard Measurements

(back to other methods)

Chapter 1: Metals

LMMB 054 Laboratory Methods for ICP-MS Analysis of Trace Metals in Precipitation (Talbot, J. and Weiss, A.)
LMMB 055 Standard Operating Procedures for Preparation, Handling and Extraction of Dry Deposition Plates: Dry Deposition of Atmospheric Particles (Paode, R. and Holsen, T.)
LMMB 056 Standard Operating Procedure for EPA’s LBL Energy Dispersive X-Ray Fluorescence Spectrometry (Kellogg, R.)
LMMB 057 Analysis of Surface Waters for Trace Elements by Inductively-Coupled Plasma Mass Spectrometry (Shafer, M. and Overdier, J.)

Chapter 2: Conventionals

LMMB 058 ESS Method 130.1: General Auto Analyzer Procedures (Wisconsin State Lab of Hygiene)
LMMB 059 ESS Method 200.5: Determination of Inorganic Anions in Water by Ion Chromatography (Wisconsin State Lab of Hygiene)
LMMB 060 ESS Method 140.4: Chloride - Automated Flow Injection Analysis (Wisconsin State Lab of Hygiene)
LMMB 061 ESS Method 220.3: Ammonia Nitrogen and Nitrate + Nitrite Nitrogen, Automated Flow Injection Analysis Method (Wisconsin State Lab of Hygiene)
LMMB 062 ESS Method 230.1: Total Phosphorus and Total Kjeldahl Nitrogen, Semi-Automated Method (Wisconsin State Lab of Hygiene)
LMMB 063 ESS Method 310.1: Ortho-Phosphorus, Dissolved Automated, Ascorbic Acid (Wisconsin State Lab of Hygiene)
LMMB 064 ESS Method 310.2: Phosphorus, Total, Low Level (Persulfate Digestion) (Wisconsin State Lab of Hygiene)
LMMB 065 ESS Method 340.2: Total Suspended Solids, Mass Balance (Dried at 103-105C) Volatile Suspended Solids (Ignited at 550C) (Wisconsin State Lab of Hygiene)
LMMB 066 Outline of Standard Protocols for DOC Analyses (Shafer, M.)
LMMB 067 Outline of Standard Protocols for Particulate Organic Carbon (POC) Analyses (Baldino, R.)
LMMB 068 ESS Method 360.2: Silica Dissolved, Automated, Colorimetric (Wisconsin State Lab of Hygiene)
LMMB 069 ESS Method 360.3: Silica, Dissolved, Micro Level Automated, Colorimetric (Wisconsin State Lab of Hygiene)
LMMB 070 ESS Method 370.2: Sulfates Colorimetric, Automated, Methylthymol Blue (Wisconsin State Lab of Hygiene)
LMMB 071 ESS Method 370.3: Sulfates Colorimetric, Automated Flow Injection, Methylthymol Blue (Wisconsin State Lab of Hygiene)
LMMB 072 Standard Operating Procedure for Chloride and Silica in Lake Water (Lachat Method) (Grace Analytical Lab)
LMMB 073 Standard Operating Procedure for Dissolved Reactive Phosphorous (Lachat Method) (Grace Analytical Lab)
LMMB 074 Standard Operating Procedure for Ammonia (Lachat Method) (Grace Analytical Lab)
LMMB 075 Standard Operating Procedure for Nitrate, Nitrite (Lachat Method) (Grace Analytical Lab)
LMMB 076 Standard Operating Procedure for Total Kjeldahl Nitrogen (Lachat Method) (Grace Analytical Lab)
LMMB 077 Standard Operating Procedure for Total and Dissolved Phosphorous (Lachat Method) (Grace Analytical Lab)
LMMB 078 Analysis of Total Suspended Particles (TSP) and Total Organic Carbon (TOC) in Air Samples: Integrated Atmospheric Deposition Network (IADN) TSP/TOC Procedure (Wassouf, M. and Basu, I.)
LMMB 079 Standard Operating Procedures for Determining Total Phosphorus, Available Phosphorus, and Biogenic Silica Concentrations of Lake Michigan Sediments and Sediment Trap Material (Johengen, T.)
LMMB 080 Standard Operating Procedure for Perkin Elmer CHN Analyzer (Model 2400) (Eadie, B.)
LMMB 081 Quality Assurance Plan for the Use of Sediment Traps (Eadie, B.)

Chapter 3:Radiochemistry

LMMB 082 Standard Operating Procedure for Primary Productivity Using 14C: Laboratory Procedures (Grace Analytical Lab)
LMMB 083 LProtocol for Standard Analysis for Cesium-137 (Robbins, J. and Edgington, D.)
LMMB 084 Determination of the Activity of Lead-210 in Sediments and Soils (Edgington, D. and Robbins, J.)

Chapter 4:Biomonitoring

LMMB 085 Standard Operating Procedure for Chlorophyll-a and Pheophytin-a (Turner Designs Method) (Grace Analytical Lab)
LMMB 086 ESS Method 150.1: Chlorophyll - Spectrophotometric (Wisconsin State Lab of Hygiene)
LMMB 087 Standard Operating Procedure for Phytoplankton Analysis (Grace Analytical Lab)
LMMB 088 Standard Operating Procedure for Zooplankton Analysis (Grace Analytical Lab)
LMMB 089 Quality Assurance Project Plan: Diet Analysis for Forage Fish (Davis, B. and Savino, J.)

Chapter 5:Shipboard Measurements

LMMB 090 Standard Operating Procedure for GLNPO Turbidity: Nephelometric Method (Palmer, M.)
LMMB 091 Standard Operating Procedure for GLNPO Total Alkalinity Titration (Palmer, M.)
LMMB 092 Standard Operating Procedure for Electrometric pH (Palmer, M.)
LMMB 093 Standard Operating Procedure for Meteorological Data Aboard the R/V Lake Guardian (Palmer, M.)
LMMB 094 Standard Operating Procedure for GLNPO Specific Conductance: Conductivity Bridge (Palmer, M.)
LMMB 095 Total Hardness Titration (Palmer, M.)
LMMB 096 Standard Operating Procedure for the Analysis of Dissolved-Phase Organic Carbon in Great Lakes Waters (Grace Analytical Lab)
LMMB 097 Standard Operating Procedure for the Analysis of Particulate-Phase Organic Carbon in Great Lakes Waters (Grace Analytical Lab)
LMMB 098 Standard Operating Procedure for the Sampling and Analysis of Total Suspended Solids in Great Lakes Waters (Grace Analytical Lab)

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