v>EPA
United States
Environmental Protection
Agency
Handbook
A Compendium of Chemical, Physical
and Biological Methods for Assessing
and Monitoring the Remediation of
Contaminated Sediment Sites
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A Compendium of Chemical, Physical and Biological Methods
for Assessing and Monitoring the Remediation of Contaminated Sediment Sites February 17,2003
A Compendium of Chemical, Physical and
Biological Methods for Assessing and
Monitoring the Remediation of
Contaminated Sediment Sites
EPA Contract No. 68-W-99-033
Work Assignment 4-20
Submitted to
U.S. Environmental Protection Agency
Prepared by
Battelle Memorial Institute
397 Washington Street
Duxbury MA 02332
February 17, 2003
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A Compendium of Chemical, Physical and Biological Methods
for Assessing and Monitoring the Remediation of Contaminated Sediment Sites February 17,2003
CONTACTS
James Lazorchak and Jon Josephs are the EPA contacts for the Compendium of Chemical, Physical, and
Biological Methods for Assessing and Monitoring the Remediation of Contaminated Sediment Sites.
James Lazorchak, Work Assignment Manager for the preparation of the Compendium, is an Aquatic
Ecotoxicologist assigned to the Ecological Exposure Research Division in Cincinnati, OH, which is under
the direction of the National Exposure Research Laboratory with headquarters in Research Triangle Park,
NC.
Jon Josephs, Deputy Work Assignment Manager for preparation of the Compendium, is an Environmental
Engineer assigned to the Hazardous Substances Technical Liaison Program, which is under the direction
of the Office of Science Policy with headquarters in Washington, DC He is stationed at the EPA Region 2
office in New York City. NY
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A Compendium of Chemical, Physical and Biological Methods
for Assessing and Monitoring the Remediation of Contaminated Sediment Sites February 17,2003
ABSTRACT
Considering the many organizations which have published methods for monitoring contaminated sediments
and the large number of documents on this subject, it can be a formidable task for a Superfund project
manager to find methods appropriate for his or her contaminated sediment site This Compendium of
Chemical, Physical and Biological Methods for Assessing and Monitoring the Remediation of Contaminated
Sediment Sites has been prepared to inform Superfund project managers and others about appropriate
methods for monitoring and assessing the remediation of contaminated sediments. Although the document
can be printed as a text document, it is also intended to be viewed on a computer screen in order to take
advantage of its hypertext links to navigate the document and to access reference documents available on
the Internet Search engines can also be utilized to locate information contained in the document.
The methods included in this document focus primarily on published or otherwise citeable chemical, physical,
and biological testing methodologies used by EPA at Superfund sites The document summarizes the
methods, including references to the methods and hypertext links to access those methods which are
available on the Internet. Without exception, it is intended that all of the methods presented will be suitable
for investigations at Superfund sites containing contaminated sediments. However, not all methods will be
suitable for all sites. The selection of methods for a particular site will depend on the site conditions,
remediation plans, budgetary constraints and other factors.
This report was submitted in fulfillment of Contract Number 68-W-99-033 by Battelle Memorial Institute under
the sponsorship of the United States Environmental Protection Agency. The report was prepared during a
period from July 6, 2001 to February 17, 2003 when the work was completed.
111
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A Compendium of Chemical, Physical and Biological Methods
for Assessing and Monitoring the Remediation of Contaminated Sediment Sites
February 17, 2003
TABLE OF CONTENTS
Tables
Table of Acronyms
1 0 Introduction
1.1 Background and Objectives ..
x
XI
1
1.2 Application and Uses of Field, Analytical, and Testing Data at Superfund Sites Containing Contaminated
Sediments ... ... 2
2.0 Momtonng Methods . ...
2 1 Water
2.1.1 Field Sample Collection and Immediate Processing In Situ Data Acquisition
8
8
. 9
Fact Sheet No. 2.1.1-1
Fact Sheet No. 2.1.1-2
Fact Sheet No. 2 1 1-3
Fact Sheet No. 2 1.1-4
Fact Sheet No 2.1.1-5
Fact Sheet No 2.1.1-6
Fact Sheet No. 2.1 1-7
Fact Sheet No. 2.1.1-8
Fact Sheet No. 2 1.1-9
Fact Sheet No 2.1 1-10
Fact Sheet No 2.1.1-11
Fact Sheet No. 2.1.1-12
Fact Sheet No 2 1.1-13
Fact Sheet No 21.1-14
Fact Sheet No 2.1.1-15
Fact Sheet No 2.1.1-16
Fact Sheet No 2.1 1-17
Method Title In Situ sampling with the Hydrolab
Datasonde3®Umt 11
Method Title: In Situ Dissolved Oxygen sampling with a
YSI Model 58 Dissolved Oxygen Meter and Probe ... 12
Method Title In Situ Sampling of Irradiance . ... 13
Method Title1 In Situ Transparency Sampling 14
Method Title Sample Collection Procedures for Marine
Water . . 15
Method No LMMB 013, Method Title In Situ Sample
Collection Using the Rosette Sampler . . .. 17
Method No ERT SOP #2013, Method Title: Water Sample
Collection with the Kemmerer Bottle and the Bacon Bomb Sampler
... ... ... 18
Method No ERT SOP # 2013. Method Title: Dip
Sampler 19
Method Title. Sample and Preservation of Water Specific
Parameters 20
Method No LMMB 014, Method Title: Sampling of
Particulate-Phase and Dissolved-Phase Organic Carbon
in Great Lakes Waters .. 24
Method No EPA Method 1669, Method Title Sampling
Ambient Water for Trace Metals at EPA Water Quality
Criteria Levels 25
Method No LMMB 065, Method Title- ESS Method 340.2.
Total Suspended Solids, Mass Balance (Dried at
103-105'C) Volatile Suspended Solids (Ignited at 550°C) 26
Method Title In situ peepers . 27
Method Title Suction Samplers .. 28
Method Title1 Physical Charactenzation of a Stream . 29
Method Title: Visual-Based Habitat Assessment .... .30
Method No LMMB 017, Method Title: USGS Field
Operation Plan Tributary Momtonng . . ... 32
IV
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A Compendium of Chemical, Physical and Biological Methods
for Assessing and Monitoring the Remediation of Contaminated Sediment Sites
February 17, 2003
Fact Sheet No 2.1.1-18 Method Title: Quality Assurance Plan for Discharge Measurements
Using Broadband Acoustic Doppler Current Profilers 33
Fact Sheet No. 2.1.1-19 Method Title: Seepage Meters 34
Fact Sheet No. 2.1.1-20 Method Title: Caged Bivalve Deployment 35
2.1 2 Chemical and Physical Analysis 36
Fact Sheet No 2.1.2-1 EPA Method No 245.7. Method Title. Mercury in Water
by Cold Vapor Atomic Fluorescence Spectrometry 37
Fact Sheet No. 2.1 2-2 EPA Method No 1631, Revision B, Method Title: Mercury
in Water by Oxidation, Purge and Trap, and Cold Vapor
Atomic Fluorescence Spectrometry 38
Fact Sheet No. 2.1.2-3 EPA Method No. 1630, Method Title. Methyl Mercury in
Water by Distillation, Aqueous Ethylation, Purge and Trap,
and CVAFS 40
Fact Sheet No 2.1 2-4 EPA Method No 1639, Method Title: Determination of
Trace Elements in Ambient Waters by Stabilized
Temperature Graphite Furnace Atomic Absorption 41
Fact Sheet No 2 1 2-5 EPA Method No. 1637, Method Title. Determination of
Trace Elements in Ambient Waters by Off-line Chelation
Pre-concentration and Stabilized Temperature Graphite
Furnace Atomic Absorption 42
Fact Sheet No. 2.1.2-6 EPA Method No. 1638, Method Title: Determination of
Trace Elements in Ambient Waters by Inductively Coupled Plasma
— Mass Spectrometry 43
Fact Sheet No. 2.1.2-7 EPA Method No. 1640, Method Title: Determination of
Trace Elements in Ambient Waters by On-Line Chelation
Pre-concentration and Inductively Coupled Plasma-Mass
Spectrometry 45
Fact Sheet No. 2.1 2-8 EPA Method No 1632, Method Title: Inorganic Arsenic in
Water by Hydride Generation Quartz Furnace Atomic
Absorption 46
Fact Sheet No. 2 1.2-9 EPA Method No 1632, Revision A, Method Title: Chemical
Speciation of Arsenic in Water and Tissue by Hydride
Generation Quartz Furnace Atomic Absorption
Spectrometry 47
Fact Sheet No. 2.1.2-10 EPA Method No. 1636, Method Title: Determination of Hexavalent
Chromium by Ion Chromatography 48
Fact Sheet No. 2.1 2-11 EPA Method No. 1624b, Method Title: Volatile Organic Compounds
by Isotope Dilution GC/MS 49
Fact Sheet No 2.1.2-12 Method No. OERR SOP #2109, Method Title' Photovac GC
Analysis for Soil, Water, and Air/Soil Gas 50
Fact Sheet No. 2.1.2-13 EPA Method No. 1625, Method Title: Semi-volatile Organic
Compounds by Isotope Dilution GC/MS 51
Fact Sheet No. 2 1.2-14 Method Title Quantitative Determination of Polynuclear
Aromatic Hydrocarbons by Gas Chromatography/Mass
Spectrometry (GC/MS) - Selected Ion Momtonng
(SIM) Mode 52
Fact Sheet No 2 1.2-15 Method No LMMB 041, Method Title: Analysis of Polychlonnated
Biphenyls and Chlorinated Pesticides by
Gas Chromatography with Electron Capture Detection 53
Fact Sheet No. 2.1.2-16 Method No. LMMB, Method Title: PCBs and Pesticides in Surface
Water by XAD-2 Resin Extracton 54
Fact Sheet No. 2 1.2-17 EPA Method No. 1613, Method Title: Tetra- through
Octa-Chlormated Dioxms and Furans by Isotope Dilution
HRGC/HRMS 55
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A Compendium of Chemical, Physical and Biological Methods
for Assessing and Monitoring the Remediation of Contaminated Sediment Sites
February 17, 2003
Fact Sheet No. 2.1.2-18 EPA Method No 1668, Method Title: Toxic Polychlormated
Biphenyls by Isotope Dilution High Resolution Gas
Chromatography/High Resolution Mass Spectrometry ... 57
Fact Sheet No. 2.1 2-19 EPA Method No. 1668, Revision A, Method Title'
Chlorinated Biphenyl Congeners in Water, Soil, Sediment,
and Tissue by HRGC/HRMS 58
Fact Sheet No. 2.1 2-20 Method No ESS Method 220.3, Method Title. Ammonia Nitrogen
and Nitrate+Nitnte Nitrogen, Automated Flow
Injection Analysis Method 59
Fact Sheet No 2.1 2-21 Method No. ESS Method 230 1, Method Title- Total
Phosphorus and Total Kjeldahl Nitrogen, Semi-Automated
Method . . .. 60
Fact Sheet No. 2.1 2-22 Method No ESS Method 310.2, LMMB 064, Method Title.
Phosphorus, Total, Low Level (Persulfate Digestion) 61
Fact Sheet No. 2 1.2-23 Method No ESS Method 310 1, LMMB 063. Method Title:
Ortho-Phosphorus, Dissolved Automated, Ascorbic Acid ... 62
Fact Sheet No. 2 1.2-24 Standard Method No. 5310, Method Title: Total Organic
Carbon 63
Fact Sheet No. 2 1.2-25 Method No LMMB 096, Method Title Standard Operating
Procedure for the Analysis of Dissolved-Phase Organic
Carbon in Great Lakes Waters . 65
Fact Sheet No. 2.1 2-26 Method No. LMMB 097, Method Title-Standard Operating
Procedure for the Analysis of Particulate-Phase Organic
Carbon in Great Lakes Waters 66
Fact Sheet No. 2.1.2-27 Method No. ESS Method 140 4, Method Title: Chloride - Automated
Flow Injection Analysis ... .... . . . 67
Fact Sheet No. 2.1 2-28 Method No. ESS Method 200.5, Method Title: Determination
of Inorganic Anions in Water by Ion Chromatography 68
Fact Sheet No 2 1 2-29 Method No LMMB 092, Method Title: Standard Operating
Procedure for Electrometric pH . . 69
Fact Sheet No 2 1 2-30 Method No. LMMB 091, Method Title: Standard Operating
Procedure for GLNPO Total Alkalinity Titration ... 70
Fact Sheet No. 2.1.2-31 Method No. LMMB 094, Method Title: Standard Operating
Procedure for GLNPO Specific Conductance: Conductivity
Bridge . .. . .71
Fact Sheet No. 2.1.2-32 Method No LMMB 090, Method Title-Standard Operating
Procedure for GLNPO Turbidity. Nephelometenc
Method ' 72
Fact Sheet No 2.1.2-33 Method No. LMMB 065, Method Title: ESS Method 340 2
Total Suspended Solids, Mass Balance (Dried at
103-105°C) Volatile Suspended Solids (Ignited at 550°C) .. 73
Fact Sheet No. 2 1.2-34 Method No. LMMB 095. Method Title: Total Hardness
Titration . . 74
VI
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A Compendium of Chemical, Physical and Biological Methods
for Assessing and Monitoring the Remediation of Contaminated Sediment Sites
February 17, 2003
2.1.3 Biological Analysis Methods .75
Fact Sheet No. 2 1.3-1 Method No ERT SOP 2024, Method Title: Acute
Freshwater Crustacean Bioassay: 48 Hours 78
Fact Sheet No. 2 1.3-2 Method No ERT SOP 2022, Method Title: Acute
Freshwater Fish Bioassay 80
Fact Sheet No 2 1.3-3 Method No. ERT SOP 2027, Method Title: Chronic
Freshwater Algae Test 81
Fact Sheet No 2.1 3-4 Method No. ERT SOP 2025, Method Title: Chronic
Freshwater Crustacean Bioassay (7 Day) 83
Fact Sheet No 2.1 3-5 Method No. ERT SOP 2028, Method Title: Chronic
Freshwater Crustaceans Bioassay (10 days) 85
Fact Sheet No 2 1.3-6 Method No ERT SOP 2026, Method Title: Chronic
Freshwater Fish Bioassay 86
Fact Sheet No. 2.1.3-7 Method No NHEERL-AED SOP 1.03.001. Method Title:
Chronic Marine Macroalgae, Champia parvula, Sexual
Reproduction Test 87
Fact Sheet No. 2 1 3-8 Method No. NHEERL-AED SOP 1.03 003, Method Title:
Acute Marine Crustacean Bioassay 88
Fact Sheet No 2.1 3-9 Method No. NHEERL-AED SOP 1.03.003, Method Title:
Acute Marine Fish Bioassay 89
Fact Sheet No. 2.1.3-10 Method No. NHEERL-AED SOP 1.03.005. Method Title:
Chronic Estuarme Survival, Growth and Fecundity Test 90
Fact Sheet No. 213-11 Method No. NHEERL-AED SOP 1.03.006, Method Title:
Chronic Echmoderm Fertilization Test 91
Fact Sheet No. 2.1.3-12 Method No. NHEERL-AED SOP 1.03.004, Method Title:
Chronic Marine Fish Bioassay 93
Fact Sheet No. 2.1.3-13 Method Title Toxicity Evaluations of Photoinduction of Polycyclic
Aromatic Hydrocarbons (PAH): In Situ
Analysis 94
Fact Sheet No 2.1.3-14 Method Title- Toxicity Evaluations of Photoinduction of Polycyclic
Aromatic Hydrocarbons Laboratory Analysis of Storm water 95
Fact Sheet No 2.1.3-15 Method No. NHEERL-AED SOP 1.03013. Method Title.
Growth and Scope for Growth Measurements with
Mytilus edulis 96
Fact Sheet No. 2 1.3-16 Method No NHEERL-AED SOP 1.03.009, Method Title: Microtox®
tests 98
Fact Sheet No. 2.1.3-17 Comparative Toxicity of 2,3,7,8-Tetrachlorodibenzo-p-Dioxin
to Seven Freshwater Fish Species During Early Life-Stage
Development 99
2 2 Sediments
101
2.21 Field Sample Collection and Processing, In Situ Data Acquisition 101
Fact Sheet No. 2.2.1-1
Fact Sheet No 2.2.1-2
Fact Sheet No 2.2.1-3
Fact Sheet No. 2.2.1-4
Fact Sheet No. 2.2 1-5
Fact Sheet No. 2.2.1-6
Fact Sheet No. 2.2.1-7
Fact Sheet No. 2.2.1-8
Method Title Grab Sampling 102
Method Title: Core Samplers 106
Method Title: Hand Collection 110
Method Title Hand Collection at Depth with SCUBA
Equipment 111
Method Title Sediment Traps 112
Method Title: Russian Peat Borer 113
Method Title- Split Core Sampler for Submerged
Sediments 114
Method Title. Sediment Processing for Chemistry and
Toxicity Testing 115
VII
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A Compendium of Chemical, Physical and Biological Methods
for Assessing and Monitoring the Remediation of Contaminated Sediment Sites
February 17, 2003
Fact Sheet No 22.1-9
Fact Sheet No. 2.2.1-10
Fact Sheet No 2.2.1-11
Fact Sheet No. 2.2.1-12
Fact Sheet No. 2.2.1-13
Fact Sheet No. 22.1-14
Fact Sheet No. 2.2.1-15
Method Title Sediment Processing for Elutriate Toxicity
Tests . . . 116
Method No. ASTM E 1391-94, Method Title: Pore Water Extraction
through Centnfugation . 117
Method No ASTM E 1391-94, Method Title: Pore Water Extraction
from Sediments through Squeezing 118
Method No. ASTM E 1391-94, Method Title Pore water extraction
from sediment from Vacuum Filtration .... 119
Method No. DRP-2-03, Method Title: Acoustic Sub-bottom Profiling
Systems . .120
Method No. EEDP-01-10, Method Title- Side Scan
Sonar .... . 121
Method No. DRP-2-3, Method Title. Settlement Phases 122
2.22 Chemical and Physical Analysis . . .
123
Fact Sheet No. 2.2.2-1
Fact Sheet No. 2.2.2-2
Fact Sheet No. 2.2 2-3
Fact Sheet No. 2 2.2-4
Fact Sheet No. 2.2.2-5
Fact Sheet No 2.22-6
Fact Sheet No. 2.2.2-7
Fact Sheet No 222-8
Fact Sheet No. 2.2.2-9
Fact Sheet No. 2.2.2-10
Fact Sheet No. 2.22-11
Method No Appendix to Method 1631, Method Title: Total Mercury
in Sludge, Sediment, Soil, and Tissue by Acid
Digestion and BrCI Oxidation 124
Method Title-Trace Element Quantification Techniques . . 125
Method Title: Analysis of Marine Sediment and Bivalve
Tissue by X-Ray Fluorescence, Atomic Absorption and Inductively
Coupled Plasma Mass Spectrometry 127
Method Title. Determination of Acid Volatile Sulfide and
Selected Simultaneously Extractable Metals in Sediment... 129
Method No. OSWER SOP #2109 Method Title Photovac
GC Analysis for Soil, Water, and Air/Soil Gas . . 130
Method No. LMMB 040, Method Title Extraction and
Clean-Up of Sediments for Semi-volatile Organics
Following the Internal Standard Method 131
Method Title Quantitative Determination of Polynuclear
Aromatic Hydrocarbons by Gas Chromatography/Mass
Spectrometry (GC/MS) - Selected Ion Monitoring
(SIM) Mode . 133
Method No LMMB 041, Method Title Analysis of Polychlonnated
Biphenyls and Chlorinated Pesticides by
Gas Chromatography with Electron Capture Detection . 134
Method No. SW846 Method 4020, Method Title. Screening
for Polychlonnated Biphenyls by Immunoassay 135
EPA Method No. 1613, Method Title Tetra- through
Octa-Chlonnated Dioxins and Furans by Isotope Dilution
HRGC/HRMS 136
EPA Method No 1668, Method Title: Toxic Polychlonnated
Biphenyls by Isotope Dilution High Resolution Gas
Chromatography/High Resolution Mass Spectrometry . .. 137
vni
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A Compendium of Chemical, Physical and Biological Methods
for Assessing and Monitoring the Remediation of Contaminated Sediment Sites
February 17, 2003
Fact Sheet No 2.2 2-12 EPA Method No 1668 Revision A, Method Title
Chlorinated Biphenyl Congeners in Water, Soil, Sediment,
and Tissue by HRGC/HRMS 138
Fact Sheet No 2.22-13 Method Title Butyltin in Sediments 139
Fact Sheet No 2 2.2-14 Method Title: Procedures for Sediment Total Organic
Carbon (TOC) Determination 140
Fact Sheet No 2.2 2-15 Method No LMMB 084, Method Title. Determination of the Activity
of Lead-210 in Sediments and Soils 141
Fact Sheet No. 2.2 2-16 Method No. NHEERL-AED SOP 1.01.005, Method Title: Sediment
Gram Size Analysis 142
Fact Sheet No. 2.2 2-17 Method Title1 Procedures for Water Content
Determination 143
Fact Sheet No. 222-18 Method No ASTM D 2573, Method Title- Standard Test
Method for Field Vane Shear Test in Cohesive Soil 144
Fact Sheet No. 2.2 2-19 Method No ASTM D 854, Method Title' Standard Test
Method for Specific Gravity of Soil Solids by Water
Pycnometer 145
Fact Sheet No. 2.2.2-20 Method No. ASTM 2434, Method Title: Standard Test
Method for Permeability of Granular Soils (Constant Head) . 146
Fact Sheet No. 2.2.2-21 Method No ASTM 2435, Method Title. Standard Test
Method for One-Dimensional Consolidation Properties of
Soil 147
Fact Sheet No. 2.2.2-22 Method No. ASTM 2487, Method Title: Standard Test
Method for Classification of Soils for Engineering Purposes (Unified
Soil Classification System) 148
Fact Sheet No 2 2 2-23 Method No ASTM 4318, Method Title: Standard Test
Method for Liquid Limit, Plastic Limit, and Plasticity Index
of Soils 149
Fact Sheet No. 2.2 2-24 Method No. 4020, Method Title Field Portable X-Ray Fluorescence
Spectrometry for the Determination of
Elemental Concentrations in Soil and Sediment 150
Fact Sheet No. 2.2 2-25 Method Title. Sediment Age Dating Using Cesium-137 .... 151
Fact Sheet No. 2.2 2-26 Method Title: Berylhum-7 as a Tracer of Short Term Sediment
Deposition 152
223 Biological Analysis Methods . .. . 153
Fact Sheet No. 2.2.3-1 Method Title: Acute Freshwater Crustacean Sediment
Bioassay Flow-through 158
Fact Sheet No. 2.2 3-2 Method Title. Acute Freshwater Crustacean Sediment
Bioassay. In Situ Exposures 159
Fact Sheet No 2.23-3 Method Title Acute Freshwater Crustacean Sediment
Bioassay: Static Laboratory Exposures 160
Fact Sheet No 2 2 3-4 EPA Method No. 100.1, Method Title: Acute/Chronic
Freshwater Amphipod and Freshwater Insect Larvae
Sediment Bioassay 161
Fact Sheet No. 2 2 3-5 EPA Method No 100.4, Method Title: Chronic Freshwater
Amphipod Sediment Bioassay . 163
Fact Sheet No 2 2 3-6 EPA Method No. 100 5. Method Title. Life-Cycle
Freshwater Midge Sediment Bioassay 164
Fact Sheet No 2.2 3-7 Method Title: Acute Larval Bivalve Sediment
Bioassay 165
Fact Sheet No. 2.2 3-8 Method Title Acute Echmoderm Sediment
Bioassay 166
Fact Sheet No. 2 2.3-9 Method Title Acute Marine Crustacean Sediment
Bioassay . . 167
IX
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A Compendium of Chemical, Physical and Biological Methods
for Assessing and Monitoring the Remediation of Contaminated Sediment Sites
February 17, 2003
Fact Sheet No. 22.3-10
Fact Sheet No. 2 2.3-11
Fact Sheet No. 2.23-12
Fact Sheet No. 2.23-13
Fact Sheet No 2.2.3-14
Fact Sheet No. 22.3-15
Fact Sheet No. 2.2.3-16
Fact Sheet No. 2.2.3-17
EPA Method No 100.4, Method Title- Acute Marine
Amphipod Crustacean Sediment Bioassay 168
Method No ASTM E1611-00, Method Title-Acute Marine
Polychaete Sediment Bioassay .... 170
Method Title: Chronic Estuanne Am phipod Sediment
Bioassay 171
Method No ASTM E1611-00, Method Title- Chronic
Marine Polychaete Sediment Bioassay 172
Method Title. Ames Mutagenicity Assay
Method Title Mutatox Genotoxicity Assay
Method No. NHEERL-AED SOP 1.03.012, Method Title
V79/ Sister Chromatid Exchange Assay
EPA Method No 100 3, Method Title Bioaccumulation
Test for Marine, Estuanne and Freshwater Sediments .
2.3 Biota
2.3.1 Chemical and Physical Analyses
173
174
175
177
179
179
Fact Sheet No. 2.3.1-1
Fact Sheet No 2.3.1-2
Fact Sheet No. 2.3.1-3
Fact Sheet No 2.31-4
Fact Sheet No. 2.3.1-5
Fact Sheet No 23.1-6
Fact Sheet No. 2.31-7
Fact Sheet No 2.3.1-8
Fact Sheet No 2.3.1-9
Fact Sheet No. 2.3.1-10
Fact Sheet No. 23.1-11
Fact Sheet No. 2.31-12
Method No. LMMB 023, Method Title: Phytoplankton
Sample Collection and Preservation in the
Great Lakes . .. 180
Method No. LMMB 015, Method Title. Chlorophyll-a
Sampling Method and Preservation Field Procedure in the
Great Lakes 181
Method Title: Chlorophyll a and Phaeophytm Field Filtering Protocols
182
Method No LMMB 016, Method Title Primary Productivity
Using 14C Field Procedure in the Great Lakes 183
Method No LMMB 024, Method Title: Zooplankton Sample Collection
and Preservation in the Great Lakes 184
Method Title: Field-based Penphyton Survey in Wadeable StreaVBS
Method Title Laboratory-Based Penphyton Survey Single
Habitat Sampling in Wadeable Streams 186
Method Title: Laboratory-Based Rapid Penphyton Survey
Multi habitat Sampling in Wadeable Streams 187
Method Title Artificial Substrate Samplers of Macro-
invertebrates in Wadeable Streams . ... . 188
Method Title- Algae and Macro invertebrate Sampling with
Frames . 190
Method No NHEERL-AED SOP 1 02001. Method Title-
Benthic Organism Collection from a Marine
Environment . 191
Method Title Benthic Macromvertebrate Protocols in a
Wadeable Stream- Single Habitat Approach, 1-Meter
Kick Net . 192
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A Compendium of Chemical, Physical and Biological Methods
for Assessing and Monitoring the Remediation of Contaminated Sediment Sites
February 17, 2003
Fact Sheet No 2.3.1-13 Method Title Benthic Macromvertebrate Protocols in a
Wadeable Stream: Multi habitat Approach: D-Frame
Dip Net 193
Fact Sheet No. 2 3.1-14 Method Title: Photographic Habitat Documentation of the
Benthic Community 194
Fact Sheet No 2.3.1-15 Method Title: Sediment Profile Camera 195
Fact Sheet No 2.3 1-16 Method Title- Macromvertebrate Drift Nets in Wadeable
Streams 196
Fact Sheet No. 2.3.1-17 Method Title: Stream-Net Samplers: Surber, Portable
Invertebrate Box Sampler, Hess Sampler, Hess Stream
Bottom Sampler, and Stream-Bed Fauna Sampler 198
Fact Sheet No. 2.3.1-18 Method Title-Mussel Collection Using Brails 199
Fact Sheet No. 2.31-19 Method Title: Electrofishmg 200
Fact Sheet No. 2.31-20 Method Title Chemical Fishing 201
Fact Sheet No. 2.3 1-21 Method Title: Fish Collection Using Seme Nets 202
Fact Sheet No. 2.3.1-22 Method Title: Entanglement Nets 203
Fact Sheet No. 2.3.1-23 Method Title: Entrapment Devices ... 204
Fact Sheet No. 23.1-24 Method Title Pop Nets 205
Fact Sheet No. 2.3.1-25 Method Title. Trawls 206
Fact Sheet No 2 3 1-26 Method No LMMB 025, Method Title. Fish Processing
Method in the Great Lakes 207
Fact Sheet No. 2.3.1-27 Method Title- Fish Processing 208
Fact Sheet No. 2.3.1-28 Method Title. Swallows' Sampling Procedures 210
Fact Sheet No. 2.3.1-29 Method Title. Sample Processing of Swallows 211
2.3.2 Chemical and Physical Analysis . 212
Fact Sheet No. 2 3.2-1 Method Title. Sample Preparation for Metal Contaminants
in Tissue 213
Fact Sheet No 2 3.2-2 Method No. Appendix to Method 1631, Method Title- Total Mercury
in Tissue, Sludge, Sediment, and Soil by Acid
Digestion and BrCI Oxidation 214
Fact Sheet No. 2.3 2-3 Method No LMMB 052, Method Title Versatile
Combustion-Amalgamation Technique for the Photometric
Determination of Mercury in Fish and Environmental
Samples 215
Fact Sheet No 2.3.2-4 Method No NS&T, Method Title Trace Element
Quantification Techniques 216
Fact Sheet No. 2.3 2-5 Method Title: Analysis of Marine Sediment and Bivalve
Tissue by X-Ray Fluorescence, Atomic Absorption and
Inductively Coupled Plasma Mass Spectrometry . . ... 217
Fact Sheet No. 2.3.2-6 EPA Method No. 1632, Revision A, Method Title:
Chemical Speciation of Arsenic in Water and Tissue by
Hydride Generation Quartz Furnace Atomic Absorption
Spectrometry 218
FactSheetNo.2.32-7 Method No LMMB 043. Method Title: Extraction and Lipid Separation
of Fish Samples for Contaminant Analysis and
Lipid Determination 219
Fact Sheet No 2.3.2-8 Method No. NS&T, Method Title: Purification of Biological
Tissue Samples by Gel Permeation Chromatography of
Organic Analyses 220
XI
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A Compendium of Chemical, Physical and Biological Methods
for Assessing and Monitoring the Remediation of Contaminated Sediment Sites
February 17, 2003
Fact Sheet No. 2.3.2-9 Method Title: Quantitative Determination of Polynuclear
Aromatic Hydrocarbons by Gas Chromatography/Mass
Spectrometry (GC/MS) - Selected Ion Monitoring
(SIM) Mode 221
Fact Sheet No. 2.3.2-10 Method No. LMMB 041, Method Title: Analysis of
Polychlonnated Biphenyls and Chlorinated Pesticides by
Gas Chromatography with Electron Capture Detection . 222
FactSheetNo. 2 3.2.11 EPA Method No 1613. Method Title. Tetra- through Octa-Chlonnated
Dioxins and Furans by Isotope Dilution
HRGC/HRMS 223
FactSheetNo 23.2-12 EPA Method No 1668, Method Title. Toxic Polychlorinated Biphenyls
by Isotope Dilution High Resolution Gas Chromatography/High
Resolution Mass Spectrometry 225
Fact Sheet No. 2.3 2-13 EPA Method No. 1668 Revision A, Method Title-
Chlorinated Biphenyl Congeners in Water, Soil, Sediment,
and Tissue by HRGC/HRMS 226
Fact Sheet No. 2.3.2-14 Method Title1 Determination of Percent Dry Weight for
Tissues 227
Fact Sheet No 2.3 2-15 Method Title Determination of Percent Lipid in Tissue ... 228
Fact Sheet No. 2.3.2-16 Method Title: Microwave Extraction of marine Tissue for Semivolatile
Organic Analyte .. 229
233 Biological Analysis Methods 231
Fact Sheet No. 2.3.3-1 Method Title Laboratory Identification, Enumeration and
Biomass Measurements of Penphyton in Wadeable
Streams 232
Fact Sheet No. 2 3.3-2 Method Title: Laboratory Periphyton Biomass
Determination 234
Fact Sheet No. 2.3.3-3 Method Title1 Laboratory Analysis of Benthic Macro-
invertebrates in Wadeable Streams 235
FactSheetNo 23.3-4 Method Title Laboratory Analysis of Water Column
Organisms. 237
Fact Sheet No 2.3.3-5 Method No LMMB 026 - Appendix 2 & LMMB 027 -
Appendix B, Method Title SOP-2' Lab Analysis of Lake
Trout Stomachs and Data Entry, Appendix B. Standard
Operating Procedure for Lab Analysis of Coho Salmon
Stomachs and Data Entry 239
Fact Sheet No. 2 3.3-6 Method Title: Gonadal Analysis .... 240
Fact Sheet No. 2.3.3-7 Method Title1 Histopathological Evaluations of Target and
Non Target Fish Species . . . 241
Fact Sheet No. 2.3.3-8 Method No NS&T. Method Title: Histopathology
Analysis .... . . 242
Fact Sheet No 2.3.3-9 Method Title- Index of Biotic Integrity (IBI) 243
Fact Sheet No. 2.3.3-10 Method Title. Fish Bioassessment I and II 244
3 0 References .... .. ... 245
Index 252
xn
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TABLES
Table 2 1.1-1. A Summary of Sample Sizes, Containers, Preservation Techniques, and
Holding Times for Water 22
Table 2.1.3-1. A Summary of Test Types and lexicological Endpomts for Liquid-Phase
Toxicity 76
Table 2.2.1-1. A Summary of Sediment Grab Devices 104
Table 2.2 1-2 A Summary of Sediment Coring Devices 108
Table 223-1 A Summary of Test Types and Toxicological Endpomts for Solid-Phase
Toxicity 154
Table 231-1 A Summary of Stream Net Samplers Used to Collect Organisms from
Flowing Water 197
Xlll
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Table of Acronyms
ADCP
AVS
AWQC
BAFS
BSAFS
CAD
CB
CDD
CDF
CHV
COC
CVAA
CVAFS
CTD
CWT
DBT
DCM
DMA
DO
DOC
EGD
EICP
EMAP
EMDL
ERL
ET
FAA
4BT
GC
GC/ECD
Acoustic Doppler Current Profiler
Acid Volatile Sulfide
Ambient Water Quality Criteria
Bioaccumulation Factors
Biota-Sediment Accumulation Factors
Confined Aquatic Disposal
Chlorinated Biphenyl
Chlorinated Dibenzo-p-dioxms
Chlorinated Dibenzofurans
Chronic Value
Constituents of Concern
Cold Vapor Atomic Absorption
Cold Vapor Atomic Fluorescence Spectrometry
Conductivity, Temperature, Depth
Coded Wire Tags
Dibutyltm
Dichloromethane
Dimethylarsmic Acid
Dissolved Oxygen
Dissolved-phase Organic Carbon
Effluent Guidelines Division
Extracted Ion Current Profile
Environmental Momtonng and Assessment Program
Estimated Method Detection Limit
Effects Range Low
Ecotox Threshold
Flame Atomic Absorption
Tetra Butyltm
Gas Chromatography
Gas Chromatography using Electron Capture Detection
XIV
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GFAA
GPC
HIB
HOC
HPLC
IA
IBI
1C
ICI
ICP-MS
INAA
IR
LC50
LIR
LOEC
MBT
MDL
ML
MMA
MS
NOEC
NPDES
NTU
PAH
PAR
PCB
POC
PSDDA
RBP
SAI
SCE
Graphite Furnace Atomic Absorption
Gel Permeation Chromatography
Hilsenhoffs Family Biotic Index
Hydrophobia Organic Contaminants
High-performance Liquid Chromatography
Inorganic Arsenic
Index of Biotic Integrity
Ion Chromatography
Invertebrate Community Index
Inductively Coupled Plasma Mass Spectrometry
Instrumental Neutron Activation Analysis
Infrared
Lethal Concentration for 50%
Load Increment Ratio
Lowest Observable Effects Concentration
Monobutyltm
Method Detection Limit
Minimum Level
Monomethylarsonic Acid
Mass Spectrometer
No Observable Effects Concentration
National Pollutant Discharge Elimination System
Nephelometenc Turbidity Units
Polycyclic Aromatic Hydrocarbons
Photosynthetically Active Radiation
Polychlonnated Biphenyl
Particulate-phase Organic Carbon
Puget Sound Dredged Disposal Analysis
Rapid Bioassessment Protocols
Simple Autecological Indices
Sister Chromatid Exchange
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SDS
SEC
SEM
SFG
SIM
SOP
SPE
SPI
SPM
STPGFAA
TBT
TEC
TIC
TIC
TOO
TCD
VSS
XRF
Soxhlet/Dean -Stark
Sediment Exposure Chamber
Simultaneously Extracted Metal
Scope For Growth
Selected Ion Monitoring
Standard Operating Procedure
Solid-phase Extraction
Sediment Profiling Imaging
Settling Particulate Matter
Stabilized Temperature Platform Graphite Furnace Atomic Absorption
Tributyltm
Threshold Effects Concentrations
Tentatively Identified Compounds
Total Inorganic Carbon
Total Organic Carbon
Thermal Conductivity Detection
Volatile Suspended Solids
X-Ray Fluorescence
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1.0 INTRODUCTION
1.1 Background and Objectives
The extent and severity of chemical contaminants in freshwater and marine sediments and their
impacts on ecological and human health have been studied by EPA and other federal, state,
tribal, and local organizations for over the past 30 years. Over this period of time, field and
laboratory tools and techniques have continuously improved and new methods have developed,
and a body of institutional knowledge has been accumulated and refined regarding suitable
methods for sample collection and field processing, laboratory processing and chemical analysis,
and toxicology testing and bioaccumulation or other effects studies. This body of knowledge
comprises methods manuals, guidance documents, standard methods, and published
governmental reports, as well as published manuscripts in the scientific literature.
To disseminate information about current EPA methods and research on contaminated
sediments, EPA assembled this compendium of methods. Methods presented focus primarily on
published or otherwise citeable chemical, physical, and biological (toxfcity and bioassessment)
testing methodologies used by EPA at Superfund sites to determine the effects of chemical
contaminants on aquatic life and human health. Although priority is given to those methods that
have demonstrated efficacy at Superfund sites, the document also includes methods employed by
other EPA and other federal and state programs at non-Superfund contaminated sediment sites.
The following agencies and programs have contributed significantly to the study of contaminated
sediments and are the source of many of the methods or secondary references contained in this
compendium.
Federal
Environmental Protection Agency
Office of Research and Development
Office of Water
Office of Science and Technology
Office of Wetlands Oceans and Watersheds
Office of Wastewater Management
Office of Solid Waste and Emergency Response
Office of Pollution Protection and Toxics
Office of Pesticide Programs
Great Lakes National Program Office
National Oceanic and Atmospheric Administration
National Status and Trends Program
• Hazardous Material and Response Division
Damage Assessment and Remediation Program
U.S. Army Corps of Engineers
Waterways Experiment Station
New England Division
Seattle District
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U.S. Navy
U.S. Fish and Wildlife Service
U.S. Geological Survey/National Biological Survey
Interaaencv
National Dredging Team
Puget Sound Dredged Disposal Analysis (PSDDA) Program
Considering the many organizations which have published methods for monitoring contaminated
sediments and the large number of documents on this subject, it can be a formidable task for a
Superfund project manager to find methods appropriate for his or her contaminated sediment site.
To the best of our knowledge, no compilation of such methods has been prepared to date. This
document summarizes many of the published methods from these agencies and programs related
to the characterization of contaminated sediments and contaminated sediment sites. Additionally,
related methods published as American Society for Testing and Materials Standards or Standard
Methods for the Examination of Water and Wastewater (APHA 1999) are also included, as
needed, to provide complete information in certain topic areas. Where a number of methods are
available for a given monitoring activity, not all methods will necessarily be included In this
document. If an EPA method is available, it will generally be given priority for inclusion. A method
published by another Federal agency will often be included If it is significantly different from the
EPA method or if an EPA method is not available. Methods published by other sources may be
included if Federal methods are not available or if the methods have special merit.
The compendium is divided in four sections. The first section addresses the application and uses
of monitoring data. While many of the monitoring methods have been developed for purposes
other than monitoring at Superfund sites, the first section addresses applications within the
Superfund decision making process, and not the broader area of marine or aquatic environmental
monitoring. The monitoring methods are presented in three sections by the matrix being
monitored — water, sediment, and biota. Each of these sections contains separate subsections
on sampling methods and immediate field processing, chemistry and physical analysis methods,
and biological analysis methods. In situ data collection methods are presented in the sampling
methods section. Some of the methods, particularly the chemistry methods, are applicable to
more than one matrix and, thus, have been presented more than once. Effort has been made in
these cases to reduce redundancy as much as possible.
1.2 Application and Uses of Field, Analytical, and Testing Data at Superfund Sites
Containing Contaminated Sediments
The collection of chemical, physical, and biological data at Superfund sites containing
contaminated sediments is used to support human health and ecological risk assessment. To
support human health risk assessment, the contaminated media to which humans may be
exposed must be characterized. Exposure may be through routes such as ingestlon of (the edible
portions of) contaminated fish and shellfish, mgestion of contaminated drinking water, and dermal
contact during swimming and wading. (Monitoring to characterize air, terrestrial species and avian
species impacted by contaminated sediments is, with few exceptions, not addressed by this
document.) More monitoring methods may be needed to support ecological risk assessment than
to support human health risk assessment because of the variety of biota and the complexity of
interactions involving contaminants and aquatic ecosystems.
Monitoring and monitoring data are important during the decision making process, which includes
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the following activities:
• Site Assessment (including Preliminary Assessment and Site Inspection)
• Planning and Implementing Removal Actions
• Remedial Investigation and Risk Assessment
• Feasibility Study/Remedy Selection (following NCP criteria as the basis for decision
making)
• Remedy Implementation and Monitoring Recovery
Remedial Investigation and Risk Assessment
During the initial site assessment, remedial investigation information on the extent and magnitude
of chemical contamination at the site is obtained. At contaminated sediment sites, water and
sediment samples are often collected and analyzed for Constituents of Concern (COCs).
Because the toxicity of many contaminants is dependent upon physical properties of media , as
well as the potential receptors, additional chemical, physical, and biological parameters are also
collected; for example:
Water- hardness, alkalinity, pH, suspended organic matter, dissolved oxygen level,
dissolved organic matter, salinity, temperature, depth
Sediment - pH, total organic carbon, clay content and type, grain size distribution,
redox potential, depth of sample
Habitat structure - bottom characteristics, grain size distribution, cobbles, boulders,
benthic community structure, fish community structure, vegetation, and debris, among
others
Data on the presence of endangered or threatened species, sensitive species, and species of
economic or recreational importance, and information on critical or sensitive habitats are also
collected.
These data will be used in the development of a screening-level problem formulation and
ecological effects evaluation and screening-level preliminary exposure estimates. Often,
appropriate Ecotox Thresholds (ETs) will be used during the preliminary stages. ETs are defined
as media-specific contaminant concentrations above which there is sufficient concern regarding
adverse ecological effects to warrant further site investigation (USEPA 1996a). At contaminated
sites, the benchmarks commonly used to assess preliminary risk (establish the ETs) include:
Water - National Ambient Water Quality Criteria (AWQC). Water quality for both
water and pore water is evaluated by comparison to AWQC for protection of aquatic
life as specified by USEPA in numerous guidelines. These criteria, most recently
updated in 1999 (USEPA 1999a), are intended to accurately reflect the latest
scientific knowledge of the effects of these chemicals on aquatic life. The current
AWQC list recommended criteria for 157 pollutants.
Sediment- (1) Effects Range Low values (ERL) (Long and Morgan 1990, USEPA
1992a, Long et al. 1995); (2) Threshold Effects Concentrations (TECs) (MacDonald
et al., 2000). ER-Ls have been developed from correlated biological and chemical
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data from laboratory and field studies combined with modeling studies representing
marine and estuanne environments. TECs for 28 chemicals can be used to screen
freshwater sediment for risk to benthic organisms but are not necessarily protective
of higher trophic level organisms.
EPA Superfund has developed an ET program that calculates site-specific ETs by adjusting for
pH and hardness in surface water and TOC in sediments (USEPA 1996a). The ET calculations
use as a baseline the risk-based benchmarks referenced above.
During the screening-level problem formulation/ecological effects evaluation and again during the
risk characterization, the ecological significance of potential ecological receptors, as described in
the Ecological Risk Assessment Guidance for Superfund (USEPA 1997a) is also estimated.
During the problem formulation phase, ecological attributes that will function as assessment
endpoints are identified and an assessment of the proposed endpoints is made that will help
determine risk.
During problem formulation, the significance of adverse lexicological, biological, and ecological
effects to receptors is considered as part of the selection process for assessment endpoints.
Examples of endpoints for contaminated sediment sites include:
• Individual Level -Endangered or threatened species known to be present
Population Level - Sensitive fish population, sensitive macroinvertebrate population, or
sensitive bird population exposed to COCs
Community Level - Distribution and abundance of fish and avian communities, benthic
macroinfauna communities, and aquatic plant communities
Distinguishing potential and current adverse effects due to releases of contaminants at population
and community levels from normal fluctuations requires knowledge of the natural variability
inherent in the ecosystem (population fluctuations, presence/absence, abundance, and diversity).
During the risk characterization phase, the likelihood, duration, and magnitude of risk to the
receptors represented by assessment endpoints, the spatial and temporal extent of the risk, and
the estimation of COCs below which contaminants would no longer be of concern are all
developed. As presented in USEPA 1994a, candidate assessment endpoints in field studies at
contaminated sediment sites can include
Type
Populations
Measurement Endpoint
Survival and reproduction of fish
Survival, growth, and reproduction of aquatic
insect eating or fish-eating birds and
mammals
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Communities
Biomass
Productivity and respiration
Species richness
Species density
Relative abundance
Dominance
Diversity
Evenness
Similarity/difference between Superfund site
and reference site
Similarity/difference in guild structure between
Superfund site and reference site Presence,
absence, or population density of indicator
species
The types of organisms/data collected and methods that may be used for collection include
Biota
Method
Penphyton
Scraping
Coring (or sampling with a grab)
Suction
Artificial substrate
Plankton
Trapping
Pumping
Netting (towing)
Water sampling
Benthic Macroinvertebrates
Dredging or digging
Stream netting, sweep netting
Coring (or sampling with a grab)
Artificial substrate
Fish
Seining
Trawling
Passive netting (gill, trammel, or hoop nets)
Electrofishing
Chemical collection
Birds
Auditory and visual studies
Nesting success
Trapping
Additionally, sediment toxicity tests provide another mechanism to determine if contaminated
sediments are causing adverse effects in organisms in a controlled laboratory setting. The tests
that are commonly used for testing contaminated sediments include, aquatic, sediment, and
microbial tests. Many are highly standardized and have the advantage of wide acceptance.
Standardization has also resulted in the advantage of multiple laboratories with qualifications to
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perform the testing. Aquatic toxicity tests include both freshwater and marine acute and chronic
toxicity tests. Freshwater and marine sediment toxicity tests include acute and chronic tests of
whole sediment or sediment interstitial water.
Several USEPA and other agency documents establishing testing methods for the suitability of
dredged material for disposal in the marine and freshwater environments have been prepared
(USEPA/USACE 1991, USEPA/USACE 1992, USEPA/USACE 1998, USEPA 1994a, USEPA
2000a, USACE/WDNR/WDEC 2000). While these documents do not specifically address the
Superfund program, they present the various approaches taken for the management of
contaminated sediments, including the use of both sediment chemistry and toxicity data in
contaminated sediment evaluation.
Remedy Selection/Feasibility Studies
While monitoring and field data acquisition can occur in the above phases of the Superfund risk
assessment process, the field data will also need to be acquired for the remedy selection. The
remedies to be considered at contaminated sediment sites include
Monitored natural recovery
Containment in-place (in situ capping)
Treatment in-place
Removal and disposal of contaminated sediments in confined aquatic disposal (CAD)
facility
Removal and upland containment.
The extent to which one of these remedies is superior needs to be determined on a case by case
basis based on site data, appropriately acquired following sound project planning and the
application of sound monitoring methods and data assessment techniques. As presented in
Sediment Management Work Group (1999), the appropriate questions that need to be answered
to guide remedial at contaminated sediment sites include
• How long will it take natural recovery to return the site to acceptable conditions?
• Will dredging and removal accelerate this process?
• Will other remedial options (i.e., capping) accelerate the process?
• What are the risks (for example, from large storm events) of leaving the contaminated
sediment in place, or of removing the engineered clean sediment cap?
The answers to the above questions can be derived from an understanding of the site from site
characterization studies, the appropriate application of transport and fate models and ecological
and human health risk assessments, leading to the development of a site conceptual model of the
transport and fate of COCs at the site that will lead to a risk-based remedy decision.
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Specific site condition information needs to be collected and evaluated when considering an in situ
capping remediation alternative at contaminated sediment sites, including:
• Physical environment - For example, bathymetry will influence the ability to place an in
situ cap in many areas and will also influence dispersion at the site during dredging or
capping. Bottom slope needs to be considered. Moderate slopes can rule out the
ability to cap without the placement of a physical barrier to prevent downslope
movement.
• Hydrodynamic conditions - Stability of the cap over time (typically 30 years) needs to
be determined. This determination will require data such as normal water column
currents or channel flow, tidal fluctuations, wave and storm induced bottom currents, or
flow during flood conditions need to be considered. Some of these data will feed into
modeling studies, which may be needed to understand conditions at open water sites.
Hydrogeological conditions - Groundwater discharge to near shore areas of lakes,
rivers and estuaries is common in many areas of United States and groundwater flow
through a contaminated sediment site can transfer a fraction of the contaminants to
the overlying surface water. In this circumstance, a determination of the magnitude of
groundwater flow and thickness of the contaminated layer should be made.
Additionally, data on sediment physical characteristics, such as water content, grain
size and clay content and type, organic content, plasticity indices, and specific gravity,
are also required to evaluate site conditions and cap design. Engineering
measurements of sediment shear strength and compressibility are also required.
Monitoring activities associated with the evaluation of fate and transport processes for site
assessment, risk characterization, remedy selection, or post remedy monitoring can include those
with the purpose of:
• Characterizing stream flow and the potential for sediment deposition and/or scouring
• Assessing naturally occurring biodegradation of contaminants (which may include
methods to characterize sediment geochemistry, biodegradation products, microbial
populations, chiral analytes, efc.)
• Assessing diffusive transport of contaminants through sediments to the water column
Assessing water flow across the sediment/water column interface
• Assessing the consolidation of sediments resulting from compressive forces and
biodegradation
• Determining changes in the location of the sediment/water interface
• Assessing the mobility of contaminants (e.g., speciation methods for metals, total
organic carbon, acid volatile sulfides, pH, redox potential, efc.)
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• Characterizing the physical characteristics of sediments (e.g., sediment cohesion,
shear strength, particle size distribution, etc.)
Monitoring activities facilitating the implementation of remedial actions can include those with the
purpose of:
• Evaluating monitored natural recovery (e.g., by decrease in concentrations of COCs,
decrease in toxicity
• Facilitating installation of in situ caps
• Determining the long-term performance and condition of in situ caps (e.g., by
measuring cap thickness over time, measuring COCs in sediment cap porewater over
time)
• Evaluating aquatic system recovery following installation of in situ caps
• Facilitating remedial dredging
• Evaluating aquatic system recovery following completion of remedial dredging
• Ensuring that remedial construction activities do not have the potential to produce and
are not producing immediate adverse effects (e.g., by monitoring turbidity, dissolved
oxygen, acute toxicity testing)
The methods presented in the next several sections are frequently used for assessment of
environmental conditions at contaminated sediment sites and provide data to address many of the
data uses described above. Many of these methods were originally developed for the analysis of
water and wastewater or for the analysis of solid waste have been used without modification for
marine or aquatic investigations. Other methods originally developed for those purposes have
been modified for contaminated sediment investigations, often to lower detection limits needed for
risk assessments or to facilitate working with a high salinity water or sediment matrix. However,
many of the methods were specifically developed for working in the aquatic or marine
environment at contaminated sites, and elsewhere. Without exception, it is intended that all of the
methods presented will be suitable for investigations at Superfund sites containing contaminated
sediments. However, not all methods will be suitable for all sites. The selection of methods for a
particular site will depend on the site conditions, remediation plans, budgetary constraints and
other factors.
2.0 MONITORING METHODS
2.1 Water
Water sample collection methods, and chemical, physical, and biological analyses have
continuously been developed and implemented over the years to evaluate the health of our
nations streams, lakes, rivers, ponds, creeks, lagoons, estuaries, oceans and surface
impoundments.
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At Superfund sites, water samples are specifically collected with the following objectives in mind
(USEPA. 1994a):
To determine if the contaminant is hazardous by identifying its composition and
characteristics,
To determine if there is an imminent or substantial threat to public health or welfare or
to the environment;
To determine the need for long-term action;
To develop containment and control strategies;
To evaluate appropriate disposal/treatment options; and,
To verify treatment goals or clean up levels.
In order to achieve the aforementioned objectives, field sampling and analytical strategies are
designed to provide site-specific information because characteristics and sampling strategies vary
widely. The following fact sheets relating to water are divided into sections pertaining to field
sample collection and processing, chemical and physical laboratory analyses and biological
laboratory analyses. These fact sheets intend to provide Superfund managers with a summary of
the existing methods that may be applicable to their site, their relative strengths, and their relative
weaknesses.
2.1.1 Field Sample Collection and Immediate Processing, In Situ Data Acquisition
Section 2.1.1 presents methods for field sample collection, field or immediate sample processing,
and in situ data acquisition. In situ data acquisition primarily collects those data easily and
economically collected with various sensors and includes parameters such as salinity,
conductivity, temperature, pH, dissolved oxygen, light transmission, and light attenuation. Data
collection in situ is often automated and allows for data acquisition over broad spatial and
temporal scales. Because many biological processes in the environment are affected, directly or
indirectly, by the physical characteristics of the environment, the data collected in situ are vital in
site assessments at aquatic sites. Water samples are also collected in numerous ways and
brought back to the laboratory to identify chemical contaminants that may disrupt existing physical
and biological processes and what effects those chemical contaminants may have on resident
organisms. These samples and analyses are crucial in determining potential exposure pathways
based on the concentration of the chemical in the environment and then the chemical's behavior
in the environment based on biological, chemical, and physical parameters. Measurement and
collection methods vary based on the characteristics of the water body in question. Therefore,
numerous methods are provided.
Many of the field sampling and data collection methods for water are routinely performed to
evaluate the health and biological integrity of our surface waters. Thus, they originate from
programs unrelated to contaminated sediments. Many of the methods have been taken from
USEPA Environmental Monitoring and Assessment Program documents. Other sources of
methods for water column field collection include:
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• The USEPA and the Puget Sound Water Quality Action Team
• The USEPA's Lake Michigan Mass Balance Study Methods Compendium
• The USEPA's Environmental Response Team
• The USEPA's Environmental Research Laboratory-Narragansett
• Standard Methods for Examination of Water and Wastewater
• ASTM
• Journal publications
The USEPA's Rapid Bioassessment Protocols
10
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Fact Sheet No
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1 1-1
In Situ Sampling with the Hydrolab Datasonde3*Unit
This procedure describes one of several CTD devices used to collect high-quality in
situ data for salinity, temperature, dissolved oxygen (DO) concentration, pH, and
water depth
The Hydrolab DatasondeS® unit is one of several commercial units that collect in
situ Conductivity, Temperature, and Depth (CTD) data, and also measures pH and
DO to obtain a vertical profile of water column conditions.
After calibration, the Hydrolab is connected to a winch cable, and the protective
covers on the probes are removed and the stirrer is connected The unit is lowered
over the side and allowed to equilibrate at the surface for at least two minutes
While the unit is equilibrating, a QC check is performed with a YSI DO probe,
refractometer and a thermometer to ensure that the readings from all equipment
agree.
The Hydrolab unit is lowered at intervals specific to the relative depth of the site,
allowing the unit to stabilize at each specified stop during descent. Data can be
acquired on the descent and ascent
Salinity, conductivity, temperature and dissolved oxygen parameters are commonly
collected at all stations where samples for water quality are collected.
The Hydrolab is a relatively small unit that may be hand deployed, if necessary.
The Hydrolab is much more expensive than alternate sampling equipment such as
the YSI data probe, refractometer and thermometer Without proper calibration, the
Hydrolab or other CTD units may record erroneous information.
Strobel, C J 2000 Coastal 2000 - Northeast Component: Field Operations Manual
U.S. Environmental Protection Agency , National Health and Environmental Effects
Research Laboratory, Atlantic Ecology Division, Narragansett, R.I EPA/620/R-
00/002.
http //www epa qov/emap/nca/html/docs/c2knefm Last Accessed: 1/31/2003
html
II
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1 1-2
In Situ Dissolved Oxygen Sampling with a YSI Model 58 Dissolved Oxygen Meter
and Probe
This method describes the use of a YSI Dissolved Oxygen Meter and Probe to take
in situ oxygen measurements in the water column.
After checking the batteries and replacing the probe membrane, the YSI Model 58
Dissolved Oxygen(DO) Meter and Probe must be calibrated before sampling at
each station. The meter is then set to 0.1 mg/L mode If measuring the DO in other
than surface water, collect water in a Go-Flo® bottle Measure the salinity with a
refractometer Insert the stirrer-probe unit directly into the Go-Flo bottle and turn on
the stirrer. When the meter reading has stabilized, record the oxygen value on the
data sheet. Turn the stirrer off, rinse the probe with freshwater, and store the unit
out of sunlight
DO is an important water quality parameter for surface water aquatic life. The YSI
Model 58 Dissolved Oxygen Meter and Probe can be used to take oxygen
measurements at the surface as a Quality Control check on DO measurements
determined by other methods. Probes are used mainly on in situ instruments for
providing continuous water-column profiles of dissolved oxygen.
The YSI Model 58 Dissolved Oxygen Meter and Probe is small and transportable It
is a good, quick way to check on the accuracy of the Hydrolab. The measurement
of DO directly in sampling bottles reduces sampling bias associated with sample
transfer.
The device must be calibrated at every station prior to use. The device could
produce erroneous data if the mem brane is at all damaged or dried out The probe
method is not commonly used for oceanographic studies in which measurements
are made on discrete samples of seawater
Strobel, C J 2000 Coastal 2000 - Northeast Component: Field Operations Manual
U.S. Environmental Protection Agency , National Health and Environmental Effects
Research Laboratory, Atlantic Ecology Division, Narragansett, R.I. EPA/620/R-
00/002.
http //www epa gov/emap/nca/html/docs/c2knefm html Last Accessed
1/31/2003
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.1-3
In Situ Irradiance Measurements
This method describes the manner in which a vertical profile of light intensity can be
measured for the purpose of calculating a light attenuation coefficient at each
station.
Photon flux, or Irradiance is the amount of light that diffuses the water referenced to
the input. Photosyn (helically active radiation (PAR) is measured to determine the
absorption rate of that light by phytoplankton.
To obtain a PAR profile, a deck sensor and an underwater sensor are connected to
an independent data logger The deck sensor is placed in a location where it is not
shaded. The underwater sensor is lowered on the sunny side of the boat to a depth
of about 10 cm (representing surface). Record the values from both sensors.
Lower the underwater sensor to 0.5 meters and record the values. Then lower the
sensor at given intervals depending on the relative depth of the sampling location
and record the values. Repeat the process on the upcast.
PAR is important in understanding the dynamics of the "photic zone" which helps to
understand lake health issues such as photosynthesis, and toxic algae blooms and
eutrophication. Irradiance and PAR are measured for the purpose of calculating a
light attenuation coefficient at each station which can be used in productivity
assessments or for site assessments
PAR sensors require no field calibration, but they should be returned to the
manufacturer prior to each field season for annual calibration. PAR sensors provide
more quantitative data to derive light attenuation data in a more exact manner.
PAR sensors are more expensive than other light attenuation methods.
Strobel, C.J. 2000 Coastal 2000 - Northeast Component: Field Operations Manual
U.S. Environmental Protection Agency , National Health and Environmental Effects
Research Laboratory, Atlantic Ecology Division, Narragansett, R.I. EPA/620/R-
00/002
http //www epa qov/emap/nca/html/docs/c2kn
efm html
Last Accessed: 1/31/2003
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2 1.1-4
In Situ Transparency Measurements, Secchi disk profile
This method describes the manners in which a vertical profile of light can be
measured for the purposes of determining water column transparency.
To obtain a Secchi profile, a 20 cm black and white Secchi disk ts lowered until it is
no longer visible. Note the depth using the markings on the line. Slowly raise the
disk until it just becomes visible and note the depth Repeat this process 3 times and
record the average of the readings.
The Secchi disk measures water column transparency and may be best used when
transparency is high
The Secchi disk can be used on any vessel, and computer data loggers are not
necessary.
Secchi disks data may vary amongst investigators. More room for human error
PSWQAT. 1997 Recommended Guidelines for Sampling Marine Sediment, Water
Column, and Tissue in Puget Sound, Puget Sound Protocols and Guidelines. Puget
Sound Water Quality Action Team, Olympia, WA.
http-//wwwosat.wa qov/Publications/ Last Accessed: 1/31/2003
protocols/protocol html
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Fact Sheet No
Method Title
Purpose
Method Summary
Data
Uses/Application
21 1-5
Sample Collection Procedures for Marine Water
This method describes the methods and different type of water bottles used to
collect marine water column samples
Water samples should be collected prior to "bottom related" activities (sediment
grabs and trawling) to assure that bottom sediments are not re-suspended. These
samples should also be collected on a day when it is possible to ship samples on
the same or following day to meet toxicity testing holding times, if necessary.
The typical water bottle sampler consists of a cylindrical tube with stoppers at each
end, and a closing device that is activated from the surface by a messenger or an
electrical signal Multiple water samplers can be attached sequentially to a vertical
hydrowire for sampling at multiple depths on a single cast, or they can be mounted
on a rosette frame (see fact sheet 2.1 .1 .-6, often in conjunction with an in situ sensor
array) which allows for collection of replicate samples at the same depth.
After the sampler is cocked, it is lowered to a designated depth Avoid deploying
water bottles in surface slicks as these can contaminate samples with organic
compounds. If contamination by the micro-layer is of concern, use samplers that are
designed to remain closed until they have descended below the microlayer (i.e., Go-
Flo™ bottle from General Oceamcs, Inc. Miami, Florida). Teflon™-lmed Go-Flo™
bottles are recommended when sampling marine water that will be analyzed for
ambient or trace levels of mercury or other metals upon proper cleaning Niskm
bottles are also often used to collect water samples, however these bottles remain
open as they descend through the water column, and the enclosure mechanism is
on the inside of the bottle, making them difficult to clean.
Once the sampler reaches the desired depth, it should be allowed to equilibrate to
ambient conditions for approximately 1 minute before it is closed. If reversing
thermometers are involved, equilibration should be 5 minutes. After equilibrium, the
closing device is activated by a messenger or electric signal, and the sampler is
retrieved. To ensure that all samples are truly representative of the water column
within a specific water parcel, it is advisable that they be collected from a single cast.
As the water samplers are being brought on board, each bottle should be checked
immediately for leakage of sample water around the seals. If the sample has been
compromised, the cast should be repeated.
Water bottle samplers are used to collect water column samples for laboratory
analyses of conventional, metals, orgamcs and microbiological analytical
procedures and toxicity tests
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Advantages
Limitations
Reference
Website
21.1-5{contd.)
Both Niskm and Go-Flo bottles can be deployed individually or attached to a large
rosette sampler which collects in situ data while water samples are being collected.
The Go-Flo design allows it to be deployed (and returned) in the closed position,
reducing the possibility of sample contamination from surface slicks and the
microlayer. These bottles also have external springs therefore there is no risk of
sample contamination The Go-Flo bottles are commonly used to collect samples
later analyzed for metals or organics.
The EMAP Program provides similar guidance regarding marine water collection
(USEPA, 1990a).
Holding times for collecting samples must be observed. Niskm bottles are generally
not used to collect samples later analyzed for sensitive organics or metal analyses
since they are deployed in the open position and the spring used to close the cap is
located on the inside of the bottle
PSWQAT. 1997 Recommended Guidelines for Sampling Marine Sediment, Water
Column, and Tissue in Puget Sound, Puget Sound Protocols and Guidelines Puget
Sound Water Quality Action Team, Olympia, WA.
httpV/wwwDsat wa aov/Publications/p Last Accessed: 1/31/2003
rotocols/protocol html
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.1-6
Field Sampling Using Rosette Sampler, LMMB 013
This procedure describes the collection of water samples using a Rosette Sampler.
The Rosette sampler is the primary sampling instrument for the collection of all
nutrient parameters, phytoplankton, chlorophyll a, Phaeophytm a, and dissolved
oxygen, temperature, total suspended solids, turbidity, specific conductance, and
pH
The system consists of 12 water sampling bottles (8 L Niskm or Go-Flo bottles), a
CTD (conductivity, temperature and depth sensor) attached at the bottom of the
Rosette, an A-frame, a multiconductor cable, a variable speed winch, and a deck
unit with attached computer The bottles can be closed in any predetermined order,
remotely from the deck of the vessel while the array is submerged at the various
sampling depths The CTD is built to provide real time information on a number of
water quality parameters as it moves through the water column. During sampling,
the Rosette/CTD system is lowered to the bottom to define the temperature profile of
the water column The sampling depths are then selected. After collection of
samples with the Rosette sampler, the sampler is brought on board and the water
samples are transferred from the Niskm or Go-Flo bottles to various sample bottles,
depending on analysis, for storage until processing and analysis. During sampling,
each bottle is rinsed with sample water, emptied, and filled with sample water. The
cap is replaced after addition of the preservative, or immediately if no preservative is
added Dissolved oxygen samples are processed immediately.
Rosette samplers are typically used in open water, both freshwater and marine
environments, where samples from multiple stations and depths will be required.
Real time in situ water column data can be collected to determine the best depths
for water sample collection Each discrete water sample has a corresponding set of
water quality parameter data.
Dissolved nutrient samples must be filtered before analysis, and must be filtered
within one hour of collection.
USEPA. 1997b. Lake Michigan Mass Balance Study Methods Compendium,
Volume 1: Sample Collection Techniques, EPA 905-R-97-012c. Great Lakes
National Program Office, U S Environmental Protection Agency, Chicago, IL.
http.//www epa qov/qrtlakes/lmmb/meth Last Accessed: 1/31/2003
ods/mbross odf
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.1-7
Water Sample Collection with the Kemmerer Bottle and the Bacon Bomb Sampler,
ERT SOP #2013
Both the Kemmerer Bottle and the Bacon Bomb Sampler can be used to collect
surface water in situations where site access from a boat or structure is available
and where samples at depth are required
A properly decontaminated, preset Kemmerer bottle or Bacon Bomb Sampler may
be lowered to a predetermined depth to collect an aqueous sample.
The Kemmerer Bottle can be used for general purpose sampling at the surface or at
specified depths The all-angle head locks the sampler in the open posibon and
unlocks when struck by the messenger, closing both end seals of the sampler. The
sampler is retneved and samples are transferred to appropriate sampling container
The Bacon Bomb Sampler opens when a protruded plunger strikes bottom. It
closes as the sampling device is hoisted back into the water column. By attaching a
cord to the upper end of the plunger, samples may also be taken from an
intermediate level as well. The sampler is then retrieved and the sample is
transferred to the appropriate sampling container
These samplers can collect any sort of water sample that then may be used for
chemistry analysis, nutrients analysis, or toxicity studies.
These samplers can collect samples from a range of depths The Kemmerer bottle
has few moving parts and needs little maintenance.
The sampling stations need to be accessible by boat or from land The samples
could be cross contaminated if sample equipment is not appropriately
decontaminated in between stations
USEPA 1994b. Surface Water Sampling, SOP # 2013, in Compendium of ERT
Standard Operating Procedures Environmental Response Team Compendium of
ERT Standard Operating Protocols Office of Solid Waste and Emergency
Response, U S. Environmental Protection Agency, Edison NJ.
httD'//www ert orq/oroducts/2013 pdf
lUcfisssed 1/31/2003
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Fact Sheet No
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website •
2.1.1-8
Dip Sampler, ERT SOP # 2013
The Dip sampler is generally used to collect surface water samples in a situation
where the sample is to be recovered from an outfall pipe or along a lagoon bank
where direct access is limited.
The dip sampler is extended into the sample location to collect sample. The
sampler is retrieved and the sample is transferred to the appropriate container
These surface water samplers can collect any sort of liquid sample that then may be
used for water chemistry analysis, nutrients analysis, or toxicity studies.
The long handle on dip samplers allows them to collect samples from discrete
locations. Dip samplers are extremely durable. They can be useful in weedy
habitats where other samplers may not work
The sampling location must be within reach of the investigator. The samples could
potentially be cross-contaminated if the sampler is not properly cleaned between
sample collections.
USEPA 1994b. Surface Water Sampling, SOP # 2013, in Compendium of
Environmental Response Team Compendium of Standard Operating Procedures.
Office of Solid Waste and Emergency Response, U.S. Environmental Protection
Agency, Edison NJ.
http //www ert org/products/2013 pdf L tetessed: 1/31/2003
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
2.1 1-9
Sample and Preservation of Water Specific Parameters
This method describes the sample collection procedures unique to conventionals,
metals, organics, and microbiological analytical parameters. See Table 2.1.1-1 for
details pertaining to recommended sample sizes, containers, preservation
techniques and holding times for water.
For analysis of conventional parameters, those parameters subject to biological
alteration should be measured first and within 15 minutes of sampling. Dissolved
oxygen should be the first parameter collected, followed in order of priority by those
parameters which would be the most affected by subsampling delays.
For analysis of total metals or total mercury, the samples should be acidified to pH
<2 using ultrapure HNO3. Samples that will be analyzed for mercury speciataon
should be preserved with HCI rather than HNO3 Samples that will be analyzed for
both dissolved and particulate metals should be filtered as soon as possible, within
24 hours of collection The filtrate, which contains the dissolved fraction, should be
preserved by acidifying to pH<2 using ultrapure HNO3 The particulate fraction,
which is retained on the filter, is frozen for preservation
For organics analysis, the samples for analysis of volatile organic compounds are
collected first in 40 ml VOA vials leaving no head space. The samples should be
protected from possible contamination such as fuels, winch grease, exhaust, and
solvents that may be present on or around a research vessel. Preserve water
samples collected for organics analysis as soon as possible, according to the
guidelines summarized in the attached table.
For microbiological analyses, it is important to collect from the microlayer, or
surface-most layer of water. The microlayer is most easily included when using the
scoop method. The scoop method involves plunging an open bottle straight down to
a depth of 1 5 to 39 cm below the water surface, moving it horizontal to the surface
while tipping it slightly to let trapped air escape, and removing the bottle in a vertical
position. Approximately 2 5 cm of head space is required in the sample container
Sample containers should be isolated from contact with wet ice as it could impart
contamination to the sample
These samples are then shipped to analytical laboratories where the
aforementioned analyses are performed to determine water chemistry.
Filtration is used for metals analysis since it is inexpensive and yields a sample that
is directly suitable for chemical analysis.
Holding times must be met in order to appropriately analyze the samples. Care
must be taken to avoid any sort of contamination of these samples since they will be
analyzed with sensitive procedures
Small amounts of particulate metals are collected during filtration, which make it
difficult to use them for low-level metal analyses
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Fact Sheet No.
Reference
Website
2.1.1-9(conld.)
PSWQAT. 1997. Recommended Guidelines for Sampling Marine Sediment, Water
Column, and Tissue in Puget Sound, Puget Sound Protocols and Guidelines. Puget
Sound Water Quality Action Team, Olympia, WA.
http //www osat wa qov/Pubhcations/
protocols/protocol. htm I
Last Accessed: 1/31/2003
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Table 2.1 .1 -1 . A Summary of Sample Sizes, Containers, Preservation Techniques, and Holding Times for
Water (PSWQAT. 1997.)'
Parameter
Alkalinity
Total Hardness
Total Phosphorous
Orthophosphate
PH
Salinity
Turbidity
Total Suspended
Solids
Dissolved Oxygen
Winkler
Dissolved Oxygen
Probe
Ammonia-N
Nitnte-N
Nitrate-N
Silica
Chlorophyll a
Volatile Organics
Minimum
Sample
Size (ml)
100
100
50
50
25
200
100
1,000 to
4,000
125
125
100
100
100
200
25 to 1,000
80
Container
Glass or
Polyethylene
Glass or
Polyethylene
Glass or
Polyethylene
Glass or
Polyethylene
Glass or
Polyethylene
Glass or
Polyethylene
Glass or
Polyethylene
Glass or
Polyethylene
Glass Bottle
with Glass Top
Glass Bottle
with Glass Top
Glass or
Polyethylene
Glass or
Polyethylene
Glass or
Polyethylene
Polyethylene
Glass or
Polyethylene
(Dark)
Glass -2 40 ml
vials, No Head
space
Preservation Technique
Refrigerate, 4* C
Refrigerate, 4* C
HNO3 to pH<2
Refrigerate, 4' C
H2SO4to pH<2
Refrigerate. 4" C
Filter on site
None
None
Refngerate, 4' C
Refrigerate, 4' C
Fix with MnCI2 and Alk
lod (2 ml ea )
None
Refngerate, 4* C
H2SO4to pH<2
Refngerate, 4' C
Refrigerate, 4' C
Refngerate, 4* C
Store filters frozen (-20 ' C)
in the dark
Refrigerate, 4* C
HCI to pH<2
Holding Time
14 Days
6 Months
28 Days
48 Hours
Analyze Immediately
28 Days
48 Hours
7 Days
8 Hours (store in the dark)
Analyze Immediately
28 Days
48 Hours
48 Hours
28 Days
28 Days
14 Days
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Table 2.1. 1-1. (contd.)
Parameter
Semi-volatile
Organics
Total Mercury and
Diss. Mercury
Total Metals and
Diss Metals
Microbiology
Minimum
Sample
Size (ml)
1,000 to
2,000
500
1,000
500
Container
Glass
Teflon™ or
Glass with
Teflon™ Cap
Polyethylene
or Teflon™
HOPE
(Autoclaved)
Preservation Technique
Refrigerate, 4* C
Refrigerate, 4' C
HNO3 to pH<2
Refrigerate, 4' C
HN03 to pH<2
Refrigerate, 4' C
Holding Time
7 Days
28 Days
6 Months
24 Hours
1 PSWQAT. 1997 Recommended Guidelines for Sampling Marine Sediment, Water Column, and Tissue in Puget
Sound, Puget Sound Protocols and Guidelines. Puget Sound Water Quality Action Team, Olympia, WA
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Fact Sheet No.
Method Title
Purpose
Method Summary
21 1-10
Sampling of Particulate-Phase and Dissolved-Phase Organic Carbon in Great Lakes
Waters, LMMB 014
This method describes the sampling of water for particulate-phase organic carbon
(POC) and dissolved-phase organic carbon (DOC).
Water samples are collected using either a submersible pump or Rosette sampler
(see Fact sheet 2.1.1-6) The volume of sample to be filtered is measured in a
graduated cylinder. Prior to filling, the cylinder is rinsed twice with sample water.
The water sample for POC/DOC analysis is vacuum filtered through an ashed 47
mm diameter glass fiber filter (0.7 urn pore-size) in an all-glass filtration apparatus
Samples are filtered simultaneously in duplicate. The samples are acidified with 0 2
N HCI during the filtration to remove inorganic carbonates. The POC is retained on
the filter, and the DOC is collected in the filtrate The volume of sample required to
produce a reliable POC measurement varies with station location, depth, and time of
year. If the filter becomes visibly loaded with particles and the flow of water through
the filter slows co
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/ Application
Advantages
Limitations
Reference
Website
2.1.1-11
Sampling Ambient Water for Trace Metals at EPA Water Quality Criteria Levels, EPA
Method 1669
This method is for the collection and filtration of ambient water samples for
subsequent determination of total and dissolved metals (antimony, arsenic,
cadmium, chromium (III and VI), copper, lead, mercury, nickel, selenium, silver,
thallium, zinc).
Method 1669 is "performance-based"; i.e., an alternate sampling procedure or
technique may be used, so long as neither samples nor blanks are contaminated
when following the alternate procedures. Before samples are collected, all sampling
equipment and sample containers are cleaned in a laboratory or cleaning facility
using detergent, mineral acids, and reagent water. After cleaning, sample containers
are filled with weak acid solution, individually double-bagged, and shipped to the
sampling site. If samples are to be collected for determination of trivalent chromium,
the sampling team processes additional QC aliquots are processed. Upon arrival at
the sampling site, one member of the two-person sampling team is designated as
"dirty hands"; the second member is designated as "clean hands " All operations
involving contact with the sample bottle and transfer of the sample from the sample
collection device to the sample bottle are handled by the individual designated as
"clean hands." "Dirty hands" is responsible for preparation of the sampler (except the
sample container itself), operation of any machinery, and for all other activities that do
not involve direct contact with the sample. All sampling equipment and sample
containers used for metals determinations must be nonmetallic and free from any
material that may contain metals. Sampling personnel are required to wear clean,
nontalc gloves at all times when handling sampling equipment and sample
containers. Sam pies for dissolved metals are filtered through a 0.45 urn capsule filter
at the field site. After filtering, the samples are double-bagged and iced immediately.
Acid preservation of samples is performed in the field or in the laboratory. Field
preservation is
necessary for determinations of trivalent chromium.
This method is applicable for use in EPA's data gathering and monitoring programs
associated with the Clean Water Act, the Resource Conservation and Recovery Act,
the Comprehensive Environmental Response, Compensation and Liability Act, and
the Safe Drinking Water Act.
Clean sampling methods reduce/eliminate bias associated with sample collection
handling.
Samples may become contaminated by numerous routes. These methods are only
applicable for trace metal contaminants.
USEPA. 1997b. Lake Michigan Mass Balance Study Methods Compendium, Volume
1: Sample Collection Techniques. EPA-821-C-01-001. Great Lakes National
Program Office, U.S. Environmental Protection Agency, Chicago, IL.
http //www.epa qov/clanton/clhtml/pubtitleOW html Last Accessed: 1/31/2003
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.1-12
ESS Method 340.2: Total Suspended Solids, Mass Balance (Dried at 103-105°C)
Volatile Suspended Solids (Ignited at 550°C), in LMMB 065
To measure the portion of total solid retained by a filter from drinking, surface, and
saline waters, domestic and industrial wastes.
Water samples are collected by submersible pump or Rosette sampler (see Fact
sheet 2 1.1-6). A sample volume is selected that will yield 2 - 20,000 mg/L. ' total
suspended solids. For open-lake oligotrophic conditions, 2-4 liters will provide
enough particulate matter. For near-shore or eu trophic conditions, 200-500 ML may
be sufficient. A well-mixed sample is filtered through a preweighed standard glass-
fiber filter, and the residue retained on the filter is dried at 103 to 105 °C for at least
one hour. The increase in weight of the filter represents the total suspended solids.
If measuring TSS of estuarine water, the filter must be well rinsed with Dl water to
remove salt residue.
Following Method LMMB 098. water samples can be filtered in the field and then
frozen at -10°C until final weighing in the laboratory.
The Environmental Research Laboratory - Narragansett (NHEERL-AED) SOP
1.02.004 and Standard Method 2540D also describe similar methods for measuring
total suspended solids (USEPA and Naval Construction Battalion Center, 1992;
APHA. 1999).
TSS is an ancillary parameter to the determination of hydrophobia organic
contaminants (HOCs). TSS is also commonly measured to assess water clarity or
to assess sediment transport and to norm ahze total (aqueous) contaminant data.
The samples may be filtered in the field or in portable laboratory facilities.
Excessive residue on the filter may form a water-entrapping crust. Sample size
should be limited to yield no more than 200 mg residue.
USEPA. 1997c. Lake Michigan Mass Balance Study Methods Compendium,
Volume 3: Metals. Conventbnals, Radio chemistry, and Biomonitoring Sample
Analysis Techniques, EPA 905-R-97-012c. Great Lakes National Program Office,
U.S. Environmental Protection Agency, Chicago, IL.
http-//www epa gov/qrtlakes/lmmb/methods/ Last Accessed- 1/31/2003
methd340 odf
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/ Application
Advantages
Limitations
Reference
Website
2.1.1-13
In situ Peepers
This method describes an in situ method to collect pore water.
A peeper, as described in this method, is a mesh-sided chamber that is inserted into
the sediment for the purpose of collecting pore water. Peepers are placed in situ
below the sediment surface with only the tubes emerging above the surface. The
chambers (constructed using 500-ml polyethylene bottles, mesh sides, tygon tubing
and a 50-ml syringe that slowly extracts the pore water) are buried in shallow waters
and sediment packed around the unit to ensure overlying waters are not in contact
with side mesh windows. Immediately following burial, water in the chamber is
evacuated to enhance entry and equilibration of pore water. After several minutes,
day-0 samples are collected.
The syringe is capped and returned to the laboratory for analysis of the extracted
water. Pore water is collected on day-0 and over predetermined time periods of up
to a month.
In situ peepers are used to collect pore water for lexicological testing. The device
may also be modified to suitable collect samples for chemical contaminant analyses.
In situ sampling reduces sampling and laboratory-related errors that may affect
organism response (i.e., resuspension of sediments that organisms would otherwise
not be exposed to).
There may be site-specific limitations that would prevent the deployment of a
peepers.
Sarda, N. and G. A. Burton. 1995 Ammonia Variation in Sediments: Spatial,
Temporal, and Method-Related Effects. Environmental Toxicology and Chemistry.
Vol. 14: 9.
N/A
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/ Application
Advantages
Limitations
Reference
Website
2.1.1-14
Suction Samplers
Suction samplers can be used to collect water that is then analyzed for various
chemicals of concern. This method is suitable for pore water samples analyzed for
ammonia.
The suction method uses an aquarium stone and a hand-operated vacuum pump to
extract pore water from surficial sediment in situ. The air stone is buried under the
surface of the sediment and the suction is applied. An imposed vacuum sucks pore
water into an in-ground porous cup. In simple systems, the water is stored in the
suction cell and is subsequently sucked or blown into a sample flask placed on the
ground surface. The vacuum is not maintained between samples.
Suction samplers are able to extract pore water in situ for chemical analysis.
In situ sampling reduces sampling and laboratory-related errors that may affect
organism response (ie., resuspensbn of sediments that organisms would otherwise
not be exposed to).
There may be site-specific limitatbns that would prevent the deployment of a suction
sampler.
Sarda, N. and G. A. Burton. 1995. Ammonia Variation in Sediments: Spatial,
Temporal, and Method-Related Effects. Environmental Toxicology and Chemistry.
Vol. 14:9.
N/A
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Method Summary
Data
Uses/ Application
Advantages
Limitations
Reference
Website
2.1.1-15
Physical Characterization of a Stream
These methods describe the data needed to characterize the physical attributes of a
stream needed for a habitat assessment.
Physical characterization of stream habitat includes descriptions of the:
• General stream characteristics such as an analysis of the stream subsystem
(where relevant), stream type (i.e., cold-water vs. warm-water), and stream
origin (i.e., glacial, montane, swamp, bog);
• Watershed features such as the predominant land use type surrounding the
stream, local watershed nonpoint source pollution, and local watershed erosion;
• Riparian vegetation up to 18 meters from the stream bed;
• Instream features such as estimated reach length, estimated stream width,
sampling reach area, estimated stream depth, velocity, canopy cover, high water
mark, proportion of reach represented by stream morphological types,
channelization, and dam presence;
• Surrounding woody debris in contact with the stream, noted by a wading visual
observer;
• The most dominant type of aquatic plants;
• Water quality parameters such as temperature, conductivity, dissolved oxygen,
pH, turbidity, water odors, water surface oils, and turbidity; and,
• Sediment characteristics such as odors, oils, deposits, inorganic substrate
components, and organic substrate components.
Evaluations of habitat quality via physical characteristics and water quality
parameters are pertinent to any assessments of ecological integrity. These types of
assessments are performed by many water resource agencies to determine if
degraded habitat is the result of toxicity and/or pollution. The full assessment
includes a general description of the site, the aforementioned physical
characterization and water quality assessment, and a visual assessment of mstream
and riparian habitat quality (Fact Sheet 2.1.1-16).
Most of the aforementioned data can be collected with field investigations in a quick
and relatively inexpensive manner.
These types of assessments are not sufficiently comprehensive to adequately
identify all causes of impact.
Barbour. et al.. 1999. Rapid Bioassessment Protocols for Use in Streams and
Wadeable Rivers: Periphyton, Benthic Macroinvertebrates and Fish, Second
Edition. EPA 841-B-99-002. Office of Water. U.S Environmental Protection
Agency, Washington, D.C.
htto //www epa qov/owow/monitonnq/rbp/
chOSmam html#Section%205 2
Last Accessed: 1/31/2003
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Method Title
Purpose
Method Summary
Data
Uses/ Application
Advantages
Limitations
2.1.1-16
Visual-Based Habitat Assessment
These methods describe the process for performing a visual-based habitat
assessment of a stream. Habitat parameters pertinent to the assessment of habitat
quality include those that characterize the stream "micro scale" habitat (e.g..
estimation of embeddedness), the "macro scale" features (e.g., channel
morphology) and the riparian and bank structure features that are most often
influential in affecting the other parameters.
First, a 100 meter reach of a stream must be selected for the assessment. The
entire sampling reach is then evaluated for each of the following parameters listed
below:
• Epifaunal substrate/available cover;
Embeddedness of rocks and snags;
Pool substrate characterization;
Velocity/depth combinations;
Pool variability;
• Sediment deposition;
• Channel flow status;
• Channel alteration;
• Frequency of riffles (or bends);
• Channel sinuosity;
Bank stability;
Bank vegetative protection; and
• Riparian vegetative zone width.
An additional 7 general physical habitat attributes are also important in determining
stream ecology:
• Channel dimensions;
• Channel gradient;
Channel substrate size and type;
• Habitat complexity and cover;
Riparian vegetation cover and structure;
• Anthropogenic alterations, and
• Channel-riparian interaction.
The habitat assessment process involves rating the parameters as optimal,
suboptimal, marginal, or poor based on criteria included in the data sheets.
Habitat assessments based on visual observation can be separated into 2 basic
approaches- one designed for high-gradient streams and one designed for low-
gradient streams. Some state programs have adapted this approach using
somewhat different or fewer parameters.
Standardized parameters list and protocol allows for some intercomparison amongst
sites.
Many of the data parameters are qualitative, thus assessments made at the same
location by different biologists may vary. The protocol suggests that a team of 2 or
more trained biologists should perform the assessment to enhance data quality.
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Reference
Website
2.1.1-16 (contd.)
Barbour, et al., 1999. Rapid Bioassessment Protocols for Use in Streams and
Wadeable Rivers: Periphyton, Benthic Macroinvertebrates and Fish, Second
Edition. EPA 841-B-99-002. Office of Water, U.S. Environmental Protection
Agency, Washington, D.C.
htto //www eoa aov/owow/monitorina/rbp/
chOSmain html#Section%205 2
Last Accessed: 1/31/2003
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Method Title
Purpose
Method Summary
Data
Uses/ Application
Advantages
Limitations
Reference
Website
2.1.1-17
USGS Field Operation Plan: Tributary Monitoring, in LMMB 017
This method describes the collection of water samples and field data from streams.
At each proposed sampling station, a cross-section of the stream is measured, and
the data will be used to subdivide the cross-section into three equal flow areas. The
centroid of each of these areas is identified on a field map. At each centroid, water
samples and Hydrolab parameters (i e., temperature, conductivity, dissolved
oxygen, pH) are collected at 0.2 and 0.8 times the depth. Samples are collected
during downstream flow, which is established for at least % hour prior to initiating
sample collection. Water samples from each of the 6 sampling locations are
composited. Water is collected for PCB, PAH, pesticide, and Atrazine analyses
using a submersible pump and passed through a 293 mm. stainless steel,
pentaplate filter holder. 2-5 glass fiber filters are used, depending on the
concentration of suspended material in the water column. Filters will be folded and
placed in aluminum foil pouches. The filtered samples will be stored in carboys until
analysis. Water for DOC, POC, and conventional constituents is also collected
using the pump. Secchi disk measurements are made at each centroid location for
each cross-section. Velocity and flow direction are recorded at each subsamplmg
location.
Several ASTM Methods deal with the measurement of open channel flow. These
methods include 01941, D3858, 04409, D5089, D5129, and 05130 (ASTM.
2001a).
Situations where samples are required for dissolved and organic contaminants.
This method provides a standardized approach for obtaining representative stream
samples
This collection method is limited to organic contaminants. Not applicable for trace
metal contaminants. Not applicable for chlorophyll, dissolved/particulate nutrients,
or TSS.
USEPA. 1997b . Lake Michigan Mass Balance Study Methods Compendium,
Volume 1: Sample Collection Techniques, EPA 905-R-97-012c. Great Lakes
National Program Office, U.S. Environmental Protection Agency, Chicago, IL.
htto //www epa aov/artlakes/lmmb/metho
ds/field96 odf
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.1-18
Quality Assurance Plan for Discharge Measurements Using Broadband Acoustic
Doppler Current Profilers
To measure velocities and discharge in the riverine and estuarine environment.
The Acoustic Doppler Current Profiler (ADCP) is an electronic instrument that is
used to measure water velocities. The instrument functions by transmitting acoustic
signals into the water column. The velocity of particles in the water column, and
therefore the velocity of the water, is calculated by comparing the frequency of the
transmitted signals compared to the frequency of backscatter signals reflected off
the particles. The instrument can be mounted to the side of a boat and towed
through the water column. The ADCP measures the velocity of the water column
relative to the movement of the vessel to which it is attached. Multiple transects of
data are averaged to reduce variation due to turbulence and velocity surges. At
least 4 transects should be made at each site to ensure a valid determination of
discharge.
Additional information regarding the use of ADCPs is found in Dredging Research
Technical Note DRP-1-16 (U.S. Army Engineer Waterways Experiment Station
1994).
The ADCP can be used to measure water velocities and discharge in a variety of
aquatic environments.
Measurement time is reduced; data can be collected throughout the water column
and cross section; stationing devices are not necessary.
The ADCP and its associated software are complex systems that should be used
only be highly trained personnel. High initial cost is also a major disadvantage. This
instrumentation is also unable to function in shallow water. The ADCP can
accurately measure discharge for only a limited range of flow conditions.
Lipscomb, SW. 1995. Quality Assurance Plan for Discharge Measurements Using
Broadband Acoustic Doppler Current Profilers. USGS Open-File Report 95-701 .
htlp //il.water usqs qov/adCD/reoorts/OFR9
5-701 html
Last Accessed: 1/31/2003
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.1-19
Seepage Meters
To determine the exchange of ground water to surface water and vice versa.
The Krupaseep is a prototype seepage meter device constructed of translucent
polycarbonate plastic domes of varying size. Each dome has a vertical skirt to
anchor it into deep organic muds. A port in the top of each dome allows flow-
through of water. Flow meters are installed in this port, and water quality meters are
installed on the inside and outside of the dome. When in use, the domes are
pressed into the river bottom until the top of each dome is 14 inches above the
mudlme. The monitoring equipment on each dome is tethered back to computers
onshore that record real-time water quality data, including photosynthesis-activated
radiation, on the inside and outside of the seepage meter and record the inflow or
outflow (flux) via heat pulse technology. Riverside solar panels charge the batteries
that power the flow meter computer and data logger. Water quality samples can
also be collected using hoses mounted on both the internal and external surfaces of
the dome and a onshore peristaltic pump.
A knowledge of the groundwater flux is needed to evaluate the significance of
contaminant flux into the water column from capped contaminated sediments.
This unit allows for the collection, both continuous and discrete, of water quality
parameters both inside and outside of the seepage meter. Measures of flux and
water quality can be made remotely.
The location of the meter is restricted to a radial operating distance of 160 feet from
the computers. Divers are required for installation and service of the units. Weekly
maintenance is required under harsh environmental conditions.
USGS. 2001 . The Krupaseep. Next Generation Seepage Meter.
httD //Sofia usas aov/sfrsf/entdiSDlavs/krupa Last Accessed- 1/31/2003
seep/
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.1-20
Caged Bivalve Deployment, AED LOP 1 .02.002, Revision 1
Deployment and retrieval of caged bivalves for environmental monitoring.
Four mussel baskets are deployed along a trawl (similar to long-line). Each trawl
has a surface floatation (lobster buoy) and an anchor (cinder block) at either end.
The mussel baskets are attached by leaders to cinder blocks fixed along the trawl
and are suspended approximately one meter above the bottom with sub-surface
floatation. Four replicate mussel baskets placed 50' apart are adequate to
characterize an area for chemical bioaccumulatoon, though this number dependent
upon localized conditions. The desired length of the trawl line is 170' plus 2X the
high water depth at the deployment location..
Each basket is fabricated from a 18" x 12* rectangle of black polyethylene V4" mesh
netting rolled into a cylinder, and secured with cable ties. The ends of the cylinder
are also closed with cable ties. Each basket contains 25 blue mussels, 5-7 cm in
length. The baskets are prepare in the laboratory and the baskets and mussels are
transported to the field site in coolers.
In the field, the mussel baskets are attached to the trawl leaders with cable ties. The
trawl is deployed sequentially beginning with one surface buoy followed by each of
the cinder blocks and finally the second surface buoy. Retrieval is the reverse of
deployment, beginning with the "down wind* buoy. Mussel baskets should be
placed in coolers as they are removed from the line.
Caged bivalve deployments are used to obtain tissue for chemical bioaccumulation
studies, frequently as part of environmental monitoring projects.
Relatively low cost and simple method with potental for revealing different
biomarkers of toxicity, identifying the chemicals responsible for the effects
measured, delineating affected areas, and specifying risks to aquatic fauna of
environmental contamination.
Permits may be required from local harbor master and/or appropriate regulatory
agencies. Other users of waterway, such as boat captains ans commercial lobster
men, must be considered. Weather may Inhibit or prohibit deployment and retrieval.
This procedure was written to meet the specific needs of the research program at
the U.S. EPA-Atlantic Ecology Division. It is not a U.S. EPA Standard Method and
must not be referred to as such. Mention of trade names or commercial products
does not constitute endorsement or recommendation for use.
Unpublished laboratory SOP, EPA NHEERL-AED, Narragansett, Rl
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2.1.2 Chemical and Physical Analyses
Section 2.1.2 contains methods for sample preparation and chemical and physical analysis of
water. These methods characterize the chemical composition and physical properties of water
samples collected by methods described in Section 2.1.1. Samples are often analyzed for the
presence of various inorganic and organic contaminants that may pose a threat to human or
ecological health. Many of the methods described have been developed over time to optimize the
detection, identification, and quantification of potential chemicals of concern. Several are
performance-based and may be further modified to enhance the accuracy and precision of the
method.
A variety of methods may exist for the analysis of a particular chemical parameter, all with varying
levels of quantification or degrees of sensitivity. Less sensitive methods may be used as a
screening tool during the initial site assessment to identify potential chemicals of concern. Follow-
up analysis may include the use of very precise methods that provide unequivocal identification
and trace level quantification of analytes. This variety also provides alternative methods useful in
the analysis of many types of water samples. Interferences from certain compounds in a water
sample may be avoided by the use of an alternative method.
Other than describing the water column itself, the physical properties of water often influence the
behavior of contaminants in the water column, and they may be helpful in further understanding
the fate of contaminants in the environment. Physical parameters may change the solubility and
chemical form of various chemical components in water.
Many of the chemical and physical methods described in these fact sheets are routinely
performed and fairly standardized. As a result, more than one source of information is often cited
in each method description. Specifically, the following sources provided methods information for
section 2.1.2:
• The USEPA's Office of Water
• The USEPA's Lake Michigan Mass Balance Study Methods Compendium, 1997v The
USEPA's Test Methods for Evaluating Solid Waste, Physical/Chemical Methods
(SW846 Methods)
• NOAA's National Status and Trends Program, 1998
• Standard Methods for Examination of Water and Wastewater, 1999
• ASTM
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-1
Mercury in Water by Cold Vapor Atomic Fluorescence Spectrometry, EPA Method
245.7
To determine the concentration of mercury (Hg) in filtered and unfiltered
water by cold-vapor atomic fluorescence spectrometry (CVAFS).
A 100- to 2000-mL sample is collected directly into a fluoropolymer
bottle using sample handling techniques specially designed for collection of mercury
at trace levels. For dissolved Hg, the sample is filtered through a 0.45-um capsule
filter. The sample is preserved by adding 5 ml_/L of pretested 12N HCI. Inorganic
Hg compounds and organic mercury species are oxidized by a potassium
bromate/potassium bromide reagent. After oxidation, the sample is sequentially
prereduced with NH2OH HCI to destroy the excess bromine, then the ionic Hg is
reduced with SnCL, to convert Hg(ll) to volatile Hg(0). The Hg(0) is separated from
solution by purging with high punty argon gas through a semipermeable dryer tube.
The Hg passes into an inert gas stream that carries the released Hg(0) into the cell
of a cold-vapor atomic fluorescence spectrometer (CVAFS) for detection The
concentration of Hg is determined by atomic fluorescence spectrometry at 253.7 nm.
The method detection limit (MDL) and minimum level of quantization (ML) in this
method are 1.8 ng/L and 5.0 ng/L, respectively. This method may be used to
determine Hg up to 200 ng/L and may be extended by dilution of
the sample. The normal calibration range for ambient water monitoring is 5 ng/L to
100 ng/L.
A similar method for the detection of total mercury is ASTM Method D3223 (ASTM,
2001 a).
This method is applicable to drinking water, surface and ground waters, marine
water, and industrial and municipal wastewater.
Wide analytical range makes method suitable for contaminated sites
Ambient mercury levels frequently are below the detection limit provided by this
method.
USEPA. 2001 a. Method 245.7- Mercury in Water by Cold Vapor Atomic
Fluorescence Spectrometry, Draft, EPA 821-R-01-008. Office of Water, U.S.
Environmental Protection Agency, Washington, DC.
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
2.1.2-2
Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic
Fluorescence Spectrometry, EPA Method 1631, Revision B
This method is for determination of mercury (Hg) in filtered and
unfiltered water by oxidation, purge and trap, desorption, and cold-vapor atomic
fluorescence spectrometry (CVAFS).
A 100- to 2000-mL sample is collected directly into a fluoropolymer bottle. For
dissolved Hg, the sample is filtered through a 0.45-um capsule filter. The sample is
preserved by adding either HCI or BrCI solution. If a sample will also be used for the
determination of methyl mercury, it should be preserved with HCI solution only. Prior
to analysis, a 100-mL sample aliquot is placed in a specially designed purge vessel,
and 0.2N BrCI solution is added to oxidize all Hg compounds to Hg(ll). After
oxidation, the sample is sequentially prereduced with NH2OH HCI to destroy the free
halogens, then reduced with SnCl, to convert Hg(ll) to volatile Hg(0). The Hg(0) is
separated from solution by purging with nitrogen onto a gold-coated sand trap. The
trapped Hg is thermally desorbed from the gold trap and carried into the cell of a
cold-vapor atomic fluorescence spectrometer (CVAFS) for detection.
This method is for determination of Hg in the range of 0.5-100 ng/L and may be
extended to higher levels by selection of a smaller sample size. The method
detection limit for Hg has been determined to be 0.2 ng/L when no interferences are
present. The minimum level of quantization (ML) has been established as 0.5 ng/L.
An MDL as low as 0.05 ng/L can be achieved for low Hg samples by using a larger
sample volume, a lower BrCI level (0.2%), and extra caution in sample handling.
For the analysis of water samples using Methods LMMB 048 and 049 (USEPA,
1997d), subsamples are oxidized with BrCI solution and heated for at least an hour
(preferably overnight) at 70°C before prereduction and analysis. Aliquots of 125-
500 mL are purged and trapped. For particulate samples, the filter is treated in a
similar fashion as the water samples, except that 2 mL of hydroxylamine HCI is used
to produce samples. Method LMMB 048 has a mean detection limit of
approximately 0.1 ng/L.
This method is for use in EPA's data gathering and monitoring programs
associated with the Clean Water Act, the Resource Conservation and Recovery Act,
the Comprehensive Environmental Response, Compensatbn and Liability Act, and
the Safe Drinking Water Act.
The dual amalgam trap system and fluorescence detector provide greater sensitivity
and specificity in the presence of interferences, and this system must be used to
overcome interferences, if present, and to achieve the sensitivity required, if
necessary. The detection range of this method generally provides detecton of
mercury in ambient surface waters.
This method does not distinguish between methyl mercury and inorganic mercury
species.
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Reference
Website
2.1.2-2(contd.)
USEPA. 1999b. Method 1631, Revision B: Mercury in Water by Oxidation, Purge
and Trap, and Cold Vapor Atomic Fluorescence Spectre metry, EPA 821-R-99-005.
Office of Water, U.S. Environmental Protection Agency, Washington, DC.
htto //www eoa aov/clanton/clhtml/oubtitleOW
html
Last Accessed: 1/31/2003
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Method Title
Purpose
Method Summary
Data Uses/ Application
Advantages
Limitations
Reference
Website
2.1.2-3
Methyl Mercury in Water by Distillation, Aqueous Ethylation, Purge and Trap,
and CVAFS, EPA Method 1630
This method is designed for determination of CH3Hg in the range of 0 02-5 ng/L
and may be extended to higher levels by selection of a smaller sample size.
A 100-2000 ml sample is collected directly into fluoropolymer or borosilicate
bottle(s). For dissolved CH3Hg, samples are filtered through a 0.45-^m capsule
filter. Fresh water samples are preserved by adding 11.6 M HCI. while saline
samples ([Cl - ] > 500 ppm) are preserved with 9 M H2S04. Prior to analysis, a
45-mL sample aliquot is placed in a specially designed fluoropolymer distillation
vessel, and 35 ml of the water is distilled into the receiving vessel at 125° C
under N2 flow. After distillation, the sample is adjusted to pH 4.9 and ethylated
in a closed purge vessel. The ethyl analog of CH3Hg, methylethyl mercury, is
separated from solution by purging with N2 onto a graphitic carbon (Carbotrap ®
) trap. The trapped methylethyl mercury is thermally desorbed from the trap,
carried through a pyrolytic decomposition column, which converts organo
mercury forms to elemental mercury (Hg 0), and then into the cell of a cold-
vapor atomic fluorescence spectrometer (CVAFS) for detection.
The method detection limit for CH3Hg has been determined to be 0.02 ng/L
when no background elements or interferences are present. The minimum level
(ML) has been established as 0.06 ng/L. An MDL as low as 0.009 ng/L can be
achieved for low CH3Hg samples by using extra caution in sample handling and
reagent selection, particularly the use of "for ultra-low level
only" distillation equipment.
This method is for use in EPA's data gathering and monitoring programs
associated with the Clean Water Act. the Resource Conservation and Recovery
Act, the Comprehensive Environmental Response, Compensatbn and Liability
Act, and the Safe Drinking Water Act.
Methyl mercury is frequently required for risk assessments. This method
provides the sensitivity to determine ambient levels in most aqueous samples.
Samples may become contaminated by numerous routes. Potential sources of
trace metals contamination include: metallic or metal-containing labware (e.g.,
talc gloves that contain high levels of zinc), containers, sampling equipment,
reagents, and reagent water; improperly cleaned or stored equipment, labware,
and reagents; and atmospheric inputs such as dirt and dust. Even human
contact can be a source of trace metals contamination.
USEPA. 200 1b. Method 1630. Methyl Mercury in Water by Distillation,
Aqueous Ethylation, Purge and Trap, and CVAFS. EPA 821-R-01-020. Office
of Water, U.S. Environmental Protection Agency, Washington, DC.
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Method Title
Purpose
Method Summary
Data
Uses/ Application
Advantages
Limitations
Reference
Website
2.1.2-4
Determination of Trace Elements in Ambient Waters by Stabilized
Temperature Graphite Furnace Atomic Absorption, EPA Method 1639
This procedure is for the determination of dissolved elements (antimony, cadmium,
nickel, selenium, trivalent chromium, zinc) in ambient waters by Stabilized
Temperature Graphite Furnace Atomic Absorption (GFAA). It may also be used for
determination of total recoverable element concentrations in these waters.
For total recoverable analysis of an aqueous sample containing undissolved material,
analytes are first solubilized by gentle refluxing with nitric and hydrochloric acids.
After cooling, the sample is made up to volume, mixed, and centnfuged or allowed to
settle overnight prior to analysis. To determine dissolved analytes in a filtered
aqueous sample aliquot, the sample is prepared for analysis by the appropriate
addition of nitric acid, and then diluted to a predetermined volume and mixed before
analysis The analytes listed in this method are determined by stabilized temperature
platform graphite furnace atomic absorption (STPGFAA).
Metal MDL (M9/L) ML (|ig/L)
Antimony 1.9 5
Cadmium 0.023 0.05
Chromium (III) 0.1 0.2
Nickel 0.65 2
Selenium 0.83 2
Zinc 0.14 0.5
ASTM Method D1687 describes a similar (and alternative) method for the
measurement of hexavalent and total chromium in water (ASTM, 2001 a). ASTM
Methods D3557 and D3859 describe the analysis of cadmium and selenium by
GFAA, respectively. ASTM Method D3919 and SW846 Method 7000A describe the
analysis of several elements by atomic absorption methods (ASTM. 2001 a; USEPA
SW846.
This method is for use in EPA's data gathering and monitoring programs
associated with the Clean Water Act, the Resource Conservation and Recovery Act,
the Comprehensive Environmental Response, Compensatbn and Liability Act, and
the Safe Drinking Water Act.
GFAA techniques in addition to ICP-MS methods are frequently required to obtain all
trace metal analytes of interest.
Samples may become contaminated by numerous routes. This method should be
used by analysts experienced in the use of graphite furnace atomic absorption
spectroscopy.
USEPA. 1996b. Method 1639: Determination of Trace Elements in Ambient Waters
by StabDized Temperature Graphite Furnace Atomic Absorption, EPA 821-R-96-006.
Office of Water, U.S. Environmental Protection Agency. Washington, DC.
http //www epa gov/clanton/clhtml/pubtitleO
W html
Last Accessed: 1/31/2003
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Method Title
Purpose
Method Summary
Data Uses/Applicaton
Advantages
Limitations
Reference
Website
2.1.2-5
Determination of Trace Elements in Ambient Waters by Off-Line dictation Pre-
concentration and Stabilized Temperature Graphite Furnace Atomic Absorption,
EPA Method 1637
This procedure is for the determination of dissolved elements in ambient
waters, namely cadmium and lead. It may also be used for determination of
total recoverable element concentrations in these waters.
For total recoverable analysis of an aqueous sample containing undissolved
material, analytes are first solubDized with nitric acid. After cooling, the sample is
made up to volume, mixed, and centrifuged or allowed to settle overnight before
analysis. For the determination of dissolved analytes in a filtered aqueous
sample aliquot, the sample is made ready for analysis by the appropriate
addition of nitric acid, and then diluted to a predetermined volume and mixed
before analysis.
This method is used to preconcentrate trace elements using an iminodiacetate
functionalized chelating resin. After a sample is prepared, it is buffered using an
on line system before it enters the chelating column. Group I and II metals, as
well as most amons, are selectively separated from the analytes by elutaon with
ammonium acetate at pH 5.5. The analytes are subsequently eluded into a
simplified matrix consisting of 0.75 M nitric acid. The eluded sample is collected
and then analyzed by stabilized temperature platform graphite furnace atomic
absorption (STPGFAA).
The method detection limits for Cd and Pb have been determined to be 0.0075
pg/L and 0 036 ug/L, respectively. The minimum levels (ML) have been
established as 0.02 and 0.1 ug/L, respectively.
Similar methods include ASTM Methods D3557 for cadmium and D3559 for
lead(ASTM,2001a).
This method is for use in EPA's data gathering and monitoring programs
associated with the Clean Water Act, the Resource Conservation and Recovery
Act, the Comprehensive Environmental Response, Compensation and Liability
Act, and the Safe Drinking Water Act.
Off line Pre-concentration methods eliminate many sample handling
procedures, reducing sources of contamination. GFAA analysis affords
extremely low detection limits.
Due to its sensitivity, interferences can occur with GFAA analysis. This method
should be used by analysts experienced in the use of graphite furnace atomic
absorption spectroscopy.
USEPA. 1996c. Method 1637: Determination of Trace Elements in Ambient
Waters by Off-Line Chelation Pre-concentration and Stabilized Temperature
Graphite Furnace Atomic Absorption, EPA 821-R-96-004. Office of Water, U.S.
Environmental Protection Agency, Washington, DC.
http://www epa gov/clanton/clhtml/pubti Last Accessed- i/ai/?nna
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data Uses/Application
2.1.2-6
Determination of Trace Elements in Ambient Waters by Inductively
Coupled Plasma — Mass Spectrometry, EPA Method 1638
This procedure is for the determination of dissolved elements (antimony,
cadmium, copper, lead, nickel, selenium, silver, thallium, zinc) in ambient
waters. It may also be used for determination of total recoverable element
concentrations in these waters.
For total recoverable analysis of an aqueous sample containing undissolved
material, analytes are first solubSized with .nitric and hydrochloric acids. After
cooling, the sample is made to volume, mixed, and centrifuged or allowed to
settle overnight prior to analysis. For the determination of dissolved analytes in a
filtered aqueous sample aliquot, the sample is prepared for analysis by the
appropriate addition of nitric acid, and then diluted to a predetermined volume
and mixed before analysis. The digested sample is introduced into a radio
frequency plasma, where energy transfer processes cause desolvation,
atomization, and ionzation. The ions are extracted from the plasma through a
differentially pumped vacuum interface and separated on the basis of their
mass-to- charge ratio (m/z) by a mass spectrometer. Ions transmitted through
the mass analyzer are detected by an electron multiplier or Faraday detector
and the resulting current is processed by a data handling system.
1638 1638 LMMB 057
Metal MDL(pg/L) ML(ug/L) ML(ng/L)
Aluminum 25/15
Antimony 0.0097 0.02
Arsenic 15/10
Cadmium 0.025 2.5/0.5
Chromium 20/8
Copper 0.087 0.2 8/4
Lead 0.015 0.05 3/0.5
Nickel 0.33 1
Selenium 0.45 1
Silver 0.029 0.1 1.5/0.3
Thallium 0.0079 0.02
Zinc 0.14 0.5 10/2.5
ICP-MS detection limits listed for LMMB 057 are for pneumatic and ultrasonic
nebulizaton. respectively (USEPA, 1997c).
Standard Method 3120B, ASTM Method D5673, and SW846 Method 6020
describe the analysis of metals by ICP-MS (APHA, 1999; ASTM. 2001 a;
USEPASW846).
This method is for use in EPA's data gathering and monitoring programs
associated with the Clean Water Act. the Resource Conservation and Recovery
Act. the Comprehensive Environmental Response, Compensation and Liability
Act, and the Safe Drinking Water Act.
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Advantages
Limitations
Reference
Website
2.1 2-6 (contd.)
Analysis by ICP-MS provides a high level of sensitivity for some elements that
are difficult to determine by other methods. Up to 20 elements can be
determined from a single sample.
This method should be used by analysts experienced in the use of inductively
coupled plasma mass spectrometry (ICP-MS).
USEPA. 1996d. Method 1638: Determination of Trace Elements in Ambient
Waters by Inductively Coupled Plasma-Mass Spectrometry. EPA
821-R-96-005. Office of Water, U.S. Environmental Protection Agency.
Washington, DC.
htto //www eoa aov/clanton/clhtml/Dubti
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for Assessing and Monitoring the Remediation of Contaminated Sediment Sites
February 17,2003
Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-7
Determination of Trace Elements in Ambient Waters by On-Line Chelation
Pre-concentration and Inductively Coupled Plasma-Mass Spectrometry, EPA
Method 1640
This procedure is for the determination of dissolved elements (cadmium, copper,
lead, nickel) in ambient waters. It may also be used for determination of total
recoverable element concentrations in these waters.
This method is used to preconcentrate trace elements using an iminodiacetate
functbnalized chelatng resin system that is connected directly to the ICP-MS.
Following acid solubilizafaon, the sample is buffered prior to the chelafing column
using an on line system. Group I and II metals, as well as most anions, are
selectively separated from the analytes by elution with ammonium acetate at pH 5.5.
The analytes are subsequently eluded into a simplified matrix consisting of dilute
nitric acid and are determined by ICP-MS using a directly coupled on line
configuration.
Metal MDL(ug/L) ML(ug/L)
Cadmium 0.0024 0.01
Copper 0.024 0.1
Lead 0.0081 0.02
Nickel 0.029 0.1
This method is for use in EPA's data gathering and monitoring programs
associated with the Clean Water Act, the Resource Conservation and Recovery Act,
the Comprehensive Environmental Response, Compensation and Liability Act, and
the Safe Drinking Water Act.
The on line Pre-concentration system allows for reduced sampling handling,
minimizing the risk of sample contamination. Method 1640 is a convenient method
for the detection of a short list of toxic metals.
Neither mercury nor arsenic can be measured with this method.
USEPA. 1996e. Method 1640: Determination of Trace Elements in Ambient
Waters by On-Line Chelation Pre-concentration and Inductively Coupled
Plasma-Mass Spectrometry, EPA 821-R-96-007. Office of Water, U.S.
Environmental Protection Agency, Washington, DC.
http //www epa qov/clanton/clhtml/pubtitleOW Last Accessed: 1/31/2003
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for Assessing and Monitoring the Remediation of Contaminated Sediment Sites
February 17,2003
Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-8
Inorganic Arsenic in Water by Hydride Generation Quartz Furnace Atomic
Absorptbn. EPA Method 1632
This method is for determination of total inorganic arsenic (As) in filtered and
unfiltered water by hydride generation and quartz furnace atomic absorption
detection. This method is designed for measurement of dissolved and total arsenic
in the range of 10-200 ng/L.
A 100-2000 mL sample is collected directly into a sample bottle. The sample is
either field or laboratory preserved by the addition of 10% HN03, depending on the
time between sample collection and arrival at the laboratory. An aliquot of sample is
placed in a specially designed reaction vessel and 6 M HCI is added. Before
analysis, 4% NaBH4 solution is added to convert organic and inorganic arsenic to
volatile arsines. The arsines are purged from the sample onto a cooled glass trap
packed with 15% OV-3 on Chromasorb ® WAW-DMCSO, or equivalent. The
trapped arsines are thermally desorbed, in order of increasing boiling points, and
carried into the quartz furnace of an atomic absorption spectrophotometer for
detection.
The first arsme to be desorbed will be AsH3 , which represents total inorganic
arsenic in the sample.
The method detecton limit for total inorganic arsenic has been determined to be 3
ng/L when no background elements or interferences are present. The minimum
level (ML) has been established at 10 ng/L.
ASTM Method D2972B, Standard Method 31 14B, and SW846 Method 7061A all
describe similar methods for the hydride generation atomic absorption detection of
arsenic in water (ASTM, 2001a; APHA. 1999; USEPA SW 846)
The method is for use in EPA's data gathering and monitoring programs associated
with the Clean Water Act.
Automation of this method reduces error and
potential sources of contamination.
This method does not provide data on arsenic speciation. which is sometimes
required in risk assessments.
USEPA. 1996f. Method 1632: Inorganic Arsenic in Water by Hydride Generation
Quartz Furnace Atomic Absorption. EPA 821-R-96-013. Office of Water, U.S.
Environmental Protection Agency, Washington, DC.
http //www epa qov/clanton/clhtml/pubtitleO
W html
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February 17,2003
Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-9
Chemical Speciaton of Arsenic in Water and Tissue by Hydride Generation Quartz
Furnace Atomic Absorptbn Spectrometry, EPA Method 1632, Revision A
This method is for determination of inorganic arsenic (IA), arsenite (As +3 ),
arsenate (As +5 ), monomethylarsonic acid (MMA), and dimethylarsinic acid (DMA)
in filtered and unfiltered water by hydride generation and quartz furnace atomic
absorption detection. This method is designed for measurement of As species in
water in the range 0 01-50 ug/L.
Aqueous sample — A 500- to 1000-mL water sample is .collected directly into a
cleaned sample bottle. Water samples are preserved in the field by the additon of
6M HCI. The recommended holding time is 28 days.
An aliquot of water sample is placed in a specially designed reaction vessel, and 6M
HCI is added. NaBH4 solution is added to convert IA, MMA, and DMA to volatile
arsines. Arsines are purged from the sample onto a cooled glass trap packed with
15% OV-3 on Chromosorb ® W AW-DMCS, or equivalent. The trapped arsines are
thermally desorbed, in order of increasing boiling points and carried into the quartz
furnace of an atomic absorption spectrophotometer for detection. To determine the
concentration of As +3, another aliquot of water sample or tissue digestate is placed
in the reaction vessel and Tris-buffer is added. The procedure is repeated to quantify
only the arsine produced from As +3. The concentration of As +5 is the
concentration of As +3 subtracted from the concentration of IA.
Analyte MDL ML
IA (As +3 +As +5 ) 0.003 ug/L 0.01 pg/L
Arsenite (As +3 ) 0.003 ug/L 0.01 ug/L
MMA 0.004 ug/L 0.01 ug/L
DMA 0.02 ug/L 0.05 ug/L
The method is for use in EPA's data gathering and monitoring programs associated
with the Clean Water Act.
The relative amounts of carcinogenic arsenite (As +3) to total arsenic varies with
surface water body and varies with pH. This method directly quantifies arsenite.
Depending upon As levels at site, speciation may not be necessary.
USEPA. 2001 c. Method 1632, Revision A: Chemical Speciation of Arsenic in
Water and Tissue by Hydride Generation Quartz Furnace Atomic Absorption
Spectrometry, EPA 821-R-01-006. Office of Water, U.S. Environmental Protection
Agency, Washington, DC.
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-10
Determination of Hexavalent Chromium by Ion Chromatography, EPA Method 1636
This method is for the determination of dissolved hexavalent chromium (as CrO42" )
in ambient waters at EPA water quality criteria (WQC) levels using ion
Chromatography (1C).
An aqueous sample is filtered through a 0.45 urn filter, and the filtrate is adjusted to
a pH of 9-9.5 with a concentrated buffer solution. A measured volume of the sample
(50-250 uL) is introduced into the ion Chromatography. A guard column removes
organics from the sample before the Cr(VI), as Cr042-, is separated on a high
capacity anion exchange separator column. Post column derivatizaton of the Cr(VI)
with diphenylcarbazide is followed by detection of the colored complex at 530 nm.
The method detection limit (MDL). and the minimum level (ML) for
hexavalent chromium (Cr(VI)) are 0.23 ug/L and 0.5 ug/L, respectively.
ASTM Method D5257 and SW846 Method 7199 also describe the analysis of
hexavalent chromium by Ion Chromatography (ASTM, 2001 a; USEPA SW846).
The method is for use in EPA's data gathering and monitoring programs associated
with the Clean Water Act.
This method provides the rapid and reproducible isolation and analysis of Cr (VI)
without interference from other Cr species.
Samples containing high levels of anionic species, such as sulfate and chloride, may
cause column overload. Samples containing high levels of organics or sulfides
cause rapid reduction of soluble Cr(VI) to Cr(lll). Samples must be stored at 4°C
and analyzed within 24 hours of collection unless preserved with sodium hydroxide.
USEPA. 1996g. Method 1636: Determination of Hexavalent Chromium by Ion
Chromatography, EPA 821-R-95-029. Office of Water, U.S. Environmental
Protection Agency, Washington, DC.
http://www epa qov/clanton/clhtml/pubtitle
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February 17,2003
Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/ Application
Advantages
Limitations
Reference
Website
2.1.2-11
Volatile Organic Compounds by Isotope Dilution GC/MS, EPA Method 1624b
This method is designed to determine the volatile toxic organic pollutants.
Stable isotopically labeled analogs of the compounds of interest are added to a 5 mL
water sample. The sample is purged at 20-25'C with an inert gas in a specially
designed chamber. The volatile organic compounds are transferred from the
aqueous phase into the gaseous phase where they are passed into a sorbent
column and trapped. After purging is completed, the trap is back flushed and heated
rapidly to desorb the compounds into a gas chromatography (GC). The compounds
are separated by the GC and detected by a mass spectrometer (MS). The labeled
compounds serve to correct the variability of the analytical technique. Identification
of a compound (qualitatve analysis) is performed by comparing the GC retention
time and the background corrected characteristic spectral masses with those of
authentic standards. Quantitative analysis is performed by GC/MS using extracted
ion current profile (EICP) areas. Isotope dilution is used when labeled compounds
are available; otherwise, an internal standard method is used. The Minimum Level
for most VOC compounds is either 10 or 50 ug/L.
Similar methods for the determination of volatile organic compounds and volatile
aromatic organic compounds are presented in Standard Methods 6210 and 6220,
respectively (APHA. 1999). SW846 Methods 5030B, 5035. and 8260B and ASTM
Method D5790 describe the preparation and analysis of volatile organics by GC/MS
(USEPA SW846); ASTM, 2001 a).
The method is designed to meet the survey requirements of Effluent Guidelines
Division (EGD) and the National Pollutants Discharge Elimination System (NPDES)
under 40 CFR Parts 136.1 and 136.5 VOC in ambient waters is sometimes
monitored at sites of suspected contaminated groundwater inflow.
The combination of GC retention time and MS characterization provides
unequivocal identification of analytes.
The GC/MS portions of this method are for use only by analysts experienced with
GC/MS or under the close supervision of such qualified persons. Samples can be
contaminated by diffusion of volatile organic compounds (particularly methylene
chloride) through the bottle seal during shipment and storage. Contamination by
carry-over can occur.
USEPA. 1989a. Method 1624, Revision B: Volatile Organic Compounds by Isotope
Dilution GC/MS. EPA440-1 -89-023. Office of Water, U.S. Environmental Protection
Agency, Washington, DC.
Rev B not available online Last Accessed:
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February 17,2003
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Method Title
Purpose
Method Summary
Data Uses/Application
Advantages
Limitations
Reference
Website
21.2-12
Photovac GC Analysis for Soil, Water, and Air/Soil Gas. ERT SOP# 2109
This method is designed as a field screening procedure for the tentative
identification of various volatile organic compounds.
Water samples are collected in triplicate in 40-mL VOA vials with Teflon™-lmed
silicone septum screw caps. The vials are filled completely, with no visible air
bubbles. A 20-mL aliquot of sample from one of the three sample triplicates is
pipetted into a second, clean VOA vial. The vial is capped, shaken vigorously
for one minute, and allowed to stand at room temperature for at least 30
minutes for vapor phase equilibration. An aliquot of the water head space is
then removed from the vial and injected into the GC using a gas-tight syringe.
The GC uses an ultraviolet light source and photoionization detector. The other
two vials are analyzed within seven days by another method to confirm the field
screening data.
Typical MDLs for this method range from 1 ppb to 5 ppb.
ERT SOPs # 2108 and #2107 describe the operation of specific models of
Photovac Gas Chromatographs.
Site assessment/characterization and health and safety surveys.
The data generated with this method allows for rapid evaluation of site
conditions.
Pollutant identification is only tentative.
USEPA 1994b. SOP # 2109: Photovac GC Analysis for Soil, Water, and
Air/Soil Gas. Environmental Response Team. Compendium of ERT Standard
Operating Protocols. Office of Solid Waste and Emergency Response, U.S.
Environmental Protection Agency, Edison NJ
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Method Title
Purpose
Method Summary
Data
Uses/ Application
Advantages
Limitations
Reference
Website
2.1.2-13
Semi-volatile Organic Compounds by Isotope Dilution GC/MS, EPA Method 1625
Revision B
This method is used to determine the semi-volatile toxic organic pollutants (i.e.,
PAHs) in water.
This method is performance-based. Stable isotopically labeled analogs of the
compounds of interest are added to a one liter water sample. The sample is
extracted at pH 12-13, then at pH <2 with methylene chloride using continuous
extraction techniques. The extract is dried over sodium sulfate and concentrated to
a volume of 1 mL. An internal standard is added to the extract, and the extract is
injected into the gas chromatography (GC). The compounds are separated by GC
and detected by a mass spectrometer (MS). The labeled compounds serve to
correct the variability of the analytical technique. Identification of a compound
(qualitative analysis) is performed by comparing the GC retention time and
background corrected characteristic spectral masses with those of authentic
standards. Quantitative analysis is performed by GC/MS using extracted ion current
profile (EICP) areas. Isotope dilution is used when labeled compounds are available;
otherwise, an internal standard method is used.
The method detection limit for most compounds of interest is 10 ug/L. The MDL for
some compounds is 20 or 50 ug/L.
Similar methods for the extraction and analysis of semi-volatile organic compounds
are Standard Method 6410B and SW846 Method 8270C (APHA, 1999).
The method is designed to meet the survey requirements of Effluent Guidelines
Division (EGD) and the National Pollutants Discharge Elimination System (NPDES)
under 40 CFR Part 136.1.
Mass spectral analysis, combined with gas chromatographic compound retention
time, provides unequivocal compound identification. Isotope dilution corrects
recovery and performance of each compound of interest.
The GC/MS portions of this method are for use only by analysts experienced with
GC/MS or under the close supervision of such qualified persons. The suites of
stable isotopes required for this analysis are often prohibitively expensive for use in
routine monitoring programs.
USEPA. 1989b. Method 1625, Revisbn B: Semi-volatile Organic Compounds by
Isotope Dilution GC/MS. EPA440-1-89-023. Office of Water. U.S. Environmental
Protection Agency, Washington, DC.
Rev B not available online Last Accessed:
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February 17, 2003
Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-14
Quantitative Determination of Polynuclear Aromatic Hydrocarbons by Gas
Chromatography/Mass Spectrometry (GC/MS) - Selected Ion Monitoring (SIM)
Mode
To determine low concentrations of polycyclic aromatic hydrocarbons (PAHs) and
their alkylated homologues in extracts of water, sediments and biological tissues.
Just prior to analysis, an aliquot of internal standard solution is added to the sample
extract producing a final internal standard concentration of approximately 40 ng/mL.
The analytical system includes a temperature programmable gas chromatography
with a DB-5MS fused silica capillary column. Helium is used as the carrier gas, and
the samples are handled by an auto sampler capable of making 1 - 4 ul injections.
A five point calibration curve is established to demonstrate the linear range of the
detector. The effluent from the GC capillary column is routed directly into the ion
source of the mass spectrometer (MS). The MS is operated in the SIM mode using
appropriate windows to include the quantization and confirmation masses for target
PAHs. For all compounds detected at a concentration above the MDL. a
confirmation ion is checked to confirm its presence. The response factors of the
surrogate relative to each of the calibration standards are calculated, followed by the
calculation of the sample extract concentration. The sample concentration for each
compound is calculated by dividing the sample extract concentration by the sample
amount.
PAH concentrations, particularly pyrene, are one of the primary risk factors
associated with contaminated waters. PAH data obtained from this analysis are
used for site characterization and risk assessments.
GC/MS in the SIM mode provides unambiguous and sensitive detection for PAHs.
The PAH quantization method is very rigorous because PAHs have very strong
molecular ion peaks under the mass spectrometric conditions used. Also, the
availability of labeled surrogates internal standards of many of the analytes makes
very accurate determinations of analyte concentrations possible. Analysis of
alkylated PAH homologues can provide site-specific information that can be used in
source identification or product identification.
GC/MS in SIM mode cannot be used for simultaneous screening for other organic
contaminants of similar polarity or volatility; cannot be used to identify tentatively
identified compounds (TICs).
NOAA. 1998. Sampling and Analytical Methods of the National Status and Trends
Program, Mussel Watch Project- 1996 Update, NOAA Technical Memo NOS ORCA
130. National Oceanic and Atmospheric Administration, Silver Spring. MD 233 pp.
N/A Last Accessed:
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February 17,2003
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-15
Analysis of Polychlorinated Biphenyls and Chlorinated Pesticides by Gas
Chromatography with Electron Capture Detection. LMMB 041
To quantify chlorinated hydrocarbons (i.e., chlorinated pesticides and PCBs) in
sample extracts.
This method is based on high resolution, capillary gas Chromatography using
electron capture detecton (GC/ECD). Extracts normally have a holding time of 40
days. This method provides for initial, ongoing and final calibrations, which are done
as part of the analytical run. If the response for any peak exceeds the highest
calibration solution, the extract is diluted, a known amount of surrogate and TCMX
solution added, and the sample reanalyzed for those analytes that exceeded the
calibration range. Concentrations in the samples are calculated based on the
internal standard method. Data are reported as ng/g dry weight.
Other methods describing the analysis of PCBs and pesticides by GC/ECD are
NS&T methods, ASTM Methods D5317 and D3534, and SW846 Methods 8081 A
and 8082 (NOAA, 1998; ASTM, 2001a).
PCBs and persistent pesticides (particularly DDT and metabolites) are two of the
primary risk factors of contaminated waters. Data are used in site characterization
and in risk analysis.
The ECD is very sensitive and allows for detection of the chlorinated hydrocarbons
at trace concentrations (ppb).
The detector does not have a linear response over a wide concentration
range and must be used by sufficiently trained personnel. Second column analysis
must be performed to provide unequivocal compound identification. These methods
do not measure the 12 World Health Organization congeners, which may be desired
data in some risk assessments.
USEPA. 1997d. Lake Michigan Mass Balance Study Methods Compendium.
Volume 2: Organic and Mercury Sample Analysis Techniques. EPA905-R-97-012c.
Great Lakes National Program Office. U.S. Environmental Protection Agency.
Chicago, IL.
http //www epa.qov/qrtlakes/lmmb/methods/
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February 17,2003
Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-16
PCBs and Pesticides in Surface Water by XAD-2 Resin Extraction, LMMB 039
This method is used to determine congener specific PCB and pesticide
concentrations at trace levels in surface water.
Water samples (80 - 160 L) are filtered for particulates and the dissolved PCBs are
collected using an XAD-2 resin column. Filters and resin columns are stored at 4°C
until analysis. The filters and resin are Soxhlet extracted using 50% acetone/50%
hexane for 16 hours The water remaining in the samples is extracted with hexane.
The sample extracts are concentrated and dried with sodium sulfate. The samples
are run through a Florisil column and then through a silica column. Two fractions
are collected from the silica column. The first fraction is eluded with hexane and
contains the PCBs, HCB, and p.p' DDE. The second fraction is eluded with 25%
ethyl ether in hexane and contains alpha-BHC, lindane, the chlordanes, nonachlors,
p.p'DDD, p.p'DDT. and toxaphene. These fractions are concentrated and further
cleaned with sulfuric acid. Sample extracts are analyzed by GC/ECD according to
Method LMMB 041 . Confirmation of pesticides in the second fraction is performed
on a second column or by GC/MS.
Preparation of XAD-2 Resin is presented in SW846 Method 0010: Appendix A
(USEPA SW846).
Water quality assessments under Clean Water Act, RCRA, or CERCLA
Extraction of water through resin perm its the economical extraction of large volumes
(>20 L) with this method.
XAD-Z resin is difficult to prepare for trace PCB application.
USEPA. 1997d. Method LMMB 039: PCBs and Pesticides in Surface Water by
XAD-2 Resin Extracton, Lake Michigan Mass Balance Study Methods
Compendium. Volume 2: Organic and Mercury Sample Analysis Techniques. EPA
905-R-97-012c. Great Lakes National Program Office, U.S. Environmental
Protection Agency, Chicago, IL.
http //www epaaov/grtlakes/lmmb/methods/ Last Accessed: 1/31/2003
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Purpose
Method Summary
Data
Uses/Application
2.1.2-17
Tetra- through Octa-Chlorinated Dioxms and Furans by Isotope Dilution
HRGC/HRMS, EPA Method 1613
This method is for determination of tetra through octa-chlorinated dibenzo-p-dbxins
(CDDs) and dibenzo furans (CDFs) in water.
This method is "performance-based." Stable iso topically labeled analogs of 15 of
the 2,3,7,8-substituted CDDs/CDFs are spiked into a 1 L water sample, and the
sample is extracted by one of three procedures:
1 . Samples containing no visible particles are extracted with methylene
chloride in a separatory funnel or by the solid-phase extraction technique. The
extract is concentrated for cleanup.
2. Samples containing visible particles are vacuum filtered through a glass-fiber
filter. The filter is extracted with toluene in a Soxhlet/Dean-Stark (SDS) extractor.
and the filtrate is extracted with methylene chloride in a separatory funnel. The
methylene chloride extract is concentrated and combined with the SDS extract prior
to cleanup.
3. The sample is vacuum filtered through a glass-fiber filter on top of a solid-phase
extraction (SPE) disk. The filter and disk are extracted in an SDS extractor, and the
extract is concentrated for cleanup. After extraction, 37CI4-labeled 2,3,7,8-TCDD is
added to each extract to measure the efficiency of the cleanup process. Sample
cleanups may include back-extraction with acid and/or base, and gel permeation.
alumina, silica gel, Florisil and activated carbon chromatography. High-performance
liquid chromatography (HPLC) can be used for further isolation of the 2,3,7,8-
isomers or other specific isomers or congeners. After cleanup, the extract is
concentrated to near dryness. Immediately prior to injection, internal standards are
added to each extract, and an aliquot of the extract is injected into the gas
chromatography. The analytes are separated by the GC and detected by a high-
resolution (210,000) mass spectrometer.
Minimum
CDD/CDF Level (pg/L) CDD/CDF ML(pg/L)
2.3,7,8-TCDF 10 1, 2,3,4.7 ,8-HxCDD 50
2,3,7,8-TCDD 10 1. 2,3,6,7 ,8-HxCDD 50
1 ,2,3,7,8-PeCDF 50 1 .2,3,7 ,8.9-HxCDD 50
2,3,4,7,8-PeCDF 50 1, 2,3,4,6,7 ,8-HpCDF 50
1,2,3,7,8-PeCDD 50 1, 2,3,4,7 ,8.9-HpCDF 50
1,2,3,4,7,8-HxCDF 50 1. 2.3,4,6,7 ,8-HpCDD 50
1,2,3,6.7,8-HxCDF 50 OCDF 100
1,2,3,7,8,9-HxCDF 50 OCDD 100
2,3,4,6,7,8-HxCDF 50
This method is also described in SW846 Method 8290 (USEPA SW846.
The method is for use in EPA's data gathering and monitoring programs associated
with the Clean Water Act, the Resource Conservation and Recovery Act, the
Comprehensive Environmental Response, Compensation and Liability Act, and the
Safe Drinking Water Act.
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Advantages
Limitations
Reference
Website
2.1 2-17 (contd)
Method 1613 is able to meet detection limits required for human health and
ecological risk assessments.
The GC/MS portions of this method are for use only by analysts experienced with
HRGC/HRMS or under the close supervision of such qualified persons.
USEPA. 1994c. Method 1613: Tetra- through Octa-Chlorinated Dioxms and Furans
by Isotope Dilution HRGC/HRMS, EPA 821-B-94-005. Office of Water, U.S.
Environmental Protection Agency. Washington, DC.
httDWwww eca aov/clarilon/cihtml/DubtilleOW h
tml
Last Accessed: 1/31/2003
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-18
Toxic Polychlorinated Biphenyls by Isotope Dilution High Resolution
Gas Chromatography/High Resolution Mass Spectrometry, EPA Method 1668
This method is for determination of the toxic Polychlorinated Biphenyls (PCBs) in
water.
This method is performance-based. Stable isotopically labeled analogs of the toxic
PCBs are spiked into a 1-L sample, and the sample is vacuum filtered through a
glass-fiber filter on top of a solid-phase extraction (SPE) disk. Sample com ponents
on the filter and disk are eluded with methylene chlonde and the eluant is
concentrated for cleanup. After extraction, samples are cleaned up using back-
extraction with sulfunc acid and/or base, and gel permeation, silica gel, Flonsil and
activated carbon chromatography. High-performance liquid chromatography (HPLC)
can be used for further isolation of specific isomers or congeners. After cleanup, the
extract is concentrated to neardryness. Immediately prior to injection, internal
standards are added to each extract, and an aliquot of the extract is injected into the
gas chromatography. The analytes are separated by the GC and detected by a high-
resolution (210,000) mass spectrometer.
The Method Detection Limit (MDL) for PCB #126 has been determined as 40 pg/L in
water using this method.
IUPAC EMDL(pgfl-) EML(pg/L)
77 5 20
123. 126 40 100
118/167/156/157/169/180/170/189 60 200
114 600 2000
105 400 1000
EMD: = Estimated Method Detection Limit; EML = Estimated Minimum Level
The method is for use in EPA's data gathering and monitoring programs associated
with the Clean Water Act, the Resource Conservation and Recovery Act, the
Comprehensive Environmental Response, Compensation and Liability Act, and the
Safe Drinking Water Act.
Method 1668 provides data for most, but not all, of the "dfoxin-iike" PCBs, including
those with the highest TEFs, as determined by the World Health Organization. This
method provides detection limits frequently required in risk assessments.
The GC/MS portions of this method are for use only by analysts experienced with
HRGC/HRMS or under the close supervision of such qualified persons. Method
1668 does not provide data for all of the "dioxm-like" PCBs, as does Method 1668A.
USEPA. 1997e. Method 1668: Toxic Polychlonnated Biphenyls by Isotope Dilution
HRGC/HRMS, EPA-821-R-97-001. Office of Water, U.S. Environmental Protection
Agency, Washington, DC.
http//www epa qov/clanton/clhtml/pubtitleOW h
tml
Last Accessed1 1/31/2003
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-19
Chlorinated Biphenyl Congeners in Water, Soil, Sediment, and Tissue by
HRGC/HRMS, EPA Method 1668 Revision A
This method is for congener-specific determination of more than 150 chlorinated
biphenyl (CB) congeners in water.
This method is performance-based. Stable isotopically labeled analogs of the 12
RGBs designated as toxic by WHO and labeled congeners at each level of
chlorination are spiked into a 1-L sample. The sample is extracted using solid-phase
extractbn, separatory funnel extraction, or continuous liquid/liquid extraction. After
extraction, a labeled cleanup standard is spiked into the extract which is then
cleaned up using back-extraction with sulfunc acid and/or base, and gel permeation,
silica gel, or Florisil chromatography. Activated carbon and high-performance liquid
chromatography (HPLC) can be used for further isolation of specific congener
groups. After cleanup, the extract is concentrated to 20 pL. Immediately prior to
injection, labeled injection internal standards are added to each extract and an
aliquot of the extract is injected into the gas chromatography (GC). The analytes are
separated by the GC and detected by a high-resolution (2 10,000) mass
spectrometer.
The estimated method detection limit (EMDL) for congener 126 in water is 5 pg/L
with no interferences present. Without interferences, EMDLs and EMLs are,
respectively, 5 and 10 pg/L for aqueous samples, and EMLs for extracts are 0.5
pg/uL.
EMD. = Estimated Method Detection Limit; EML = Estimated Minimum Level
This Method is for use in data gathering and monitoring associated with the Clean
Water Act, the Resource Conservation and Recovery Act, the Comprehensive
Environmental Response. Compensation and Liability Act, and the Safe Drinking
Water Act.
Method 1668A provides congener data that can be used for source identification.
Listed PCBs include the 12 World Health Organization "dioxin-like" PCBs. The
HRMS method provides lower EMDLs compared to ECD or low resolution MS
analyses and provides unequivocal congener identification.
The GC/MS portions of this method are for use only by analysts experienced with
HRGC/HRMS or under the close supervision of such qualified persons. Solvents,
reagents, glassware, and other sample processing hardware may yield artifacts,
elevated baselines, and/or lock mass suppression causing misinterpretation of
chromatograms
USEPA 1999c. Method 1668, Revision A: Chlorinated Biphenyl Cogeners in Water.
Soil, Sediment, and Tissue by HRGC/HRMS, EPA-821-R-QO-002. Office of Water.
U.S. Environmental Protection Agency. Washington. DC.
Rev A not available online Last Accessed:
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-20
ESS Method 220.3: Ammonia Nitrogen and Nitrate+Nitrite Nitrogen, Automated
Flow Injection Analysis Method, LMMB 061
This method is for the simultaneous determination of ammonia and nitrate/nitrite in
surface, drinking, and ground waters, and domestic and industrial wastes.
Water samples are collected and preserved with sulfuric acid. Samples are
analyzed directly using an automated flow injection analyzer. For ammonia, alkaline
phenol and sodium hypochlorite react with ammonia to form a blue compound that is
proportional to the ammonia concentration. Ammonia is measured colorimetrically at
630 nm. For nitrate+nitrite-N, nitrate is quantitatively reduced to nitrite using a
copperized cadmium column. The sample solution (total nitrite) then reacts with
sulfanilamide and N-(1-naphthyl)ethylenediaminedihydrochloride to form a magenta
solution. Total nitrite is measured colorimetrically at 520 nm. Nitrite alone can be
determined by removing the cadmium column. Nitrate is quantified by subtracting
the measured nitrite concentration from the measured total nitrite concentration.
Samples with a concentration of 0.02-10.0 mg NH3-N/L and 0.02-35.0 mg NO3+NO2-
N/L can be analyzed with this method These ranges can be extended through the
use of a digital diluter
ASTM Method D1426 and Standard Method 4500-NH3C also describe the
colorimetric determination of ammonia (ASTM, 2001 a; APHA, 1999). ASTM
Method D 3867 and Standard Methods 4500-NO2".B and 4500-NO3'.F describe the
analysis of nitrite and nitrate.
The spatial and temporal variations in nutrients concentrations are often critical
parameters for understanding aquatic productivity and conditons of estuanne
habitat.
EDTA used in this procedures inhibits precipitation of residual calcium and
magnesium ions. The detection range of this method includes most concentrations
found in the environment.
Since a straight line calibration curve is not obtained, a greater number of standards
is needed.
USEPA. 1997c. Method LMMB 061. ESS Method 220.3: Ammonia Nitrogen and
Nitrate+Nitnte Nitrogen, Automated Flow Injection Analysis Method, Lake Michigan
Mass Balance Study Methods Compendium, Volume 3: Metals, Conventionals,
Radio chemistry, and Biomonitoring Sample Analysis Techniques. EPA 905-R-97-
012c. Great Lakes National Program Office, U.S. Environmental Protection Agency,
Chicago, IL.
http.//www.epa qov/grtlakes/lmmb/methods/ Last Accessed: 1/31/2003
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Method Title
Purpose
Method Sum m ary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2 1 2-21
ESS Method 230 V Total Phosphorus and Total Kjeldahl Nitrogen, Semi-Automated
Method, LMMB 062
This method is for the determination of total Kjeldahl nitrogen and total phosphorus
in drinking, surface and was te waters
Water samples are collected and preserved in the field using sulfunc acid In this method.
organic nitrogen and phosphorus compounds are digested using a sulfunc acid solution
containing potassium sulfate Mercuric sulfate is used as a catalyst in the digestion
HzSO« + organic nitrogen Hg (NHt^SOi teSO*
H2S04 + organic phosphorus Hg KaPO* feSCb
Tubes of sam pie aliquots and acid are placed in a block digester, where they are heated
at 200°C for about 1 hour and then at 380°C for 75 minutes. The digestate is analyzed
spectrophotom etncally as am m onia and phosphate using an Auto Analyzer Total
phosphorus and total Kjeldahl nitrogen concentrations are obtained directly from the
plotter.
Method LMMB 058 describes the general operating and maintenance procedures for using
the Auto Analyzer The Auto Analyzer is comprised of a sam pier, proportioning pump.
manifold, colorimeter, and printer/plotter The flow of reag ents and samples are
proportioned by the pump, and air bubbles introduced into the tubing help to sep arate
samples, mix reagents, and cleanse tubing
The operating range for this method is 0 1 to 10 0 mg N/L and 0 02 to 2 00 mg P/L
Standard Method 4500-N o^B and ASTM Method D3590 describe the determination of
Kjeldahl nitrogen (APHA. 1999, ASTM, 2001a)
This method details the conversion of nitrogen compounds such as ammo acids.
proteins and peptides to am m onia and can be used to evaluate drinking, surface
and was te waters
Many water quality assessm ents require the measurem ent of total kjeldahl nitrogen
The digestion process may not convert all compounds (amines, nitro compounds.
hydrazones, oximes, semicarbazones, and some tertiary amines) to amm onia
USEPA. 1997c Method LMMB 062 ESS Method 230 1 Total Phosphorus and
Total Kjeldahl Nitrogen, Semi-Automated Method, Lake Michigan Mass Balance
Study Methods Compendium, Volume 3- Metals, Conventional, Radio chem istry.
and Biomomtonng Sam pie Analysis Techniques EPA 905-R-97-012c Great Lakes
National Program Office. U S Environmental Protection Agency, Chicago, IL
http //www epa gov/grtlakes/lmm b/methods/ ^^ Accessed 1/31/2003
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-22
ESS Method 310 2: Phosphorus, Total. Low Level (Persulfate Digestion), LMMB
064
This method is for the determination of total phosphorus in surface waters.
W ater samples are collected and preserved in the field with sulfunc acid They are stored
at 4°C until analysis To determine dissolved phosphorus, samples are filtered through a
0.45um filter before digestion The samples are digested with ammonium persulfate and
sulfuric acid in an autoclave for 30 minutes at 121°C All phosphorus is converted to
ortho-phosphate After the digestion, any paniculate matter is allowed to settle overnight.
Orthophosphate is then analyzed spectrophotometncally using an Auto Analyzer. The
phosphorus concentration is obtained directly from the plotter
Method LMMB 058 describes the general operating and maintenance procedures for using
the Auto Analyzer. The Auto Analyzer is comprised of a sampler, proportioning pump.
manifold, colonmeter, and pnnter/plotter. The flow of reagents and samples are
proportioned by the pump, and air bubbles introduced into the tubing help to separate
samples, mix reagents, and cleanse tubing
The operating range for this method is 0 002-0 200mg P/L
The persulfate digestion procedure is also described in Standard Method 4500-P.B 5
(APHA, 1999)
These measurem ents are often required for water quality studies.
The automated analysis allows economical analyses of multiple samples.
This method describes only the phosphorus method.
USEPA.1997C Method LMMB 064 ESS Method 310 2 Phosphorus, Total, Low Level
(Persulfate Digestion), Lake Michigan Mass Balance Study Methods Compendium,
Volume 3. Metals, Conventional, Radio chemistry, and Biomomtonng Sample Analysis
Techniques EPA 905-R-97-012c. Great Lakes National Program Office. U S.
Environmental Protection Agency, Chicago. IL
http //www epa gov/grtlakes/lmm b/methods/ LaSt Accessed. 1/31/2003
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.12-23
ESS Method 310.1 : Ortho-Phosphorus, Dissolved Automated, Ascorbic Acid, LMMB
063
This method is for the determination of ortho phosphate in most waters and
wastewater.
Water samples are collected, filtered through a 0.45 urn filter, cooled to 4°C, and
analyzed as soon as possible. The samples are analyzed spectrophotometrically
using an auto analyzer. In the instrument, ammonium molybdate and antimony
potassium tartrate react in an acid medium with dilute solutions of orthophosphate-
phosphorus to form an antimony-phospho-molybdate complex. This complex is
reduced to an intensely blue-colored complex by ascorbic acid. The color is
measured at 880 nm and is proportional to the phosphorus concentration. The
phosphorus concentration is obtained directly from the plotter.
Method LMMB 058 describes the general operating and maintenance procedures
for using the auto analyzer. The auto analyzer is comprised of a sampler,
proportioning pump, manifold, colorimeter, and printer/plotter. The flow of reagents
and samples are proportioned by the pump, and air bubbles introduced into the
tubing help to separate samples, mix reagents, and cleanse tubing.
The operating range for this method is 0.002-0.200mg P/L. This range may be
extended to 0.2-2.00 mg P/L by utilizing a dilution loop.
The automated ascorbic acid reduction method is also described in Standard
Method 4500-P F (APHA, 1999)
These measurements are useful for productivity assessments and site
characterizations.
The auto analyzer method provides fast, reproducible nutrient results
Barium, lead, and silver may interfere with the analysis by forming a precipitate.
USEPA. 1997c. Method LMMB 063: ESS Method 310.1: Ortho-Phosphoius,
Dissolved Automated, Ascorbic Acid, Lake Michigan Mass Balance Study Methods
Compendium, Volume 3: Metals, Convent'onals, Radio chemistry, and
Biomonitoring Sample Analysis Techniques. EPA 905-R-97-012c. Great Lakes
National Program Office, U.S. Environmental Protection Agency. Chicago, IL.
http //www epa qov/qrtlakes/lmmb/methods/ Last Accessed: 1/31/2003
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Method Title
Purpose
Method Summary
Data Uses/Application
Advantages
Limitations
2.1.2-24
Total Organic Carbon, Standard Method 5310
This method is for the determination of total organic carbon in a wide variety of
water samples.
TOG methods utilize heat and oxygen, ultraviolet irradiation, chemical
oxidants, or combinations of these oxidants to convert organic carbon to
carbon dioxide (COj). The C02 may be measured directly by a nondispersive
infrared analyzer, reduced to methane and measured with a flame lonizafaon
detector, or CO2 may be titrated chemically.
In the Combustion-Infrared Method (5310B). the sample is homogenized and
diluted as necessary, and a microportion is injected into the heated reaction
chamber of a carbon analyzer, which is packed with an oxidative catalyst. The
water is vaporized, and the carbon is oxidized to CO2 and H2O. The CO2 from
oxidation of organic and inorganic carbon is measured by means of a
nondispersive infrared analyzer. This gives the measure of total carbon. TOC
is obtained by the difference of total carbon and inorganic carbon (1C). 1C is
measured by injecting the sample into a separate reaction chamber packed
with phosphoric acid-coated quartz beads. Under acidic conditions, all 1C is
converted to COZ. which is measured. Under these conditions, organic carbon
is not oxidized and only 1C is measured. Alternatively. TOC can be measured
by first acidifying the sample and purging the inorganic carbon from the sample
and then measuring the remaining carbon.
Other methods for measuring TOC exist, such as the Persulfate-Ultraviolet
Oxidation Method (5310C) and the Wet-Oxidation Method (5310D). In both of
these methods, organic carbon is oxidized to CO2 using persulfate. ASTM
Methods D6317, D2579, D4129, D4839, and D5790 and SW846 Method 9060
also describe various methods for the analysis of total organic carbon (ASTM,
2001a;USEPASW846).
Dissolved organic carbon (DOC) can be measured by first filtering the sample
through a 0.45-Mm-pore-diam filter. Particulate organic carbon (POC) is the
fraction of TOC retained by this filter and is analyzed using a CHN elemental
analyzer.
The minimum detectable concentrations are 1 mg carbon/L, 0.05 mg organic
carbon/L, and 0.10 mg organic carbon/L can be measured with methods
5310B. 5310C, and 5310D, respectively. Method LMMB 067 (USEPA 1997c)
has an MDL of 5ug for POC.
Site characterization. TOC is also used in the assessment of trace metal and
organic contaminant data.
One of several standard methods for TOC analysis.
Acidification, purging, and sample blending may result in the loss of volatile
organic substances. Large organic particles may fail to enter the needle used
for sample injection or may oxidize slowly.
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Website
2.1. 2-24 (contd.)
APHA. 1999. Standard Methods for the Examination of Water and
Wastewater, 20th Edition.
N/A
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Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-25
Standard Operating Procedure for the Analysis of Dissolved-Phase Organic Carbon
in Great Lakes Waters. LMMB 096
To measure dissolved organic carbon (DOC) in the filtrates of water samples.
Samples are filtered immediately after collection, and stored at4°C until analysis on
the ship. Samples that are sent to the lab for analysis are frozen after arrival.
Inorganic carbon is removed from the filtrate by the addition of sulfunc acid and
purging of the sample with organic-free air. The samples are analyzed by
conversion of organic carbon to CO2 by an ultraviolet (UV) digester. The resulting
C02 is detected by a non-dispersive infrared (IR) analyzer. The concentration of
dissolved organic carbon is calculated using the peak height method.
Alternatively. Method LMMB 066 measures DOC by high temperature (680°C)
catalytic oxidation (USEPA 1997c). Inorganic carbon is first removed by
acidification and purging. The C02 resulting from organic carbon is detected by a
nondispersive infrared (IR) analyzer This method is applicable to organic carbon
concentrations from 0.2 to 50 mg/L and inorganic carbon concentrations less than
1000 mg/L.
Standard Method 5310 also describes the analysis of dissolved organic carbon
(APHA, 1999}.
Dissolved and participate metals and organic contaminant data are frequently
compared to DOC.
Both methods provide a rapid, reproducible analytical method for DOC analysis.
Results for volatile organic compounds using this method may be low.
USEPA. 19976. Method LMMB 096: Standard Operating Procedure for the
Analysis of Dissolved-Phase Organic Carbon in Great Lakes Waters, Lake Michigan
Mass Balance Study Methods Compendium, Volume 1: Sample Collection
Techniques. EPA 905-R-97-012c. Great Lakes National Program Office, U.S.
Environmental Protection Agency, Chicago, IL.
http //www epa gov/grtlakes/lmmb/methods/ Last Accessed- 1/23A7003
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February 17,2003
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-26
Standard Operating Procedure for the Analysis of Particulate-Phase Organic
Carbon in Great Lakes Waters, LMMB 097
To measure paniculate organic carbon (POC) in the filtrates of water samples.
Samples are filtered immediately after collection through glass fiber filters. Four
12mm discs are cut from each filter and allowed to dry. The disks are folded and
placed into individual tin sample containers. The disks are analyzed by catalytic
combustion using an elemental analyzer (CHNS analyzer). The sample container
with the disk is placed into a 1000°C furnace with a catalytic reactor tube. The
sample is oxidized, and the sample gases pass through a packed chromatographic
column for separation. The sample components are separated as CO2, H2, N2, and
H2S. The components are detected by thermal conductivity detection (TCD). To
calculate POC concentration in mg/L, the resulting mass of carbon from the four
discs per sample are summed, multiplied by an area correction factor, and divided
by the volume of water filtered.
Alternatively, Method LMMB 067 first treats the sample filters with sulfurous acid,
dries the filters at 60°C for 20-30 minutes, acidifies the filters again and dries them
again for 1 hour prior to analysis (EPA 905-R-97-012c). The entire filter is analyzed
using a CHN elemental analyzer The method detection limit for this procedure is 5
ug of organic carbon remaining on a GF/F filter. The maximum amount of carbon
measurable is approximately 5 mg of carbon.
Standard Method 5310 also describes the analysis of particulate organic carbon
(APHA, 1999).
Normalization of trace metal and organic contaminant data; flux measurements.
This method can be highly automated.
Results for volatile organic compounds using this method may be low.
USEPA. 1997b. Method LMMB 097. Standard Operating Procedure for the
Analysis of Particulate-Phase Organic Carbon in Great Lakes Waters, Lake
Michigan Mass Balance Study Methods Compendium, Volume 1: Sample Collection
Techniques. EPA 905-R-97-012c. Great Lakes National Program Office, U.S.
Environmental Protection Agency, Chicago, IL.
http //www epa qov/qrtlakes/lmmb/methods/ Last Accessed: 1/23/2003
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-27
ESS Method 140.4: Chloride - Automated Flow Injection Analysis, LMMB 060
This method is for the determination of chloride in drinking water, surface water,
saline water, domestic and industrial wastes.
Water samples are collected and analyzed within 28 days. Samples are analyzed
directly using an automated flow injection analyzer. This method is based on the
interaction of chlorine ions and mercuric thiocyanate. As a result, a highly colored
solution is formed, which is measured colonmetrically.
Samples with a concentration of 1.0-100 mg CI/L can be analyzed directly. This
range can be extended through the use of a digital diluter.
Standard Method 4500-CI' E also describes the automated analysis of chloride
(APHA, 1999). Alternative methods for measuring chlorine include litraSon and use
of ion-selective electrode. These are described in ASTM Method D512 and
Standard Methods 4500-Cr B, C, and D (ASTM, 2001 a; APHA, 1999). The ion-
selective electrode method can measure chloride concentrations up to 1000 mg
CI/L.
The EPA recognizes chloride in drinking water as a secondary standard.
This method is capable of analyzing up to 100 samples per hour.
Since a straight line calibration curve is not obtained, a greater number of standards
is needed.
USEPA. 1997c. Method LMMB 060: ESS Method 140.4: Chloride - Automated
Flow Injection Analysis, Lake Michigan Mass Balance Study Methods Compendium,
Volume 3: Metals, Conventional, Radio chemistry, and Biomonitoring Sample
Analysis Techniques. EPA 905-R-97-012c. Great Lakes National Program Office,
U.S. Environmental Protection Agency, Chicago, IL.
http //www epa qov/qrtlakes/lmmb/methods/ Last Accessed: V23/2003
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-28
ESS Method 200.5: Determination of Inorganic Anions in Water by Ion
Chromatography, LMMB059
This method is for the determination of chloride, n'rtrate-N, and sulfate in drinking
water, surface water, and mixed domestic and industrial wastewater.
Water samples are collected and preserved as follows:
Chloride: No preservation required. Analyze within 28 days.
Nitrate-N-: Cool to 4°C. Analyze within 48 hours.
Sulfate: Cool to 4"C. Analyze within 28 days.
Samples are filtered through a 0.45 urn filter to remove paniculate matter. A portion
of the sample (usually 5 mL) is injected into the ion Chromatography, comprised of a
guard column, separator column, suppressor column, and conductivity detector .
The anions are separated based on their affinity for the exchange sites of the resin
in the analytical and guard column. Anions are identified base on their retention
times compared to known standards. Results are reported as mg/L.
Alternative methods for the determination of anions (including additional anions,
such as phosphate and nitrite) by Ion Chromatography are Standard Method 41 10B,
ASTM D4327, and SW846 9056 (APHA, 1999; ASTM, 2001a,USEPA SW846).
Site characterization/site assessment.
The suppressor column reduces background conductivity.
Phosphate is not analyzed with this method. Nitrite can interfere with the detection
of chloride.
USEPA. 1997c Method LMMB 059: ESS Method 200.5: Determination of
Inorganic Anions in Water by Ion Chromatography, Lake Michigan Mass Balance
Study Methods Compendium, Volume 3. Metals, Conventional, Radio chemistry,
and Biomonitoring Sample Analysis Techniques. EPA 905-R-97-012c. Great Lakes
National Program Office, U.S. Environmental Protection Agency, Chicago, IL.
http //www epa gov/grtlakes/lmmb/methods/ Last Accessed: 1/23/2003
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/ Application
Advantages
Limitations
Reference
Website
2.1.2-29
Standard Operating Procedure for Electrometric pH, LMMB 092
To measure pH in drinking, surface, and saline waters; domestic and industrial
wastes.
The working range of this method is 6.0 to 10.0 pH units. Samples are collected in
clean glass or plastic containers and stored at 4°C until analysis. The pH meter is
calibrated with 7.0 and 10.0 buffers. The sample is brought to 25°C before analysis.
An aliquot of the sample is placed into a suitable container, which is then placed on
a stirrer. The pH meter electrode is submerged into the sample and the pH reading
is taken once the meter stabilizes.
ASTM Method D1293, Standard Method SM 4500-H*.B, and SW846 Method 9040B
also describe the measurement of pH of water (ASTM, 2001 a; APHA, 1999).
The pH of water is an important parameter in the solubility of trace minerals in water
and the suitability of the water to sustain life.
Little skill and training is needed to perform this analysis.
Temperature affects the electrometric response and must be compensated for.
Extremely acidic waters require a different calibration range (i.e., 4.0 and 7.0
buffers).
USEPA. 1997c. Methods LMMB 092: Standard Operating Procedure for
Electrometric pH, Lake Michigan Mass Balance Study Methods Compendium,
Volume 1: Sample Collection Techniques. EPA 905-R-97-012c. Great Lakes
National Program Office, U.S. Environmental Protection Agency, Chicago, IL.
http //www epa qov/qrtlakes/lmmb/methods/
Dhvdnon odf
Last Accessed- 1/23/2003
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-30
Standard Operating Procedure forGLNPO Total Alkalinity Titration, LMMB 091
To measure alkalinity in drinking, surface, and saline waters; domestic and industrial
wastes.
This method is designed for waters in the range of 10 - 250 mL/L total alkalinity as
CaCO3. The pH meter is calibrated with 4.0 and 7.0 buffers. 100mL of sample are
titrated with 0.0200 N sulfuric acid to pH 4.5. Total alkalinity is calculated as CaCO3
in mg/L by multiplying the volume of titrant (in ml) by 10.
Similar methods for the measurement of alkalinity are described in ASTM Methods
D1067 and D3875 and Standard Method 2320B (ASTM, 2001 a; APHA, 1999).
Alkalinity is a measure of water's natural buffering capacity, thus an important
parameter measured to assess overall water quality.
This method can be automated or semi-automated for multiple analyses
Oil, grease, and high mineral content may interfere with the alkalinity determination.
USEPA. 1997b. Methods LMMB 091: Standard Operating Procedure for GLNPO
Total Alkalinity Titration, Lake Michigan Mass Balance Study Methods
Compendium, Volume 1: Sample Collection Techniques. EPA 905-R-97-012c.
Great Lakes National Program Office, U.S. Environmental Protection Agency,
Chicago, IL.
http //www eoa aov/qrtlakes/lmmb/methods/ Last Accessed- 1/23J?nm
alkali pdf
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-31
Standard Operating Procedure for GLNPO Specific Conductance: Conductivity
Bridge, LMMB 094
To measure conductance of drinking and surface waters.
Samples are collected and stored at 4°C until analysis. The specific conductance of
the samples is measured using a self-contained conductivity meter. Care should be
taken to assure that not air bubbles are present in the conductivity cell. The
temperature is adjusted to 25°C and the conductivity read.
The approximate working range of this method of 10-500 mhos/cm.
ASTM Method D1225, Standard Method 251 OB. and SWB46 Method 9050A
describe similar methods for the measurement of conductivity of water (ASTM,
2001a: APHA. 1999). The test range of Method D1225A is 10-200000 uS/cm.
This method is applicable to the quantitative measurement of ionic constituents
dissolved in water.
The procedure and equipment are simple and easy to operate
Sample temperatures other than 25°C will cause incorrect results. Oil, grease,
algae, or dirt may interfere with the readings.
USEPA. 1997b. Method LMMB 094: Standard Operating Procedure for GLNPO
Specific Conductance: Conductivity Bridge, Lake Michigan Mass Balance Study
Methods Compendium, Volume 1: Sample Collection Techniques. EPA 905-R-97-
012c. Great Lakes National Program Office, U.S. Environmental Protection
Agency, Chicago, IL.
http //www epa aov/qrtlakes/lmmb/methods/ Last Accessed- 1/23/7003
conduct) odf
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-32
Standard Operating Procedure for GLNPO Turbidity: Nephelometeric Method,
LMMB090
To measure turbidity in drinking, surface, and saline waters.
Turbidity samples are analyzed immediately or stored at 4°C. The working range of
the turbidimeter is 0-20 nephelometeric turbidity units (NTU). Dilutions can be
performed to measure turbidities greater than 20 NTU. The instrument is calibrated
with a geometric series of calibration standards. An aliquot of the sample is warmed
to 25°C and placed into the turbidimeter for measurement. The instrument
measures turbidity by comparing the intensity of light scattered by the sample with
the intensity of light scattered by a standard reference suspension.
ASTM Method D1889 and Standard Method 2130B describe a similar method of
measuring the turbidity of water (ASTM, 2001 a; APHA, 1999). These methods have
a working range of 1.0-40 NTU.
Turbidity is measured as part of overall site characterization, as an indirect measure
of light penetration. Turbidity can also be monitored during dredging or other
sediment excavations to measure amounts of suspended material entering the
environment for site activities.
Turbidity measured with a nephelometer provides a much more rapid and
reproducible measurement compared to the filtration/color chart method.
Floating debris and air bubbles in the sample may give high readings
Condensation or scratches on the sample vial and sample color may give erroneous
readings
USEPA. 1997b. Methods LMMB 090: Standard Operating Procedure for GLNPO
Turbidity: Nephelometeric Method, Lake Michigan Mass Balance Study Methods
Compendium, Volume 1: Sample Collection Techniques. EPA 905-R-97-012c.
Great Lakes National Program Office, U.S. Environmental Protecbon Agency,
Chicago, IL.
http //www epa qov/grtlakes/lmmb/meth
ods/turbid odf
Last Accessed: 1/23/2003
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-33
ESS Method 340.2: Total Suspended Solids. Mass Balance (Dried at 103-105°C)
Volatile Suspended Solids (Ignited at 550°C), LMMB 065
To measure the portion of total solid retained by a filter from drinking, surface, and
saline waters; domestic and industrial wastes.
Water samples are collected by submersible pump or Rosette sampler. A sample
volume is selected that will yield 2 - 20.000 mg/L. total suspended solids. For
open-lake oligotrophic conditions, 2-4 liters will provide enough participate matter.
For near-shore or eu trophic conditions, 200-500 mL may be sufficient. A well-mixed
sample is filtered through a preweighed standard glass-fiber filter, and the residue
retained on the filter is dried at 103 to 105 °C for at least one hour. The increase in
weight of the filter represents the total suspended solids.
After determining TSS, the filters may be placed in a muffle furnace and ignited at
550°C for 30 minutes to determine volatile suspended solids (VSS).
Following Method LMMB 098, water samples can be filtered in the field and then
frozen at -10°C until final weighing in the laboratory.
Standard Method 2540D, ASTM Method D5907, and Standard Operating
Procedures and Field Methods Used for Conducting Ecological Risk Assessment
Case Studies describe similar methods for measuring total suspended solids
(APHA, 1999; ASTM, 2001 a; USEPA 1992b, respectively).
TSS is an ancillary parameter to the determination of hydrophobic organic
contaminants (HOCs).
Glass fiber filters can be ignited without damage, allowing TSS and VSS to be
performed on the same set of filters.
Excessive residue on the filter may form a water-entrapping crust. Sample size
should be limited to yield no more than 200 mg residue. Glass fiber filters are not
appropriate for measurement of TSS in estuarine waters.
USEPA. 1997c. Method LMMB 065: ESS Method 340.2: Total Suspended Solids,
Mass Balance (Dried at 103-105°C) Volatile Suspended Solids (Ignited at 550°C).
Lake Michigan Mass Balance Study Methods Compendium, Volume 3- Metals,
Conventbnals, Radio chemistry, and Biomomtoring Sample Analysis Techniques.
EPA 905-R-97-012c. Great Lakes National Program Office, U.S. Environmental
Protection Agency. Chicago. IL.
http://www epa qov/qrtlakes/lmmb/meth Last Accessed: 1/23/2003
ods/methd340 odf
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.2-34
Total Hardness Titration, LMMB 095
To measure the total concentration of the calcium and magnesium ions expressed
as calcium carbonate.
A water sample is collected at mid depth during un stratified conditions, or on the
mid-epilimnion and mid hypo-limmon when stratification is present A 100 mL water
sample is buffered to pH 10.1, and an indicator (such as Chrome Black T3) is then
added to the buffered sample. The indicator turns red in the presence of Ca and Mg
ions. The sample is titrated with 0.01 M EDTA, which complexes with Mg and Ca
cations, removing them from association with the indicator. When all the Mg and Ca
are complexed with EDTA, the indicator will turn blue. The volume of titrant is
recorded. Total Hardness is calculated as 10 X ml of titrant and reported as mg/L
as CaC03. Standard Method 2340C and ASTM Method D1 126 also describe the
titration analysis of hardness (APHA, 1999; ASTM, 2001 a).
An alternative method for the analysis of hardness is to determine the amount of
calcium and magnesium ions separately and then sum them to calculate total
hardness. Standard Method 2340B and ASTM Method D1126 both describe this
alternative method (APHA, 1999; ASTM. 2001 a). When determined as separate
ions, hardness is calculated as: 2.497[Ca, mg/L] + 4.1 18 [Mg. mg/L]
Hardness is measured in aquatic systems
toxicity in fish.
because it is known to mitigate metals
The reagents and chemicals required for this analysis can be obtained as
prepackage test kits. The titration method affords a means of rapid analysis, where
as the calculation method is more accurate.
This test method is not suitable for highly colored waters, which obscure the color
change of the indicator. A limit of 5 minutes is set for the duration of the titration to
minimize the tendency toward CaCO3 precipitation.
USEPA. 1997c. Method LMMB 095: Total Hardness Titration. Lake Michigan Mass
Balance Study Methods Compendium. Volume 3: Metals, Conventtonals, Radio
chemistry, and Biomonitoring Sample Analysis Techniques. EPA 905-R-97-01 2c.
Great Lakes National Program Office, U.S. Environmental Protection Agency,
Chicago, IL.
http //www epa gov/qrtlakes/lmmb/melh
ods/titratio odf
Last Accessed: 1/23/2003
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2.1.3 Biological Analysis Methods
Section 2.1.3 provides a compendium of water-related biological analyses. As mentioned
previously, once contaminants enter into an aqueous system, the contaminant's chemical nature
and the biological, chemical, or physical characteristics of the receiving water body will determine
whether it remains in the water column, becomes buried in sediment, or is ingested by organisms.
The negative impacts of contaminant exposure can be examined in laboratory toxicity tests, which
use site-specific effluents, leachates or elutriates prepared from sediments collected from the site.
All liquid-phase toxicity tests are performed to ultimately determine the lowest observable effect
concentration, the no observable effect concentration and other related parameters. These
results are then compared with chemistry data to identify and compare toxicity effects data with
contaminant exposure data to determine risk to ecological or human receptors. While elutriate
toxicity testing is performed to evaluated sediment toxicity, they are included in this section
because the same aqueous phase methods are also used to evaluate water and wastewater.
The advantages and limitations associated with each test are provided in their respective fact
sheets. However, there are general limitations in interferences associated with all liquid-phase
toxicity tests. These potential interferences are identified by some of the source documents
(USEPA, 1994d; Weber, 1991). They are listed below:
Toxicity tests do not reflect temporal fluctuations in effluent toxicity;
Non-target chemicals can cause adverse effects to the organisms giving false
results;
dissolved oxygen depletion due to biological and chemical oxygen demand and
metabolic wastes can be a problem;
The toxicant may be lost through volatilization and adsorption to the exposure
chamber; and,
The effect of the toxicant is organism dependant.
Liquid-phase toxicity tests vary considerably in test length, endpoints, and test species. Table
2.1.3-1 summarizes those toxicity tests described in the fact sheets, however it highlights the
differences between specific organisms to aid the Superfund manager with selecting the most
appropriate test for his/her site.
The toxicity test fact sheets provide methods described in USEPA guidance documents, Dredging
Manuals and ASTM reports. Specifically, the following sources provided methods information for
section 2.1.3:
• The USEPA's Environmental Response Team SOP's (USEPA, 1994b); ERT SOPs
are available online at: http://www.ert.org
www.epa.Qov/waterscienceWET/disk1/
• The USEPA's Methods document for Effluents and Receiving waters (Weber, 1991 );
• The USEPA's guidance document for contaminated sediment assessment in the Great
Lakes (USEPA, 1993a);
• The Inland Lakes Testing Manual (USEPA and USAGE, 1998);
• The USEPA's Environmental Research Laboratory-Narragansett (USEPA and the
Naval Construction Battalion Center, 1992)
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Table 2.14-1. A Summary of Teal Type* and lexicological Endpolnts for LlquM-Phau Toxlclty ' '
Teal Type/Fact
Sheet Number
Acute Freshwater
213-1
Acute Freshwater
213-1
Acute Freshwater
213-2
Chronic
Freshwater
213-3
Chronic
Freshwater
2 13-4
Chronic
Freshwater
213-5
Chronic
FreshwafiBf
213-6
Chronic
Freshwater
213-6
Chronic
Freshwater
2 1 3-17
Acute Mama
21 3-7
Acute Marne
213-g
Acute Marine
2 13-9
Acute Marine
213-9
Teat Organism
Crustacean
Crustacean
Fish
Algae
Crustacean
Crustacean
Crustacean
Fish
Fish
Macioalgaa
Crustacean
Fish
Fish
Scientific name
Dapniua magna
Dephnla Pule*
P/mepbates
Promelas
Salanastrum
caprcornutim
Canodaphnia
dubia
Daphnia magm
Dapltnm Palax
Pimeptiabs
prowalas
Pimepliales
proffteuis,
Ictaluws
punctatus.
Coregomii artedil,
Oryzfes (srjpes,
Cacastomus
conwnoraoni, Eaox
lucius, Dan/0
danio
Champa parwja
Mysidoposis
baha
Cypnnotton
vanagatua
Memdia beryfna
Endpolnts
Survival
Survival
Survival
Growth,
biosfcmulalory
effects (cell density
Survival.
reproduction
Reproduction.
growth
Reproduction.
growth
Larval Survival and
growth
Survival, growth
Sexual
repioduclnn
1-25 ppt
Survival
Survival
Test Specifics
Static, state-
renewal. 24. 48 or 96
hours
Static, static-
renewal, 24, 48 or 95
hours
Static, static-renewal.
24. 48 or 96 hours
Static. 96 hours
Static renewal. 7
days
Static-renewal. 10
days
Static-renewal. 10
days
Static-renewal, 7
days
Single exposure. 31
days (100 days for
Coregonusaitodll)
Static. 48 hours
Static-renewal, 96
hours
Static-renewal. 24. 49
or 96 hours
Static-re newel, 24. 46
or 96 hours
Comments
Commonly used (or bioassays.
optimum pH 6 8-8 5
Commonly used for bioassays.
optknum pH 6 8-8 5
Other commonly used freshwater
fish In bioassays Include the
Oncornynchus im/Aisi
Originally designed as a
autrephication test, now used In the
Superfand program for effluents
Commonly used lorbioasssys
Commonly used for bioassays.
optimum pH 8 8-8 5
Commonly used for bioassays.
optimum pH 6 8-8 5
Other commonly uted freshwater
fish in bioassaya include the
Oncorhynchus mytms
One of the few. published earty lite
stage methods
Used lor whole affluent toxicily
testng in the NPDES Program
Olhercommonly used
ostuanneAnarme mysid shrimp in
bioassays Include the
Hotmasfmysls costate and the
Neomy&fs amerfcana
Commonly used In bloasssya
Commonly used in bioassays
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Table 2. 1.3-1. (con td)
Test Type
Chronic Marina
213-10
Chronic Marine
213-11
Chronic Marine
2 1.3-12
Chronic Marine
2 1 3-12
Teat Organism
Crustacean
EC hlno donn
Fish
Fish
Scientific Name
Mysidopsls to/in
Aittcle
punctulate
Cypnnodon
vanagatm
Mania/a barylna
Endpolnts
Survival, growth.
fecundity
Toxldty to eggs and
B perm/ %
fertlteetlon
Larval survival and
growth
Larval survival and
growth
Teet Specifics
Static-renewal. 7
days
One hour
static-renewal, 7 days
static-renewal, 7 days
Comments
Other commonly used
estuanna/rnarlne mysld shrimp In
broassays Include the
Holmesimysis eostata ana
Neomysls aimncana
Chronic test but test lime Is quite
short
Commonly used In bloassays
Commonly used forbnassays
1 Three species are generally recommended for water column broassays They should represent different phyla where possible
2 Specific characterises to consider when selecting water-column test species include availability year-round, tolerance to handing and laboratory conditions.
consistent and reproducible responses to toxicants, phylogemc similarities to species characteristic of those mhabing water column at Impacted area,
availability of standardized test protocols, ability to test as Juvenles or larvae to Increase sensitivity, appropriate sensitivity
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
2.1 3-1
Acute Freshwater Crustacean Bioassay: 48 Hours, ERT SOP 2024
This static toxicity test measures the survival of the freshwater crustaceans, Daphnia
Magna and Daphnia Pulex, after exposure to leachates, effluents, or liquid phases of
sediments (i.e., elutriates or pore water) for 48 hours in the laboratory.
Larval daphnids, Daphnia Magna and Daphnia Pulex, are exposed to various
concentrations of liquid-phase test media for 48 hours in 100-mL containers (or 250
ml. USEPA 1993a). The media concentrations levels intend to span a range of
those causing zero mortality to those causing com plete mortality. If the test medium
is a liquid, dilution may be made directly for the required test concentrations. If the
test medium is a sediment, preliminary filtration and dilutions are required to produce
a liquid phase that will then be diluted to attain the above test concentrations.
Once all the exposure chambers are set up with their designated test
concentrations, the test organisms are added after being acclimated to the dilution
water in separate chambers. The experiment officially begins when half of the
organisms are in the exposure chambers. Test temperature is 20.0 +/- 2 °C for the
daphnids. The test is state; water will not be renewed throughout the duration of the
test. The endpoints are survival at 1-hour, 24-hours, and 48-hours. Organisms are
not fed during the test.
At the termination of the test, mortality and water quality parameters are recorded.
Range-finding tests may be performed prior to these analyses to determine the
appropriate test media dilutions. Reference toxicant tests will also be performed
simultaneous to these tests.
The acute toxicity tests described for use in the NPDES Permits Program indicate
that this test may be static or static-renewal and it is run for 24, 48 or 96 hours
(Weber. 1991).
A similar method for acute toxicity using Daphnia spp. is described in the
Environment Canada Method EPS 1/RM/1 1 .
The results are used to determine the lethal concentration for 50% of the test
species (LCM). The Lowest Observable Effects Concentration (LOEC) and the No
Observable Effects Concentration (NOEC) are also recorded.
Both of these species of daphnids are considered sensitive benchmark species
(USEPA and USAGE 1998). Benchmark species comprise a substantal data base,
represent the sensitive range of a variety of ecosystems and provide comparative
data on the relative sensitivity of local test species.
Liquid-phase toxicity testng is often simpler to run than bulk sediment testing;
excellent correspondence between bulk sediment contaminant concentrations and
pore water toxicity has been observed.
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Fact Sheet No.
Limitations
Reference
Website
2.1.3-1 (contd.)
Daphnia are freshwater crustaceans, therefore they cannot be used in estuanne and
marine settings.
The optimum pH range for Oaphnids is 6.8 to 8 5; therefore, the pH of the dilution
water or the concentrations may have to be adjusted prior to the start of the test.
USEPA. 1994b. 48-Hour Acute Toxicity Test Using Daphnia Magna and
Daphnia Pulex, SOP #2024. Compendium of ERT Standard Operating Protocols.
Office of Solid Waste and Emergency Response, U.S. Environmental Protecton
Agency, Edison NJ.
htto //www ert ora/oroducts/2024
fidf
Last Accessed: 1/23/2003
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.3-2
Acute Freshwater Fish Bioassay, ERT SOP 2022
These methods describe a static-renewal toxicity test using the freshwater fish.
Pimephales promelas. These tests are effective when testing the acute toxicity of
effluents, leachates and liquid phases of sediments for 96 hours in the laboratory.
The larval Pimephales promelas (fathead minnow) is exposed to various
concentrations of test media over a 96-hour period in 1-L test containers. The
medium concentration level is planned to span a range of those causing zero
mortality to those causing complete mortality. If the test medium is a liquid, dilution
may be made directly for the required test concentrations. If the test medium is a
sediment, preliminary filtration and dilutions are required to produce a liquid phase
that will then be diluted to attain the above test concentrations.
The test temperature is 25 +/- 2 °C. Fish will be fed during the acclimation period
and during the toxicity test. Test solutions will be replaced daily in exposure
chambers. Record survival at one hour and then daily thereafter. After the 96 hours
has past, final mortality and water quality measurements are recorded.
Range-finding tests may be performed prior to these analyses to determine the
appropriate test media dilutions. Reference toxicant tests will also be performed
simultaneous to these tests.
The acute freshwater fish bioassay used in the NPDES permits program indicates
that this test may be static or static-renewal and run for 24, 48 or 96 hours (Weber.
1991).
The rainbow trout, Oncorhynchus mykiss, is another benchmark freshwater fish
specie used for water column toxicity tests (USEPA and USAGE. 1998).
This test may be conducted on effluents, leachates, or liquid phase of sediments.
The results will be used to determine the lethal concentration of test media that
causes 50% mortality (LCg,). The Lowest Observable Effect Concentration (LOEC)
and the No Observable Effects Concentration (NOEC) is also recorded.
Pimephales promelas are easily reared in the laboratory and they are important
forage fish in the food chain. Pimephales promelas are considered benchmark
species indicating that they comprise a substantial database, represent the sensitive
range of a variety of ecosystems, and provide comparative data on the relative
sensitivity of local test species (USEPA and USAGE, 1998).
Please note the list of general limitations for all liquid-phase toxicity tests in the
introduction to this section.
USEPA. 1994b. 96-Hour Acute Toxicity Test Using Larval Fathead Minnows
(Pimephales proomelas) SOP #2022. Environmental Response Team .
Compendium of ERT Standard Operating Protocols. Office of Solid Waste and
Emergency Response, U.S. Environmental Protector Agency, Edison NJ
http'//www ert orq/products/2022 Last Accessed: 1/23/2003
pdf
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data Uses/Application
Advantages
2.1.3-3
Chronic Freshwater Algae Test, ERT SOP 2027
This test measures the biostimulatory capabilities of leachates, effluents, or
liquid phases of sediments (i.e., elutriates or pore water) on Se/enasfru/n
capricornutum for 96-hour exposure of in the laboratory.
The freshwater algae, Selenastrum capricornutum is exposed to various
concentrations of test media over a 96-hour period in 100-mL test containers.
The media concentration levels intend to span a range of those causing zero
mortality to those causing complete mortality. If the test medium is a liquid,
dilution may be made directly for the required test concentrations. If the test
medium is a sediment, preliminary filtration and dilutions are required to
produce a liquid phase that will then be diluted to attain the above test
concentrations.
Test temperature is 25 +/- 2 " C. The endpoint is growth. There is no water
renewal throughout the test.
Growth is measured at the end of the test by cell counts, chlorophyll content or
turbidity (light absorbance). or biomass. Cell counts are determined using an
automatic particle counter or manually under a microscope. Chlorophyll content
may be measured using in-vivo or in-vitro fluorescence or in-vitro
spectrophotometry. Turbidity is measured by spectrophotometry at 750 nm.
Biomass is measured by multiplying the cell count by the mean cell volume or
by direct gravimetric dry weight analysis.
This test can also be conducted for 24-hours using 25-mL glass borosilicate
tubes with the following dilutions: 0%, 1 0%, 25%. 50% and 94% elutriate.
This test protocol is also described in EPA guidance documents for effluents
and receiving waters and assessing contaminated sediments in the Great
Lakes (Weber, 1993;USEPA, 1993a).
Environment Canada methods EPS 1/RM/25 and EPS 1/RM/37 describe
similar tests using Selenastrum capricornutum and Lemna minor.
This method was originally designed to test for eutrophication, however it has
been recommend for use in testing the toxicity of complex effluents and has
been widely used to test single chemicals.
The results of this test will be used to determine the No Observable Effect
Concentration (NOEC), Lowest Observable Effect Concentration (LOEC) and
the Chronic Value (CHV). These results will determine the long term effects of
those sediment samples on the surrounding biotoc community.
There is currently no method for exposing algae directly to whole sediments,
thus an elutriate most dosely simulates the most likely exposure conditions for
natural algal populations.
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Fact Sheet No.
Limitations
Reference
Website
2.1.3-3 (contd.)
The concentration of natural nutrients in the test media may affect the results.
This is not a benchmark test species used for toxicity testing (USEPA and
USAGE, 1998).
Please note the list of general limitations for all liquid-phase toxicity tests in the
introduction to this section.
USEPA. 1994b. 96-Hour Static Toxicity Test Using Selenastrum
caprieornutum, SOP #2027. Environmental Response Team. Compendium of
ERT Standard Operating Protocols. Office of Solid Waste and Emergency
Response, U.S Environmental Protection Agency, Edison NJ.
http //www ert ora/oroducts/2027 odf
Last Accessed: 1/23/2003
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Method Title
Purpose
Method Summary
Data Uses/Application
Advantages
Limitations
2.1.3-4
Chronic Freshwater Crustacean Bioassay (7 Day), ERT SOP 2025
These methods describe a 7-day, static-renewal toxicity test used to measure
chronic effects from liquid-phase test media on the freshwater crustacean,
Ceriodaphnia dubia.
The freshwater water flea, Ceriodaphnia dubia, are exposed to various
concentrations of test media over a 7-day period in 30m L test chambers. The
media concentration levels intend to span a range of those causing zero
mortality to those causing complete mortality. If the test medium is a liquid,
dilution may be made directly for the required test concentrations. If the test
medium is a sediment, preliminary filtration and dilutbns are required to
produce a liquid phase that will then be diluted to attain the desired test
concentrations.
Test temperature is 25 +/- 2° C. New test media concentrations are prepared
daily. The organisms are physically transferred to newly prepared exposure
chambers. Organisms are fed daily.
Survival is recorded over a 7-day period as well as the number of broods and
the brood size. The number of males surviving are counted at test termination.
Range-finding tests may be performed prior to these analyses to determine the
appropriate test media dilutions. Reference toxicant tests will also be
performed simultaneous to these tests.
Similar freshwater crustacean species such as the Daphnia magna and the
Daphnia pulex may also be used for similar assays.
The EPA guidance documents for toxicity testing of effluents and receiving
waters also describes this method (Weber. 1991), as does Environment
Canada's method EPS 1/RM/21.
The data from these tests will be used to determine the Lowest Observable
Effect Concentration (LOEC), the No Observable Effect Concentration (NOEC),
the ECjo and the chronic value of the test media.
Ceriodaphnia dubia are commonly used test species for freshwater toxicity
testing, therefore resulting data will be comparable to a large number of
previous studies.
These organisms are benchmark species Indicating that they comprise a
substantial database, represent the sensitive range of a variety of ecosystems,
and provide comparative data on the relative sensitivity of local test
species(USEPA and USACE, 1998).
Ceriodaphnia dubia are freshwater species; they can only be used when salinity
is <1 ppt.
Please note the list of general limitations for all liquid-phase toxicity tests in the
introduction to this section.
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Reference
Website
2.1 3-4 (contd )
USEPA. 2002. 7-Day Static Renewal Toxicity Test Using Ceriodaphnia dubia.
Rev1. SOP #2025, Environmental Response Team. Compendium of ERT
Standard Operating Protocols. Office of Solid Waste and Emergency
Response, U.S Environmental Protection Agency, Edison NJ.
http //www ert orq/products/2
025 odf
Last Accessed: 1/23/2003
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Method Title
Purpose
Method Summary
Data
Uses/Applicabon
Advantages
Limitations
Reference
Website
2.1.3-5
Chronic Freshwater Crustaceans Bioassay (10 days), ERT SOP 2028
These methods describe a 10-day, static renewal toxicity test used to measure
chronic effects from contaminated test media on the freshwater daphnids, Daphnia
magna or Daphnia pulex
Larval Dapnia magna or Daphnia pulex are placed in individual 100-mL containers
and exposed to different concentrations of liquid-phase test media over a 10-day
period. If the test medium is a liquid, dilution may be made directly for the required
test concentrations. If the test-medium is a sediment, preliminary filtration and
dilutions are required to produce a liquid phase that will then be diluted to attain the
desired test concentrations.
Test temperature is 25 degrees +/- 2 ° C. Test media concentrations are renewed
every other day for the duration of the test; organisms are physically transferred into
new exposure chambers. Organisms are fed every other day. The endpoints of the
test are mortality, reproduction and growth.
Ceriodaphma dubia is also recommended as a freshwater daphnid that may be
used for similar assays (USEPA and USAGE, 1998).
This test is applicable to leachates, effluents, and liquid phases of sediments. The
data from these tests will be used to determine the Lowest Observable Effect
Concentration (LOEC), the No Observable Effect Concentration (NOEC), the EC50
and the chronic value of the test media.
All three of these species of daphnids are considered sensitive benchmark species
(USEPA and USAGE 1998). Benchmark species comprise a substantial data base,
represent the sensitive range of a variety of ecosystems and provide comparative
data on the relative sensitivity of local test species.
Daphnia are freshwater crustaceans, therefore they cannot be used in estuanne and
marine settings.
The optimum pH range for daphnids is 6.8 to 8.5; therefore, the pH of the dilution
water or the concentrations may have to be adjusted prior to the start of the test.
Please note the list of general limitations for all liquid-phase toxicity tests in the
introduction to this section.
USEPA. 1994b. 10-day Chronic Toxicity Test using Daphnia Magna or Daphnia
Pulex. SOP #2028. Environmental Response Team. Compendium of ERT
Standard Operating Protocols. Office of Solid Waste and Emergency Response,
U.S. Environmental Protection Agency, Edison NJ.
http //www ert crq/products/2028 pdf Last Accessed: 1/23/2003
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Reference
Website
2.1.3-6
Chronic Freshwater Fish Btoassay, ERT SOP 2026
These methods describes a 7-day, static-renewal toxicity test using the larval
freshwater fish, Pimephales promelas
The Pimephales promelas are exposed to various concentrations of liquid-phase
test media over a 7-day period in 500 ml - 1L test containers. The media
concentration levels intend to span a range of those causing zero mortality to those
causing complete mortality. If the test medium is a liquid, dilution may be made
directly for the required test concentrations. If the test medium is a sediment,
preliminary filtration and dilutbns are required to produce a liquid phase that will then
be diluted to attain the desired test concentrations.
Test temperature is 25 +/- 2 °C. The fish are fed daily at 4 hour intervals. New
dilutbns of test media are prepared daily. The old solution is drawn out with a
siphon and the newly prepared solutions are added to each chamber. The
endpoints are survival and growth.
Range-finding tests may be performed prior to these analyses to determine the
appropriate test media dilutions. Reference toxicant tests will also be performed
simultaneous to these tests.
The rainbow trout, Oncorhynchus mykiss, is another benchmark freshwater fish
specie used for water column toxicity tests. A method for testing acute toxicity using
rainbow trout can be found in Environment Canada's method EPS 1/RM/9.
EPA guidance for toxicity testing of effluents and receiving waters also describes
this method (Weber, 1991, USEPA, 19906), as does Environment Canada's method
EPS 1/RM/22
The results of this test will be used to determine the No Observable Adverse Effect
Concentration (NOAEC), Lowest Observable Adverse Effect Concentration
(LOAEC) and the Chronic Value (CHV). These results will determine the long term
effects of those sediment samples on the surrounding biotic community.
Pimephales promelas are easily reared in the laboratory and they are important
forage fish in the food chain. Pimephales promelas are considered benchmark
species indicating that they comprise a substantial database, represent the sensitive
range of a variety of ecosystems, and provide comparative data on the relative
sensitivity of local test species (USEPA and USACE, 1998).
USEPA 2002 7-Day Static Toxicity Test Using Larval Pimephales promelas. Rev
1. SOP #2026. Environmental Response Team. Compendium of ERT Standard
Operating Protocols. Office of Solid Waste and Emergency Response, U.S.
Environmental Protection Agency, Edison NJ.
htm //www ert orq/oroducts/2026 pdf
Last Accessed: 2/12/03
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Method Title
Purpose
Method Summary
Data
Uses/ Application
Advantages
Limitations
Reference
Website
2.1.3-7
Chronic Marine Macroalgae, Champia parvula, Sexual Reproduction Test,
NHEERL-AED SOP 1.03.001
This toxicity test measures the effects of toxic substances in effluents and receiving
waters on the sexual reproduction of the marine macroalga, Champia parvula,
during a forty-eight hour exposure.
Macroalga are exposed to different concentrations of test concentrations of effluent
test medium over a 48-hour period. The selecton of the effluent test concentrations
should be based on the objectivity of the test, however the maximum effluent
concentration which can be tested is 50% and the dilution factors may range from
0.5 to 0.3.
Three test chambers are devoted to effluent treatment and three chambers are
controls. Each test chamber will be filled with 100 mL of control or treatment water
and five female branches and one male branch. The water is not renewed
throughout the test, however each chamber is hand-swirled twice a day to mix the
water column. After 48 hours, the organisms are removed and placed in recovery
bottles. Investigators then count the cystocarps under a stereomicroscope
NPDES Guidance suggest a 5-7 day test duration (Weber, 1991).
This is a laboratory test applicable to testing toxicity of effluents and receiving
waters. The results are used to determine the sexual reproduction ability of the
macroalgae exposed to different dilutions of the test medium.
This is one of few toxicity methods developed using marine plants.
The salinity of the test water must be 30 ppt +/- 2 ppt.
Please note the list of general limitations for all liquid-phase toxicity tests in the
introduction to this section.
USEPA and the Naval Construction Battalion Center. 1992. Standard Operating
Procedures and Field Methods Used for Conducting Ecological Risk Assessment
Case Studies. Technical Document 2296, Naval Command. Control and Ocean
Surveillance Center, RDT&E Division, San Diego, CA.
http //www duxbury battelle orq/compend
lum/methods/NHEERL-AED-SOP-
1 03 001 Ddf
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February 17.2003
Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.3-8
Acute Marine Crustacean Bioassay. NHEERL-AED SOP 1.03.003
This static toxicity test measures the survival of the marine crustacean, Mysidopsis
bahia, after exposure to effluents and receiving waters for 96 hours in the laboratory.
Mysids are exposed to various concentrations (minimum of 5) of effluent test
medium over a 96-hour period in 250 ml containers. The effluent concentrations
are commonly selected to approximate a geometric series (i.e., a dilution factor of
0.5). At least 20 organisms of a given species are exposed to each effluent
concentration.
Test temperature is 20 +/- 2 ° C. Organisms will be fed during the acclimation
period and during the toxicity test. Record survival at one hour and then daily
thereafter. After the 96 hours has past, final mortality and water quality
measurements are recorded.
Range-finding tests may be performed prior to these analyses to determine the
appropriate test media dilutions. Reference toxicant tests will also be performed
simultaneous to these tests.
Other mysid shrimp species used for water column bioassays include Noomysis
amencana and the Holmesimysis costata.
This test may be conducted on effluents, leachates, or liquid phase of sediments.
The results will be used to determine the lethal concentration of test media that
causes 50% mortality (LCg,).
Mysid shnmp are considered sensitive benchmark species (USEPA and USAGE,
1998). Benchmark species comprise a substantial data base, represent the
sensitive range of a variety of ecosystems and provide comparative data on the
relative sensitivity of local test species.
Mysid shrimp are near coastal species; they are used for testing in manne/estuarine
systems with salinities between 15 and 30 ppt(ASTM Standard Method E1191;
ASTM.2001b.)
Please note the list of general limitations for all liquid-phase toxicity tests in the
introduction to this section.
USEPA and the Naval Construction Battalion Center. 1992. Standard Operating
Procedures and Field Methods Used for Conducting Ecological Risk Assessment
Case Studies. Technical Document 2296, Naval Command, Control and Ocean
Surveillance Center, RDT&E Division. San Diego, CA.
http //www duxbury baBelle orq/compend Last Accessed:
lum/methods/NHEERL-AED-SOP-
1 03 003 Ddf
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.3-9
Acute Marine Fish Bioassay, NHEERL-AED SOP 1 .03.003
These methods describe a 96-hour, static renewal acute effluent toxicity test using
the marine fish species Menidia beryllina and Cyprinodon variegatus
Marine fish species, Menidia beryllina and Cyprinodon variegatus are exposed to
various concentrations (minimum of 5) of liquid-phase test media over a 96-hour
period in 250 mL containers. The test media concentrations are commonly selected
to approximate a geometric series (/ e., a dilution factor of 0.5). At least 20
organisms of a given species are exposed to each effluent concentration.
Both species are generally used in salinities greater than 25 ppt.
Test temperature is 20 +/- 2°C. Organisms will be fed during the acclimation period
and during the toxicity test. Test solutions must be replaced daily in the exposure
chambers. Survival is recorded at one hour and then daily thereafter. After the 96
hours have passed, final mortality and water quality measurements are recorded.
Range-finding tests may be performed prior to these analyses to determine the
appropriate test media dilutions. Reference toxicant tests will also be performed
simultaneous to these tests.
A similar effluent toxicity test is also described in EPA guidance pertaining to
effluents and receiving waters (Weber, 1991).
This test may be conducted on effluents, leachates, or liquid phase of sediments.
The results will be used to determine the lethal concentration of test media that
causes 50% mortality (LCW).
Both fish species are considered benchmark species indicating that they comprise a
substantial database, represent the sensitive range of a variety of ecosystems, and
provide comparative data on the relative sensitivity of local test species (USEPA and
USAGE. 1998).
Please note the list of general limitations for all liquid-phase toxicity tests in the
introduction to this section.
USEPA and the Naval Construction Battalion Center. 1992. Standard Operating
Procedures and Field Methods Used for Conducting Ecological Risk Assessment
Case Studies. Technical Document 2296, Naval Command, Control and Ocean
Surveillance Center, RDT&E Division, San Diego, CA.
http //www.duxbury.baltelle orq/compend Last Accessed:
lum/methods/NHEERL-AED-SOP-
1 03 003 Ddf
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February 17,2003
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.3-10
Chronic Estuarme Survival, Growth and Fecundity Test, NHEERL-AED SOP
1.03.005
These methods describe a toxicity test used to measure chronic effects from
effluents and receiving waters on the estuarine mysid, Mysidopsis bahia during a
seven-day, stabc-renewal exposure.
The estuarine mysid shrimp, Mysidopsis bahia, are exposed to various
concentrations of test media over a 7-day period in 200 ml glass beakers. The
media concentration levels intend to span a range of those causing zero mortality to
those causing complete mortality. 150 mL of the appropriate effluent dilution is
added to each beaker. The test can be run with smaller volumes of water as well.
(Ho, 2000).
Test temperature range is 26 - 27° C. New test media concentrations are prepared
daily. The test organisms are fed daily.
Mortality is recorded over a 7-day period. Following the test, the live animals are
examined for eggs and the sexes are determined within 12 hours of the test
termination.
Other mysid shrimp species used in simitar analyses include Neomys/s americana
and Holmesimysis costata.
A similar effluent toxicity test is also described in EPA guidance pertaining to
effluents and receiving waters (Weber, 1991)
The data from these tests will be used to determine the Lowest Observable Effect
Concentration (LOEC), the No Observable Effect Concentration (NOEC), the ECg,
and the chronic value of the test medium.
Mysidopsis bahia are benchmark species indicating that they comprise a substantial
database, represent the sensitive range of a variety of ecosystems, and provide
comparative data on the relative sensitivity of local test species (USEPA and
USAGE. 1998).
Mysidopsis bahia are near coastal species, They are used for salinities between 15
and 30 ppt (ASTM Method E1 191; ASTM. 2001 b).
Please note the list of general limitations for all liquid-phase toxicity tests in the
introduction to this section.
USEPA and the Naval Construction Battalion Center. 1992. Standard Operating
Procedures and Field Methods Used for Conducting Ecological Risk Assessment
Case Studies. Technical Document 2296, Naval Command. Control and Ocean
Surveillance Center, RDT&E Division, San Diego, CA.
hltp //www duxbury battelle org/compend Last Accessed:
lum/methods/NHEERL-AED-SOP-
1 03 005 pdf
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Method Title
Purpose
Method Summary
Data Uses/Application
Advantages
2.1.3-11
Chronic Echinoderm Fertilization Test, NHEERL-AED SOP 1.03.006
These methods describe a toxicity test used to measure chronic effects from
effluent and receiving waters to the gametes of the sea urchin, Arbacia
punctulata, during a 48 hour exposure.
Arbacia punctulata are exposed to various effluent test concentrations that
should be based on the objectves of the study. A dilution factor of 0.5 is used
with this procedure, starting with a high concentration of 70% effluent . If the
effluent is known or suspected to be highly toxic, a lower range of effluent
concentrations should be used.
Four females and four males are placed in shallow bowls, barely covering the
animals with seawater. Both females and males will be stimulated to release
their respective eggs or sperm. The egg stock and sperm are collected.
Sperm are diluted and mixed with seawater. This sperm suspension is then
distributed to vials and the number of sperm/mL are determined.
The eggs are washed, diluted and counted. The test begins when diluted
sperm are added to each test vial containing eggs and various dilutions of the
effluent. All test vials are incubated for one hour at 20 °C. The suspension is
then mixed and incubated again for 20 minutes. Fertilization is then
determined using a Sedgwick-Rafter counting chamber. Fertilization is
indicated by the presence of a fertilization membrane surrounding the egg.
Larval development may also be measured in this test. The egg suspension
is mixed and incubated for a longer period of time: 48 hours at 20 °C. At the
termination of the test, the total number of larvae and the appropriately
developed larvae are counted to determine survival and development per
treatment
A similar toxicity test is described in the EPA guidance pertaining to effluents
and receiving waters (Weber, 1991) and in Environment Canada's method
EPS 1/RM/27.
This sperm cell toxicity test determines the concentration of a test substance
that reduces fertilization of exposed gametes relative to that of the control.
This test may also be modified and used to assess pore water toxicity once
the pore water is extracted from whole sediments.
Sea urchin toxicity tests have been proven to be extremely sensitive
indications of toxicity effects. The pore water toxicity tests with gametes and
embryos of sea urchins are approximately an order -of-magnitude more
sensitive than the 10-day solid-phase test with amphipods (Carr 2001).
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Reference
Website
21.3-11(contd)
Sea urchin toxicity tests are not considered standard toxicity tests, therefore
fewer laboratories currently perform the test. Sea urchin tests have a limited
salinity regime; therefore, they will be useful for samples from a marine
environments and select estuarine environments.
Please note the list of general limitations for all liquid-phase toxicity tests in
the introduction to this section.
USEPA and the Naval Construction Battalion Center. 1992. Standard
Operating Procedures and Field Methods Used for Conducting Ecological
Risk Assessment Case Studies. Technical Document 2296. Naval
Command, Control and Ocean Surveillance Center, ROT&E Division,
San Diego, CA.
htto://www duxburv battelle orq/co
mDendium/methods/NHEERL-
AED-SOP-1 03006gdf
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Method Title
Purpose
Method Summary
Data
Uses/ Application
Advantages
Limitations
Reference
Website
2.1 3-12
Chronic Marine Fish Bioassay, NHEERL-AED SOP 1.03.004
This method describes a 7-day, static renewal chronic aqueous toxicity testing using
the marine fish species, Menidia beryllina and Cyprinodon variegatus.
The fish species, Menidia beryllina and Cyprinodon variegatus, are exposed to
various concentrations of effluent over a 7-day period in 1-L test containers. The
media concentration levels span a range of those causing zero mortality to those
causing complete mortality. To determine effluent concentrations, one of two
dilution factors is commonly used: approximately 0.3 or 0.5.
Menidia beryllina and Cyprinodon variegatus are near coastal fish and are generally
used in salinities greater than 25 ppt.
Test temperature is 25° ± 2°C. The fish are fed daily. New dilutions of test media
are prepared daily. The old solution is drawn out with a siphon and the newly
prepared solutions are added to each chamber. The endpoints are survival and
growth.
Range-finding tests may be performed prior to these analyses to determine the
appropriate test media dilutions Reference toxicant tests will also be performed
simultaneous to these tests.
NPDES Guidance also outlines a 9-day static-renewal test with Cyprinodon
variegatus to determine effluent effects on embryo larval survival and teratogenicity
(Weber, 1991).
The results of this test will be used to determine the No Observable Effect
Concentration (NOEC), Lowest Observable Effect Concentration (LOEC) and the
Chronic Value (CHV) These results will determine the long term effects of those
sediment samples on the surrounding biotic community.
Both fish species are considered benchmark species indicating that they comprise a
substantial database, represent the sensitive range of a variety of ecosystems, and
provide comparative data on the relative sensitivity of local test species (US EPA and
USAGE, 1998).
Please note the list of general limitations for all liquid-phase toxicity tests in the
introduction to this section.
USEPA and the Naval Construction Battalion Center. 1992. Standard Operating
Procedures and Field Methods Used for Conducting Ecological Risk Assessment
Case Studies. Technical Document 2296, Naval Command, Control and Ocean
Surveillance Center, RDT&E Division, San Diego, CA.
http //www.duxbury battelle org/compend Last Accessed:
mm/methods/NHEERL-AED-SOP-
1 03 004 pdf
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.3-13
Toxicity Evaluations of Photomduction of Polycyc lie Aromatic Hydrocarbons (PAH):
In Situ Analysis
This method was designed to evaluate the degree of photoinduced toxicity during
wet-weather events via in situ experiments.
In situ chambers are constructed with two long rectangular windows to albw water
flow (holding 200 ml of water) and UV exposure (about 70% UV penetration) to
organisms inside the chambers. Chambers containing Ceriodaphma dubia are
placed on the sediment surface in the shade or in the sunlight (four replicates each)
at both a reference site and a test site. Dark mesh screens are placed over
chambers on the shaded devices to further block out UV wavelengths.
The chambers are retrieved 48-hours after being placed in the river. At test
termination, the chambers are placed in coolers with site water and transported to
the laboratory. Percent survival is determined within 6 hours of chamber collection.
Water quality analysis is conducted at both the reference site and the test sites.
Ultraviolet measurements are made at the surface and the bottom of the river.
Water is collected also at the surface and the bottom in 1-L amber polyethylene
sample bottles for PAH analysis.
Similar freshwater crustacean species such as Daphnia magna and Daphnia pulex
may also be used for similar assays.
The results of this in situ evaluation are analyzed to determine the acute toxicity of
photoinduced PAHs. In particular, these tests are helpful in determine whether PAH
effects are more prevalent after major storm events m both agricultural and urban
environments.
In situ toxicity testing reduces sampling and laboratory-related errors from the
assessment process. Fluctuating field conditions that may affect organism
response cannot be mimicked in the laboratory.
These organisms are benchmark species indicating that they comprise a substantial
database, represent the sensitive range of a variety of ecosystems, and provide
comparative data on the relative sensitivity of local test species (USEPA and
USAGE. 1998)
Please note the list of general limitations for all liquid-phase toxicity tests in the
introduction to this section.
Ireland, D.S., Burton, G.A. and G.G. Hess. 1996. In Situ Toxicity Evaluations of
Turbidity and Photoinductron of Polycyhc Aromatic Hydrocarbons. Environmental
Toxicology and Chemistry. Vol. 15: 4.
p 574-581.
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Method Title
Purpose
Method Summary
Data
Uses/ Application
Advantages
Limitations
Reference
Website
2.1.3-14
Toxicity Evaluations of Photoinduction of Polycychc Aromatic Hydrocarbons:
Laboratory Analysis of Storm water
This method was designed to evaluate the degree of photoinduced toxicity during wet-
weather events with in situ toxicity testing.
Storm water runoff samples are collected in the field, returned to the laboratory and
fractionated to measure toxicity. After an increase in toxicity is observed in the
presence of UV radiation, a modified Toxicity Identification Evaluation procedure is
performed via the following protocol (no standard protocol exists for a TIE with Storm
water).
Suspended solids are removed using glass fiber filters and the runoff is also filtered
through B and J Solid Phase Extraction™ to remove all organics. With some
modifications, the 7-day Ceriodaphnia dubia chronic toxicity test follows the U.S.
Environmental Protection Agency's standard methods.
In each 30 mL beaker, 25 mL of sample is placed in various dilutions intended to span
a range of those causing zero mortality to those causing complete mortality. One
organism is placed in each chamber. Water is renewed on days 3, 5. and 7.
Organisms are fed daily.
These tests are conducted in the presence of UV radiation. Lamps are constructed to
emit amounts of visible and UV radiation, by using two cool-white fluorescent lamps: a
350-nm and a 300-nm photreactor lamp. Survival, reproduction and PAH
concentrations are determined at the end of the 7-day test period.
The results of this evaluation are analyzed to determine the acute toxicity of
photoinduced PAHS. In particular, these tests are helpful in determine whether PAH
effects are more prevalent after major storm events in both agricultural and urban
environments.
Laboratory tests, in comparison with in situ tests, can control other parameters such
as temperature, pH etc in order to isolate effects as a result of contaminant levels.
These organisms are benchmark species indicating that they comprise a substantal
database, represent the sensitive range of a variety of ecosystems, and provide
comparative data on the relative sensitivity of local test species (USEPA and USAGE,
1998).
Please note the list of general limitations for all liquid-phase toxicity tests in the
introduction to this section.
Ireland, D.S., Burton, G.A. and G.G. Hess. 1996. In Situ Toxicity Evaluations of
Turbidity and Photoinduction of Polycylic Aromatic Hydrocarbons. Environmental
Toxicology and Chemistry. Vol. 15: 4.
p 574-581.
N/A Last Accessed:
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2.1.3-15
Method Title
Growth and Scope for Growth Measurements with Mytilus edu/is, NHEERL-AED
SOP 1.03.013
Purpose
This method describes a test used to determine growth and the scope for growth
(SFG) index using the blue mussel, Mytilus edutis. To derive the SFG index, the
test measures, the mussel's clearance rate, respiration rate and assimilation
efficiency throughout the procedure.
Method Summary
Mussels collected in different field conditions are sorted by size and placed in
individual clearance rate chambers. In these chambers, they are allowed to feed
overnight on algae pumping through the system at a set concentration. A Coulter
Counter is used to measure particles in order to determine the clearance rate.
The mussels are moved from the clearance rate chambers to chambers where
respiration measurement tools are set up. The respiration rate is measured in these
chambers with a radiometer and 450 ml glass respirometer vessels, which are
placed in the chambers with the individual mussels.
Assimilation efficiency is measured in the clearance rate chambers after the
chambers have been cleaned of fecal and algal matter and the mussels have feed
overnight. Fecal pellets are collected to determine the dry weight and ash weight of
feces. A similar procedure is completed with the cultured algae to obtain the dry
weight and ash weight of the food.
Mussel growth from pre exposure to post exposure is also determined using a
vernier caliper. Lastly, the mussel tissues are excised, dried and weighed.
Data
Uses/Application
The above method measures the following three physiological parameters in
mussels collected from different field conditions: clearance rate, respiration rate and
food assimilation efficiency. Clearance rate and assimilation efficiency
measurements are used to determine total amount of energy available, while
respiration rate is used to estimate metabolic energy costs.
These data are used to calculate the SFG index, which is a measure of the energy
available to an organism for somatic and reproductive growth after accounting for
routine metabolic costs. Mussels of similar physiological condition should
demonstrate similar SFG responses under standardized conditions; therefore,
differences in SFG are attributed to persistent physiological effects of field exposure.
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Advantages
Limitations
Reference
Website
2.1.3-15(contd.)
Investigators have found reduced growth and ultimately reduced fecundity and
fitness in Mytilus edulis after sustained reduction in SFG. The SFG index, therefore,
provides an additional way in which to quantify potential chronic effects from
changes in field conditions.
Mytilus edulis can withstand salinities ranging from 1 ppt to > 25 ppt. Mytilis is also
considered a benchmark species indicating that they comprise a substantial
database, represent the sensitive range of a variety of ecosystems, and provide
comparative data on the relative sensitivity of local test species (USEPA and
USAGE, 1998).
Please note the list of general limitations for all liquid-phase toxicity tests in the
introduction to this section.
USEPA and the Naval Construction Battalion Center. 1992. Standard Operating
Procedures and Field Methods Used for Conducting Ecological Risk Assessment
Case Studies. Technical Document 2296, Naval Command, Control and Ocean
Surveillance Center, RDT&E Division, San Diego, CA.
htto //www duxburv battelle orq/compend Last Accessed:
mm/methods/NHEERL-AED-SOP-
1 03013odf
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.1.3-16
Microtox® tests. NHEERL-AED SOP 1.03 009
This method determines acute toxicity in effluents, receiving waters and elutriates
through use of a bioluminescent bacteria. These tests are also applicable to whole-
phase sediment samples.
Microtox® tests measure acute toxic effects in'lummescent bacteria
(Photobacterium phosporeum) after exposure to effluents, receiving waters or
elutriate samples (aqueous phase of a 4:1 water to sediment mixture). Metabolic
inhibition in the luminescent organisms occurs if a sample is toxic, and the
subsequent reductions in light output are used to derive a dose-response curve from
which the effective concentration of the sample is determined.
Water samples are evaluated at 45, 22.5, 1 1 .3, and 5.6 % dilutions of the full-
strength samples. The Microtox® reagent (Photobacterium phosphreum) are
placed in the Microtox® turrets to measure initial light levels. The reagent is then
added to the respective dilutions Generally, the reagent reacts quickly to organic
compounds and toxicity is elicited within 5 minutes Metals take longer to elicit
toxicity; up to 15 minutes should be allowed. After a set exposure time, the reagent
and dilution are placed in a turret of the Microtox machine and the light levels are
recorded. The Microtox® test is also conducted with undiluted samples (e.g. 100%
test media).
Microtox® tests can be used to determine if the toxicity of liquid or solid phase
samples extracted from a contaminated environment. They can either be used
alone or in concert with other analyses screening samples as a preliminary step to
identifying potential contamination.
Microtox® tests are much quicker than traditional toxicity tests and they may be
performed in a field laboratory. They can be performed with liquid phase samples
from both freshwater and marine environments.
The apparent toxicity of elutriates can be a function of extraction solvent and overall
procedure.
Bacteria response to potential toxicity in water or sediment may not be
representative of the response of a larger organism encountering the same medium
in the wild.
USEPA. 1993a. Biological and Chemical Assessment of Contaminated Great
Lakes Sediment, EPA 905-R93-006. Great Lakes National Program Office, U.S.
Environmental Protection Agency, Chicago, IL.
http-//www duxburv battelle ora/compendium/met Last Accessed:
hods/NHEERL-AED-SOP-1 03 009 Ddf
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Fact Sheet No.
2.1.3-17
Method Title
Comparative Toxicity of 2,3,7,8-Tetrachlorodibenzo-p-Dioxin to Seven
Freshwater Fish Species During Early Life-Stage Development
Purpose
To determine and compare the toxicity of 2,3,7,8-Tetrachbrodibenzo-p-Dioxin
(TCDD) to early life stages of freshwater fish on the basis of waterborne
exposure of fertilized eggs.
Method Summary
Fish species suitable for this method include northern pike, white sucker, lake
herring, fathead minnow, channel catfish, medeka, and zebrafish. Eggs are
obtained by stripping the adult fish and artificially fertilizing the eggs in clean
water. The exposure system consists of three tanks, one egg control tank, one
solvent control tank and one test egg tank. Solvent and TCDD are added to the
tanks (minus the control tank) 30 minutes prior to the start of each egg
exposure. The recirculating flow rate in the tanks is adjusted to approximately
80 m Urn in for all tests. Eggs are checked for fungus daily during the mcubaton
period and dead eggs are removed and recorded. Following the hatch, all
organisms are released into clean-water tanks and observed daily for signs of
TCDD toxicity, which include edema, hemorrhaging, head and spinal
deformites, lethargy, loss of equilibrium, skin discoloration, and mortality.
The concentrations of TCDD in the test tanks are also measured and recorded.
GC/MS analysis is used to determine the spercific activity and radiopurity of
TCDD concentrations at the beginning and end of each exposure.
A similar method for early life-stage toxicity testng is described in Environment
Canada Method EPS 1/RM/28,1* and 2nd editions. Available from
Environmental Protection Publications, Environmental Protection Service,
Environment Canada. Ottawa, Ontario. K1A OH3, Canada.
Data Uses/Application
TCDD is the most toxic of the hydrophobia, halogenated aromatic comounds
that include polychlorinated dibenzodioxins (PCDDs), dibenzofurans(PCDFs),
and polychlorinated biphenyls (PCBs). In addition, the toxic effects of TCDD
are bioaccumulatable in aquatic systems Because of its association with
aquatic sediments, TCDD poses a potential risk to aquatic organisms. This
method describes the determination of toxicity in the early-life stages of several
fish species.
Advantages
For many fish species, the toxicity of TCDD is increased when the eggs are
exposed prior to the hatch. The mechanism involved in TCDD uptake is known
to be extremely functbnal in the very early life stages of fish and results of
toxicity (other than mortality) are measurable in the post-hatch populaton.
Limitations
Comparisons of TCDD toxicity using this method to previously tested fish
species are difficult because test conditions (exposure regimes and life stages)
may vary so much. Also, within a fish species, sensitivity to TCDD is dependant
on the age and size of the organism, and the exposure time and stage of
development.
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Reference
Website
2.1. 3-17 (cont'd)
Elonen. Gregory E., RL Spehar, GW Holcombe, RD Johnson, JD Fernandez,
RJ Erickson, JE Tietge, and PM Cook. 1998. Comparative Toxicity of 2,3,7,8-
Tetrachlorodibenzo-p-Dioxin to Seven Freshwater Fish Species During Early
Life-Stage Development. Environmental Toxicolgy and Chemistry, Vol. 17, No.
3, pp 472-483.
N/A
Last Accessed:
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2.2 Sediments
Sediment samples are collected at Superfund sites with the same objectives in mind as when
collecting water samples. These objectives, as stated in Section 2.1, are the following:
• To determine if the contaminant is hazardous by identifying its composition and
characteristics;
• To determine if there is an imminent or substantial threat to public health or welfare or
to the environment;
• To determine the need for long-term action;
• To develop containment and control strategies;
• To evaluate appropriate disposal/treatment options; and,
• To verify treatment goals or clean up levels (USEPA, 1994a).
To adequately characterize a site, the plans for sediment sampling and related analyses must be
developed in consideration of the site characteristics. Therefore, the following fact sheets relating
to sediment are divided into sections pertaining to field sample collection and processing,
chemical and physical analyses, and biological analyses. These fact sheets intend to provide
Superfund managers with a summary of the existing methods that may be applicable to their site,
the method's relative strengths, and the method's relative weaknesses.
2.2.1 Field Sample Collection and Processing, In Situ Data Acquisition
Section 2.2.1 provide field sample collection and processing methods for sediments. Sediments
are collected at Superfund sites for sediment chemistry, toxicity and benthic community analyses
to determine the extent of chemical contamination and impact of contamination on the site. The
two primary methods for sediment collection include sediment grab samplers and sediment core
samplers. However, there are quite a few different types of grabs and cores. These different
samplers are summarized following their respective fact sheets in Tables 2.2.1-1 and 2.2.1-2.
Other sediment and processing collection methods are also provided for situations where grab
and core deployment is un necessary or impossible due to physical interferences. These sample
collection methods were gathered from the following information sources:
The USEPA's Office of Water
The USEPA's Office of Research and Development
ASTM
Standard Methods for Examination of Water and Wastewater, 1999
Puget Sound Water Quality Action Team
The USEPA's Coastal EMAP Program
The USEPA's Great Lakes Program Office
Field observations and preliminary identification of sediment type are pertinent to all
sediment collections. Guidelines for making visual observations of sediment type can be
found in the US Army Corps of Engineers manual on Soil Sampling, EM 1110-1-1906.
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Applicaton
Advantages
2.2.1-1
Grab Sampling
To collect samples of the benthos for quantitative or qualitative sampling
procedures, intended to determine sediment chemistry, toxicity and/or benthic
community composition and abundance.
Grabs are to be lowered slowly from a boat or by ha'nd into the water column.
When most grabs reach the bottom their weight will cause them to penetrate the
substrate (areas of 0.02 to 0.5 m2 and depths ranging from 5 to 15 cm). The
slack on the cable allows the locking lever to release, therefore permitting the
movement that allows the horizontal locking bar to drop out of the locking notch
and allow the jaws to close as the device is raised. Other grabs are closed by
spring action or some other mechanical device after penetrating the substrate.
After the grabs are brought to the surface, they are examined for acceptability.
Collection of undisturbed sediment requires that the sampler :
-create a minimal pressure wave when descending
-form a leakproof seal when the sediment sample is taken
-prevent winnowing and excessive sample disturbance when ascending
-allow easy access to the sample surface in order that undisturbed subsamples
may be taken (USEPA, 1992c).
The required amount of sediment is removed for sub-sampling and placed in the
appropriately cleaned sample containers. (See Fact Sheet 2.2.1-8.)
Other USEPA, ASTM and APHA documents provide grab sample collection
information and details pertaining to different grab samplers (USEPA, 1992c;
ASTM Method E1391 (ASTM 2001b); Standard Method 10500 (APHA 1999).
There are many types of grabs that vary in penetration depth, surface area
sample and sampling various substrate types. The various grabs and their
respective advantages and disadvantages are detailed on the following matrix
(Table 2.2.1-1).
Grab sampling devices collect sediments that may be used to analyze for
sediment chemistry, sediment toxicity. and/or the samples may be sieved to
determine benthic community composition and abundance. They are commonly
used in estuanne and marine monitoring programs due to their ability to provide
reliable quantitative data at a relatively low cost
Since there are many types of grabs, it is easy to find one that will be effective in
various site conditions (Table 2.2.1-1). Grabs are able to sample a larger surface
area than most coring devices.
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Limitations
Reference
Website
2.2.1-1 (contd.)
Grabs have a relatively shallow and variable depth of penetration depending on
the sediment properties. As the grab sampler bites into the sediment, the
sediment is inevitably folded resulting in the loss of information concerning the
vertical structure of sediments.
The shock wave that results from the grab's deployment also results in a loss of
the fine surface sediments and water-soluble compounds and volatile organic
compounds present on the surface of the sediment.
USEPA. 1990b. Macroinvertebrate Field and Laboratory Methods for Evaluating
the Biological Integrity of Surface Waters. EPA/600/4-90/030. Office of Research
and Development, U.S. Environmental Protection Agency, Washington, D.C.
http //www eoa cov/bioiweb1/Ddf/benthos
methods ch5 odf
Last Accessed: 1/28/2003
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Table 2.2.1 -1 . A Summary of Sediment Grab Devices (USEPA. 1992c; APHA, 1999; USEPA. 1990b; Murdoch and Azcue,
1995)
Sediment Grab
Van Veen
Young Grab
(fluoro carbon
plastic or kynar
lined modified
0.1 m1 van
veen)
Orange Peel
Smith Nlclntyre
Shlpek
Peterson
Habitat
Open sea and
large lakes
Lakes and
marine areas
Marine
environments
and deep lakes
Marine,
estuarine,
adaptable to
large rivers,
lakes and
reservoirs
Used pnmanly
in marine
waters and
large inland
lakes and
reservoirs
Freshwater
lakes.
reservoirs,
nversand
estuanes
Substrate Type, Surface
Area ana reneirauon
Depth
Sand, silt, day or similar
substrates
Surface Area 0.25m1
Penetration Depth: 5-7 cm
Sand, silt, day or similar
substrates
Surface Area. 1 m1
Sandy substrates
Round grab, collects up to
1600 cm* of sediment
Used on most substrates,
designed specifically to
sample hard substrates
Surface Area 0 2 or 0 1m3
Sand, gravel, mud and clay
Surface Area. 0 4m*
Penetration Depth 10cm
Useful on most substrates;
especially hard substrates
with swift currents and
deep water
Advantages
This grab can sample
most sediment types.
Large enough to permit
sub-sampling.
Lined grabs eliminate
metal contamination
Small size reduces
pressure wave
Comes m a range of
sizes, works in deep
water, closes relatively
well to prevent sample
loss, good for
reconnaissance.
This grab is stable and
easy to control in rough
water.
This grab is good for
collecting a small sample
in deep water It has a
sample bucket from which
a sub-sample may be
obtained. It retains fine-
grained sediments
effectively
This grab can obtain a
large sample and it can
penetrate most substrate.
Disadvantages
Shock wave from descent
may disturb "fines ' Possible
incomplete closure of jaws
results in sample loss.
Possible contamination from
metal frame construction.
Sample must be further
prepared for analysis
Expensive, requires winch
Very heavy, requires power
winch. Does not sample
constant area and depth.
Loss of fines Possible
contamination from metal
frame construction Very
heavy, requires a power
winch
Possible contamination from
metal frame construction
Very heavy, requires a power
winch.
Heavy, may require winch
No cover lid to permit
subsamphng. All other
disadvantages of Ekman and
Ponar.
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Table 2.2.1-1. (contd.)
Petite Ponar
Ponar
Ekman or Box
Dredge
Deep nvers,
lakes and
reservoirs
Deep nvers,
lakes and
reservoirs
Can be used
from boat,
bridge, or pier
in waters of
various depths
Moderately hard
sediments, such as sand,
silt and mud
Surface Area. 02m2
Fine to coarse textured
sediments such as day,
hard pan, sand, gravel and
muck. Less effective in
softer sediments.
Surface Area- 05m2
Consolidated, fine textured
sediments Efficient in soft
sediments, such as silt,
muck and sludge in water
with little current.
Surface Area: .05 m2
This grab has a good
penetration for a small
grab, side plates and
screens to prevent
washout, and it can be
operated by hand without
a boat or a winch
This grab is very efficient
for hard sediments;
considered universal
sampler due to ability to
collect adequate samples
from most substrate
types.
This grab is light weight, it
can be operated by hand
It is commonly used for
benthic evaluations.
Obtains a larger sample
than coring tubes. Can be
subsampled through box
hd.
It is not effective for sampling
deep burrowing organisms or
for sampling day substrate.
Shock wave from descent
may disturb "fines." Possible
incomplete closure of jaws
results in sample loss.
Possible contamination from
metal frame construction
Sample must be further
prepared for analysis
Shock wave from descent
may disturb "fines.* Possible
incomplete closure of jaws
results in sample loss.
Possible contamination from
metal frame construction.
Sample must be further
prepared for analysis Difficult
to use in rocky or sandy
bottoms
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Fact Sheet No.
2.2.1-2
Method Title
Core Samplers
Purpose
To collect an undisturbed sediment sample from varying depths in any
substrate.
Method Summary
Prior to deployment, the sampling device is inspected to see that the sediment
retainer behind the cutting edge will provide a good seal. For a box corer, the
cable must feed through the pulley system properly and the spade must rotate
freely. All portions of the sampling device that will be in contact with the sample
(i.e, the core tube and the core liner, where applicable) should be constructed
of noncontammating material.
Cores are deployed from a suitable vessel. Cores use either inertia (i.e.,
gravity cores, piston cores) or mechanical motion (hammering or vibration) as
the primary driving force to achieve the desired penetration depth depending
on the specified depth and the sediment properties.
The amount of pull that is required to extract a core tube from the substrate
depends on the specific gravity of the device and its contents, plus the amount
of frictional force against the surface of the core tube walls that must be
overcome. During the extraction, the wire strain should be steady and
continuous; the vessel should be held stationary directly above the coring
device. Once clear of the bottom, winch take-up speed may increase.
Once the sampling device is onboard the vessel, one or both ends of the core
tube is capped if possible. Overlying water is siphoned off at the top of the
core tube (after allowing for settling time). The length of the sediment core
should be determined by comparing measurements of the length of the core
material against the overall penetration depth. The ratio of penetration depth
to core material length is calculated to determine the compaction of the
sediment during coring.
If the core is acceptable (for example, acceptable depth of penetration, surface
layer intact), the core tube (or liner) should be labeled with the core
identification number, collection date, core orientation, and length of core
material collected. Until the core sample can be extruded or split into sections,
the core tube should be secured in an upright position, taking care not to avert
the core. Cores should be split within 24 hours of collection.
Other US EPA, ASTM and APHA method documents provide specifics
regarding core sampling and determining what type of core device is
applicable (USEPA, 1990b; ASTM Method E1391(ASTM 2001 b; Standard
Method 10500 (APHA, 1999).
There are also several types of cores; these cores and their respective
advantages and disadvantages are detailed on the following table (Table 2.2.1-
2).
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Data Uses/ Application
Advantages
Limitations
Reference
Website
2.2.1-2(contd.)
Core samples can be analyzed for sediment chemistry, sediment toxicity
and/or benthic community analyses.
Core sampling removes sediments with less disnjptbn than grab and dredge
sampling. Gravity corers or hand-driven corers can collect sediments up to 1
to 2 m in depth. When vibratory corers or others using hydralics for sediment
penetration, corers can collect sediments up to 10 m in depth. Corers are
more efficient than grabs. Corers are the most accurate samplers of benthic
macroinvertebrate populations.
Core sampling provides an imprecise estimate of the standing crop of
macrobenthos, because of the small area sampled. Gravity operated samples
have limited surface area, and they require a boat and powered winch. Cores
generally sample an area 13 to 26 cm2.
Cores are more difficult to handle than grabs in rough water. They do not work
well in sandy sediments.
PSWQAT. 1997. Recommended Guidelines for Sampling Marine Sediment,
Water Column, and Tissue in Puget Sound, Puget Sound Protocols and
Guidelines. Puget Sound Water Quality Acton Team, Olympia.WA.
httD.//www.osat wa aov/Publications/
protocols/protocol odfs/field odf
Last Accessed: 1/28/2003
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Table 2J.1-2. A Summary of Sediment Coring Devices (USER A, 1992c;APHA, 1999;USEPA, 1990b; Murdoch and
Azcue,1995)
Sediment Con
Fluorocarbon
plastic or Glass
tube
Hand Corer
Push Core
Phleger Core
{Gravity Core)
KB Core
(Gravity Core)
Box Core
(Gravity Core)
Core liner
diameter
Penetration
Depth
Core diameter
Varies
Penetration
Depth- Up to 50
cm
Core diameter
3.5 to 7.5 cm ID
Penetration
Depth. 50 to
120cm
Vanes
Core diameter
3 5 cm ID
Penetration
Depth- Up to 50
cm
Core diameter
3 5 cm ID and 5
cm
Penetration
Depth: Up to 70
cm
Surface area:
typically 004
and 0.1 ctt
Penetration
Depth. Up to
1m
Substrate Type;
Habitat
Shallow
wadeable waters
or deep waters if
SCUBA
available
Soft or semi-
compacted
sediment in
shallow
wadeable
waters, deep
waters if SCUBA
available
Soft or semi-
compacted
sediment in
shallow water
Soft substrates.
semi-compacted
substrates, peat
and vegetated
roots in shallow
lakes and
marshes
Soft, fine-grained
substrates
Soft sediments
Advantages
Preserves layering and permits
historical study of sediment
deposition. Minimal risk of
contamination
Handles provide for greater ease
of substrate penetration.
Preserves layenng and permits
historical study of sediment
deposition. Minimal nsk of
contamination.
Push cores with shallow
penetration and in relatively
shallow water'do not require a
winch.
There is low risk of undisturbed
sample contamination This
sampler maintains sample
integrity relatively well It does
not require a winch
Useful for obtaining estimates of
the standing crop of
macrobenthos in soft substrates.
Winch is not required
This core samples the same
surface area as a grab, but it
disturbs the surface less Allows
forsubsamplmg
Disadvantages
Small sample size requires
repetitive sampling
Small sample size requires
repetitive sampling, Careful
handling necessary to prevent
spillage. Requires removal of
liners before repetitive sampling
Slight nsk of metal
contamination from barrel and
core cutter.
They are difficult to deploy in
areas with strong currents and
deep water. They may be
difficult to retneve if the
penetration depth exceeds 50
cm.
Careful handling is necessary to
avoid sediment spillage Small
sample, requires repetitive
operation and removal of liners
Time consuming
The messenger system used to
dose the core is sometimes
ineffective when the core does
not penetrate the sediment
vertically
This core does not penetrate
sediments deeply Hard to
handle, very heavy
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Table 25.1-2. (contd.)
Benthos Gravity
Core
Alpine Gravity
Core
Multi-Gravity
Core
Piston Core
Vlbratory-
Hammer Core
Core diameter
6.6 cm and 7.1
cm
Penetration
Depth: Up to
3m
Core diameter
35cm
Penetration
depth: 0.6, 1.2
and 1.8m
Core diameter
and penetration
depth vary.
Core diameter
typically 3. 5. or
6-
Penetration
depth: 3-20
meters
Core diameter.
typically 3, 5, or
6"
Soft, fine-grained
substrates
Compacted
substrates from
depth
Vanes
Soft substrates
All types
It has stabilizing fins that
promote vertical penetration. It
also has a valve system that
prevents sample loss It can
sample substrates from great
depths.
It can sample substrates from
great depths.
Multiple samples can be taken
from one site for comparative
studies, evaluation of sediment
samples and determination of
sediment heterogeneity over a
small area.
This core can be used for
samples requiring significant
penetration depths Relatively
undisturbed samples
This core can be used In all
types of sediments. Method of
choice for many environmental
dredging studies
More difficult to deploy and
retrieve, large device, very
heavy.
Lack of stabilizing fins makes
vertical penetration difficult This
core also disturbs surface
sediments significantly. Very
heavy.
Large and difficult to deploy and
retrieve.
A heavy crane is needed with
lifting capacity over 2000kg to
deploy and retrieve piston cores.
This device is not suitable for
sediment profiles since it
disturbs the top layer.
Large and difficult to deploy and
retrieve
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.2.1-3
Hand Collection
This method describes how sediment samples can be collected by hand in the
intertidal zone with a favorable tide.
Sediment samples may be collected by hand with a variety of sampling implements
such as spoons or trowels for surface sediments, or with hand augers or corers for
collecting sediments at discrete depths. Any sampling implement that comes in
contact with the sample should be constructed of stainless steel or Teflon™. If
individual sample collection kits are not available for each sampling location,
sampling equipment should be thoroughly decontaminated between stations by
scrubbing with a phosphate-free detergent soluton, followed with a thorough rinse
with analyte-free water. If heavy contamination by metals or organic contaminants is
expected at the site, sampling equipment may be rinsed with methanol, acetone or a
50.50 acetone/hexane mix for organics or 10% HNOS for metals.
Once the samples have been collected with one of the aforementioned tools, the
samples should be homogenized in a stainless steel bowl with a stainless steel or
Teflon™ spoon or spatula. Sample aliquots are transferred to appropriate laboratory
supplied containers and preserved as required.
These methods are used in shallow waters where a core is not needed Sediment
samples can be analyzed for sediment chemistry, sediment toxicity and/or benthic
community analyses.
Hand collection is less expensive and labor intensive than other sediment collection
techniques.
Sediments can only be collected by hand in shallow waters or locatons where the
tide has exposed the desired sampling area. This collection procedure also
increases human exposure to potential contaminants present in the samples.
PSWQAT. 1997 Recommended Guidelines for Sampling Marine Sediment, Water
Column, and Tissue in Puget Sound, Puget Sound Protocols and Guidelines. Puget
Sound Water Quality Action Team, Olympia, WA.
http //www psat wa gov/Publications/pro Last Accessed' 1/28/2003
tocols/protocol Ddfsflield odf
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2.2 1-4
Hand Collection at Depth with SCUBA Equipment
To sample benthos in locations where conventional sampling devices are not
practical and the water depth is too deep for hand-collection.
The collection of sediment samples by a diver should be considered when
undisturbed samples are required, particularly for studies of the sediment-water
interface. SCUBA certified professionals can conduct the following types of benthos
sampling: placement and retrieval of artificial substrate; use of suction samplers;
sampling with a quadrate frame; and , perhaps most importantly, identifying and
delineating substrate types for purposes of determining sampling effort (stratified
sampling) and choice of samplers.
SCUBA divers can use traditional sediment collection devices that are then analyzed
for sediment chemistry, sediment toxicity, and/or the samples may be sieved to
determine benthic community composition and abundance.
Allows for benthic sampling in locations that are inaccessible by conventional grab
sampling. Allows for more precise sampling of the sediment-water interface.
Requires certified SCUBA divers who will comply with rigid safety standards.
Somewhat expensive. The diver's visibility can be obscured if fine-grained
sediments are disturbed or if the water is turbid.
USEPA. 1990b. Macroinvertebrate Field and Laboratory Methods for Evaluating
the Biological Integrity of Surface Waters. EPA/600/4-90/030. Office of Research
and Development, U.S. Environmental Protection Agency, Washington, D.C.
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2.2.1-5
Sediment Traps
Sediment traps collect settling partrculate matter (SPM) which provides useful data
for studies of sedimentation rates and resuspension of bottom sediments.
If collecting SPM for chemical analysis, the traps should be cleaned with a
phosphate-free detergent solution, then sequentially rinsed with hoi water, 10
percent HNO3, analyte-free, pesticide grade acetone, and finally, wrapped in
aluminum foil until deployment in the field. If the sediment trap is constructed of
plexiglass, the acetone rinse should be avoided as acetone will damage the
plexiglass. Prior to deployment, the traps should be filled with two liters of high-
salinity, analyte-free water containing a preservative to reduce microbial degradabon
of the samples during deployment period.
SPM samples are collected by retrieving the traps and removing the overlying water
in the collection cylinders using a peristalic pump. The water immediately overlying
the trapped sediment is analyzed to determine the salinity and the presence of
preservative to determine if the trap was disturbed during the deployment. The SPM
is then transferred to sample containers and taken to an analytical laboratory for
processing. The paniculate fraction of the SPM is removed by centrifuge and split
into sample aliquots for chemical analysis.
Sediment trap designs vary. The trap must be made suitable for the study area.
Considerations on biofouling must be addressed and controlled appropriately with
regard to the type of samples being collected.
SPM data are used for studies of sedimentation rates and for sediment transport
studies.
Sediment traps can collect relatively large volumes of suspended matter for
transport studies (compared to filtration)
Construcbon, deployment, and retrieval often require resources beyond typical field
studies. Biological invasions of traps typically occur. Controlling agents are not
suitable for all applications.
PSWQAT. 1997. Recommended Guidelines for Sampling Marine Sediment, Water
Column, and Tissue in Puget Sound, Puget Sound Protocols and Guidelines.
Puget Sound Water Quality Action Team, Olympia, WA.
http //www psat wa gov/Publications/pro Last Accessed- 1/28/2003
tocols/orotocol odfs/field odf
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2.2.1-6
Russian Peat Borer
To collect discrete, relatively uncompressed sediment samples.
The Russian Peat Borer is a manually driven, chambered-type, side-filling core
sampler, and its components include a stainless-steel core tube, aluminum
extension rods, a stainless-steel turning handle, and a Delrin ® core head and
bottom point that support a stainless-steel cover plate.
To collect a sediment sample, the bottom point of the Russian Peat Borer is
manually inserted into sediment, with the blunt edge of the core tube turned against
the cover plate to prevent sediment from entering the tube during penetration. A
slide-hammer mechanism can be used to drive the sampler through highly
consolidated sediment or peat that is hard to penetrate. Once the sampler is driven
into the sediment to the desired depth, the core tube is turned 180 degrees
clockwise. This allows the core tube to rotate and its sharp edge to longitudinally cut
through the sediment, collecting a semicylindrical sediment core. While the core
tube is manually turned, the stainless-steel cover plate provides support so that the
collected material is retained in the core tube. The sampler is then rotated and
placed on the sampling platform in such a way that the core tube is above the cover
plate. The core tube is then manually turned counterclockwise, rotating the tube and
exposing the semicylindrical core sample on the cover plate.
The sampler can collect discrete, relatively uncompresssed core samples from
shallow to deep depth intervals with out disturbing the sediment stratification.
The sampler is lightweight and easy to operate, requiring minimal training and skill.
It does not require disassembly to extrude the sample. It requires no support
equipment other than two sawhorses for support during sample extrusion.
For deployment in deep water applcations, the sampler requires extension rods.
This sampler is not equipped with disposable core liners. During deployment, the
cover plate is exposed to different layers of sediment. Also, partially decomposed
plant matter or small stones may cause the core tube to remain in the open position
during sampling retrieval. To use this sampler, sediment must offer enough support
to keep the cover plate stationary and allow rotation of the tube core.
USEPA. 1999d. Innovative Technology Verification Report: Aquatic Research
Instruments Russian Peat Borer, EPA/600/R-01/010. Office of Research and
Development, U.S. Environmental Protection Agency, Washington, DC.
http//www epa gov/ordntmt/ORD/SITE/r
eDorts/600r01010.htm
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2.2.1-7
Split Core Sampler for Submerged Sediments
To collect undisturbed core samples of sediment up to a maximum depth of four feet
below sediment surface.
The fully assembled sampler is manually lowered into the water in such a way that
the coring tip is placed on the sediment surface. The sampler can then be either
manually pushed with the cross handle or driven with the slide-hammer or an
electric hammer to the desired sediment depth. The sampler is removed from the
sediment either manually by reverse hammering or with the tripod-mounted winch.
Once the sampler has been retrieved, either the interlocking split core tubes are
disassembled or the coring tip or top cap is removed to allow removal of the core
tube liner.
This sampler is designed to collect undisturbed, cylindrical core samples of various
types of sediment, including saturated sands and sifts, to a maximum depth of 48
inches below the sediment surface.
The sampler is lightweight and easy to operate, requiring minimal skills and training.
An (SOP) accompanies the sampler when it is purchased. A combination of
stainless-steel split core tubes can be used to collect 6- to 48-inch-long sediment
cores. Plastic core tube liners can be used with the sampler. The sampler design
uses a ball check valve-vented top cap. This feature: (1 ) allows air and water to exit
the sampler during deployment, (2) prevents water from entering the sampler during
retrieval, and (3) creates a vacuum to help retain a sediment core during sampler
retrieval.
The core tube liner is exposed to different layers of sediment contamination during
sample collection. The ball check valve-vented top cap may become clogged if the
sampler is deployed in such a way that the top cap is below the sediment surface.
The sampler cannot collect discrete samples from various sediment depths and is
subject to core shortening. Because an external power source is required to operate
the electric hammer, the sampling platform must be able to accommodate the
weight and size of a portable generator. Use of the tripod-mounted winch or similar
device limits the sampling platform locations from which the sampler can be
deployed.
USEPA. 1999e. Sediment Sampling Technology Art's Manufacturing and Supply,
Inc., Split Core Sampler for Submerged Sediments, Superfund Innovative
Technology, Evaluation Program, EPA/600/R-01/009. Office of Research and
Development, U.S. Environmental Protection Agency, Washington, DC.
hitp/Avww epa gov/ORD/S I TE /reports/6
00r01009.htm
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2.2.1-8
Sediment Processing for Chemistry and Toxicity Testing
These methods describe protocols for removing sediment samples from sampling
collection devices and processing them for laboratory analyses.
A clean stainless steel or Teflon™ spoon is used to remove sediments from grab
samples for these analyses. Surficial sediments are removed (usually 0-2 cm) and
placed in a stainless pot. The pot is then placed in a cooler on ice (not dry ice) and
stored at 4°C. This process is repeated until sufficient quantity of sediment has
been collected and composited with the other sediments (approximately 4 L).
Sediments from sediment cores are extruded and subsampled also for the following
analyses.
For organic analysis, 250 cc of sediment is placed into a 500 ml pre-cleaned, glass
bottle for chemical analysis. The sample number is recorded and the jar is wrapped
in bubble wrap (to prevent breakage) and packed in ice.
For metals, approximately 100 cc of sediment is placed into pre-cleaned, plastic
(HDPE) sampling jars. The sample number is recorded and the sample is kept on
ice at 4' C.
For Total Organic Carbon, approximately 100 cc of sediment is placed into pre-
cleaned, glass sampling jars. The sample number is recorded and the sample is
kept on ice at 4* C.
For sediment grain size, approximately 100 cc of sediment is placed into a clean
plastic (HDPE) sampling jar or wniri-pak bag. The sample number is recorded and
the sample is kept on ice at 4' C.
For sediment toxicity, the volume of sediments collected will vary depending on the
objectives and methods of the specific toxicity tests.
These methods describe the steps necessary to prepare samples for lexicological or
chemical analyses. The applicability of these tests and analyses are described in
their respective fact sheets (Sections 2.2.2 and 2.2.3).
Com positing the surface 2 cm of sediment from multiple grabs or cores allows a
representative samples to be collected. This process provides sufficient sediment
volume for toxicity testing and supporting chemistry and physical measurements.
Extreme care must be taken to ensure that the samples are not contaminated during
sampling or processing procedures.
USEPA. 2000b. Coastal 2000 Northeast Component: Field Operations Manual,
Environmental Monitoring and Assessment Program (EMAP). EPA/620/R-00/002.
Office of Research and Development, U.S. Environmental Protection Agency,
Washington, DC.
http //www epa qov/emap/nca/html/docs/c2kn Last Accessed: 1/28/2003
efm odf
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2.2.1-9
Sediment Processing for Elutriate Toxiaty Tests
This method describes how elutriate samples are prepared For toxicity tests from the
original whole-phase sediment samples.
Elutriates are prepared with one part sediments (from sampling location) and four
parts reconstituted dilution water. A 200 g sub-sample of homogenized sediment is
removed from the containers and placed in a centrifuge bottle with 800 g of dilution
water (usually site water). The contents are weighed, mixed and centrifuged. The
overlying water is removed and the elutriate sample is sub-sampled and stored in 1-
L amber bottles equipped with Teflon™-lmed lids until testing. Test organisms are
exposed to varying concentrations of the elutriate material (0%, 12.5 %, 25%, 50%
and 1 00%)for a designated period of time
Elutriate toxicity tests provide information that can be used to support inferences
about the potential toxicity of the contaminated sediments from which the elutriates
are prepared and to identify the biologically active constituents of the contaminated
sediment.
Elutriate tests are commonly used to evaluate proposals to discharge dredged
material into ocean waters, and to evaluate the potential of the dredged materials to
impact ocean ecology.
Elutriate tests albw the investigator to assess the potential hazard of contaminated
sediments to aquatic organisms, to compare the relative toxicity of contaminated
sediments from different locations, and to study the biological availability of the
contaminants associated with sediments.
Elutriate toxicity tests do not necessarily reflect the toxicity of in-place sediment.
USEPA 1 993b Assessment and Remediaton of Contaminated Sediments
(ARCS) Program: Biological and Chemical Assessment of Contaminated Great
Lakes Sediment, EPA 905-R93-006. Great Lakes National Program Office, U.S.
Environmental Protection Agency,
Chicago, IL.
N/A
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2.2.1-10
Sediment Processing for Pore Water Extraction through Centrifugataon, E1391-02
This method describes a process for separation and collection of interstitial pore
water from sediment samples to provide either a matrix for toxicity testing or an
indication of the concentration and partitioning of contaminants within the sediment
matrix.
Centrifugaton may be used to isolate interstitial water for chemical or toxicological
analyses. The centrifugation conditions (i.e., speed and temperature) will vary
considerably depending on the contaminants potentially present in the pore water.
Similarly, the filtration scheme will depend on the sediment composition and the
analytes of interest. For dissolved metals and dissolved organic carbons, sediments
should be centrifuged at high speed and filtered with a 0.2-um membrane filter.
For other dissolved organic contaminants, collodial matter, and aquatic bacteria,
sediments should be centrifuged at a lower speed and filtered through a 0.45-um
membrane fitter.
Generally, 30 minutes of centrifugation at 10,000 x g is recommended for routine
toxicity testng of interstitial waters. The temperature should be set to reflect ambient
temperature at time of collection.
Interstitial water is analyzed to either provide a matrix for toxicity tesbng or an
indication of the concentration and partitioning of contaminants within the sediment
matrix. There is some indication that interstitial water may be as useful as whole
sediment for evaluating the toxicity of some sediment-associated compounds.
Centrifugabon will extract a relatively large volume of interstitial water as compared
to other separation techniques.
Centrifugation procedures vary depending on the various compositions of the
sediments, therefore it is difficult to have an established protocol. Manipulation and
centrifugation changes the redox potential of the pore water from the in situ
conditons. Filtration may also remove toxicity. Sometimes a double centnfugation is
required to remove Tine particles.
ASTM. 2001 b. ASTM Book of Standards. Section 1 1 .05. American Society for
Testing and Materials, West Conshocken, PA.
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2.2.1-11
Pore Water Extraction from Sediments through Squeezing, ASTM E1391-02
This method describes a process for separation and collection of interstitial pore
water from sediment samples to provide either a matrix for toxicity testing or an
indication of the concentration and partitioning of contaminants within the sediment
matrix.
The apparatus used for isolation of pore water by squeezing includes a filter. The
characteristics of fitters should be considered carefully based on the types of
contaminants expected.
An example method for squeezing can be found in Manheim (1966). Briefly, the
apparatus consists of a standard laboratory press and a filter unit containing a
stainless steel screen, perforated steel plate, steel filter holder and filters. Wet
sediment is transferred into a cylinder at the top of the apparatus. The whole unit is
placed in a press and pore water is removed through a bottom filter. The extraction
time will vary depending on the amount of sediment placed in the unit.
Squeezing is used to extract pore water from loose seabed sediments. Interstitial
water is analyzed to either provide a matrix for toxicity testing or an indication of the
concentration and partitioning of contaminants within the sediment matrix. There Is
some indication that interstitial water may be as useful as whole sediment for
evaluating the toxicity of some sediment-associated compounds.
This is a rapid, reproducible method for pore water collection.
Squeezing can produce artifacts due to shifts in equilibrium from pressure,
temperature, and gradient changes It can also affect the electrolyte concentration
and redox potential compared to in situ conditions.
Filiations may remove toxicity from water samples. It is difficult to choose a filtering
scheme without knowing the cause of loxicity or the mixture of the toxicant.
ASTM. 2001b. ASTM Book of Standards. Section 1 1 .05. American Society for
Testing and Materials, West Conshocken, PA.
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2.2.1-12
Pore water extraction from sediment from Vacuum Filtration, ASTM E1391-02
This method describes a process for separation and collection of interstitial pore
water from sediment samples to provide e trier a matrix for toxicity testing or an
indication of the concentration and partitioning of contaminants within the sediment
matrix.
Vacuum filtration is one of several methods (including gas pressurizahon and
displacement) that can be used to remove pore water from sediments for chemical
analysis when only a small volume is required. A vacuum extractor consists of a
fused-gtess air stone connected to a syringe with tubing. The syringe is then used to
extract the water until sufficient volume has been collected.
Interstitial water is analyzed to either provide a matrix for toxicity testing or an
indication of the concentration and partitioning of contaminants within the sediment
matrix. There is some indication that interstitial water may be as useful as whole
sediment for evaluating the toxicity of some sediment-associated compounds.
These methods are useful for collecting small amounts of water for chemical
analysis.
Problems common to this type of method are a loss of equilibration between the
interstitial water and the solids, filter clogging, and oxidation. Further research is
needed to demonstrate the utility of this method to in situ collection of sediment pore
water.
ASTM. 2001 b. ASTM Book of Standards. Section 1 1.05. American Society for
Testing and Materials, West Conshocken, PA.
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2.2.1-13
Acoustic Sub-Bottom Profiling Systems, DRP-2-03
To collect sub-bottom data for sea-floor mapping.
High-resolution acoustic profiling systems use high power signals to penetrate the
sediments of the sea floor. The signal is reflected from interfaces between
sediment strata of different acoustic impedance. These data are printed on a
graphic recorder as a continuous two-dimensional profile. The amount of
penetration will depend on the combination of the frequency and power of the
profiler being used. A 3.5 - 14 kHz frequency pulse is typically used. Penetraton
also depends on the material type which composes the bottom and sub-bottom. For
instance, differences in soil types, density, water content, and degree of
solidification greatly influence the reflecting properties of the sub-bottom strata.
Most Sub-bottom surveys are conducted in conjunction with bathymetnc and/or side
scan sonar surveys. The survey uses a predetermined grid pattern with lines
spaced at vanable distances, depending on objectives of the survey. Small survey
boats (30 to 65 ft long) are adequate for performing a complete multi system survey.
Over-the-side, surface-towed, and hull-mounted source/receiver arrays can be
used. Data acquisition must be interfaced with the navigatbn system so that
accurate information between position and data is recorded at all times.
Environmental Effects of Dredging Technical Notes EEDP-01-5 and EEDP-01-10
also discuss Sub-bottom profilers (US Army Engineer Waterways Experiment
Station, 1989; US Army Engineer Waterways Experiment Station, 1988).
Sub-bottom profiling is also discussed in the Guidelines for the conduct of benthic
studies at aggregate dredging sites by the U K. Centre of Environment, Fisheries
and Aquaculture, available online (www planning odpm gov UK/benlhic Last
accessed 2/1 0/03).
Typical applications include the monitoring of sediment disposal sites to detect
stratification within and just below deposits.
Primary advantages associated with acoustic sub-bottom profiling are continuous
documentation of reflecting strata, rapid coverage, and relatively low cost.
The quality of records obtained in seismic reflection studies depends greatly on the
presence of subsurface horizons which will reflect acoustic energy. Records in
deep water will tend to show average conditions over an area rather than a specific
profile directly below the ship. Effective use of this instrumentation requires a
trained operator.
US Army Engineer Waterways Experiment Station. 1991. Hydrologic Surveys
Applicable to Dredging Operations. DRP-2-03.
Waterways Experiment Station, U S. Army Corps of Engineers, Vicksburg MS.
http /el erdc usarce army mil/elDubs/Ddf/dro2-
03.pdf
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2.2.1-14
Side Scan Sonar, EEDP-01-10
To qualitatively map the surface characteristics
of the sea floor.
During side scan sonar analysis, an acoustic towfish projects acoustic energy at a
frequency of 100-500 kHz in a lateral direction using a pair of transducers. The
acoustic signal bounces off of the sea floor back to the transducers on the towfish.
The received signal is transmitted through the tow cable to the shipboard receiver,
which processes the signal and produces a sonograph.
A frequency of 100 or 500 kHz is generally used for monitoring disposal sites. The
lower frequency gives a greater range (i.e., 200-400 m of bottom compared to 100
m at 500 kHz) but provides less detail. At 500 kHz, the sonar is able to distinguish
differences in bottom texture that can be used to map grain size. For example, low-
backscatter indicates a silty bottom. Sand ripples in the image can be used to
interpret grain-size variation and the movements of sediment.
Environmental Effects of Dredging Technical Notes EEDP-01-5 briefly discusses
side scan sonar (US Army Engineer Waterways Experiment Station, 1989).
Side scan sonar is also discussed in the Guidelines for the conduct ofbenthic
studies at aggregate dredging sites by the U.K. Centre of Environment, Fisheries
and Aquaculture. available online (www planning odprn qov UK/bentruc Last
accessed 2/10/03).
Typical applications include the monitoring of sediment disposal sites before and
after disposal. 300 kHz or higher frequencies can also be used for habitat mapping
(/e., sea grass beds). The information gathered with side-scan sonar may be used
to direct subsequent monitoring studies.
Overlapping coverage allows precise and continuous mapping of the sea floor. Side
scan sonar delineates the edge of disposal deposits more accurately than
bathymetric data.
The interpretation of side scan images requires some training and experience.
US Army Engineer Waterways Experiment Station. 1988. Acoustic Tools and
Techniques for Physical Monitoring of Aquatic Dredged Material Disposal Sites.
EEDP-01-10. Waterways Experiment Station, U.S. Army Corps of Engineers,
VScksburg MS.
http //www wes army mil/el/dots/pdfs/eedp01-
IJLpdf
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2.2.1-15
Settlement Plates, DRP-2-03
To monitor changes in thickness of various layers of dredged and capping material
in confined upland or aquatic disposal sites.
Telescoping settlement plates are used to measure changes in height of individual
material layers at disposal site. The lower tier plate is placed on the foundation
sediment before the dredged material is deposited. After dredged material disposal,
a second tier settlement plate is slipped over the riser pipe of the lower tier and
comes to rest on the surface of the dredged material. After placement of the cap, a
third tier settlement plate is placed over the riser pipe of the second tier, and the
plate rests on the surface of the cap. Readings are made to determine changes in
individual layer thickness.
Riser pipes and settling plate can be constructed from a variety of materials. For
aquatic disposal sites, settlement plates can be designed and constructed to have a
unit weight approximating that of water so that the plates do not sink through the soft
dredged material or cause consolidation of the underlying material.
Monitoring sediment consolidation at dredged material disposal sites, consolidation
of cap at ISC sites, and consolidation of sediment and/or cap at CAD sites.
Exact changes in thickness (i.e., settlement) of various layers of deposited material
can be directly measured. Settlement of the foundation sediments can be
determined using a stationary benchmark relative to the lower tier riser pipe.
Divers must be used to place the plates and make the settlement readings. The
riser pipes/settlement plates are vulnerable to accidental disturbance, removal, or
damage by boating, fishing, or dredge disposal activities.
US Army Engineer Waterways Experiment Station. 1989. Monitoring Dredged
Material Consolidation and Settlement at Aquatic Disposal Sites, Environmental
Effects of Dredging Technical Notes EEDP-01-5. Waterways Experiment Station.
U.S. Army Corps of Engineers, Vicksburg MS.
htlp //www wes army mil/el/dots/pdfs/eedpO Last Accessed. 1/30/2003
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2.2.2 Chemical and Physical Analysis
Section 2.2.2 contains methods for sample preparation and the chemical and physical analysis of
sediment and soil. These methods characterize the chemical composition and physical properties
of sediment/soil samples collected by methods described in Section 2.2.1. Samples are often
analyzed for the presence of various inorganic and organic contaminants that may pose a threat
to human or ecological health. Many of the methods described have been developed over time to
optimize the detection, identification, and quantification of potential chemicals of concern. Several
are performance-based and may be further modified to enhance the accuracy and precision of the
method.
A variety of methods may exist for the analysis of a particular chemical parameter, all with varying
levels of quantification or degrees of sensitivity. Less sensitive methods may be used as a
screening tool during the initial site assessment to identify potential chemicals of concern. Follow-
up analysis may include the use of very precise methods that provide unequivocal identification
and trace level quantification of analytes. This variety also provides alternative methods useful in
the analysis of many types of sediment or soil samples. Interferences from certain compounds in
a sample may be avoided by the use of an alternative preparation or analytical method.
The physical properties of soil/sediment often influence the behavior of soil/sediment in the
environment, and they may be helpful in further understanding the fate of contaminants
associated with soil/sediment.
Many of the chemical and physical methods described in these fact sheets are routinely
performed and fairly standardized. As a result, more than one source of information is often cited
in each method description. Specifically, the following sources provided methods information for
section 2.1.2:
• The USEPA's Office of Water
• The USEPA's Lake Michigan Mass Balance Study Methods Compendium, 1997v
• The USEPA's Test Methods for Evaluating Solid Waste, Physical/Chemical Methods
(SW846 Methods)
• NOAA's National Status and Trends Program, 1998
• Standard Methods for Examination of Water and Wastewater, 1999
• ASTM
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Reference
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2.2.2-1
Total Mercury in Sludge, Sediment, Soil, and Tissue by Acid Digestion and BrCI
Oxidation, Appendix to Method 1631
These procedures may be used in conjunction with EPA Method 1631 B for
determination of mercury in sludge, sediment, soil, tissue, industrial samples, and
certified reference materials.
Digestion 1— This procedure is preferred for matrices containing organic materials,
such as sludge and plant and animal tissues, because the organic matter is
completely destroyed. In this procedure, a 0.2 - 1.5 g sample is digested with
HNOyH2S04. The digestate is diluted with BrCI solution to destroy the remaining
organic material.
Digestion II— This procedure is preferred for geological materials because of rapid
and complete dissolution of cinnabar (HgS), which is otherwise more slowly
attacked by the BrCI in Digestion I. In this procedure, a 0.5 - 1.5 g sample is
digested with aqua regia (HCI/HNO3 ) to solubilize inorganic materials.
The Hg concentration in the digestate is determined using EPA Method 1631B.
These procedures, in conjunction with Method 1631B, allow determination of Hg at
concentrations ranging from 1.0 to 5000 ng/g in solid and semi-solid matrices.
The method detecton limit for Hg has been determined to be in the range of 0.24 to
0.48 ng/g when no interferences are present. The minimum level of quantization
(ML) has been established as 1.0 ng/g. These levels assume a sample size of 0.5 g.
Method LMMB 050 (USEPA 1997b, EPA 905-R-97-012c) describes the automated
digestion and analysis of total mercury in sediment samples using the Cold Vapor
technique.
Mercury is one of the primary risk factors in many contaminated sediments and is
one of the primary contaminants measured as part of a chemical assessment.
The dual amalgam trap system and fluorescence detector provide greater sensitivity
and specificity in the presence of interferences, and this system must be used to
overcome interferences, if present, and to achieve the sensitivity required, if
necessary. For some site monitoring programs, total mercury is measured because
it is a more rapid method compared to methyl mercury.
In cases where total mercury exceeds threshold values, samples may need to be
analyzed for toxic methyl mercury to determine risk.
USEPA 2001 d. Appendix to Method 1631. Total Mercury in Sludge. Sediment, Soil,
and Tissue by Acid Digestion and BrCI Oxidation, EPA-821-R-01-013. Office of
Water U.S. Environmental Protection Agency, Washington, DC.
http //www brooksrand com/FileLib/1 Last Accessed. 1/30/2003
631^df
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Method Summary
Data Uses/Application
Advantages
Limitations
2.2.2-2
Trace Element Quantification Techniques
To determine major and trace elements in sediment and biological tissue
samples utilizing atomic absorption and neutron activation techniques.
Sediment samples are homogenized and freeze dried, and the dry aliquot is
homogenized. Approximately 0.2 g of dried sediment is weighed and
transferred to a Teflon™ bomb. Samples are digested by adding 3 ml HN03
and placing the bombs in a 130°C oven for approximately 12 hours. The
bombs are removed, 2 ml of concentrated HP are added, and the bombs are
returned to the oven for 12 hr. After cooling, 18 ml of 4% boric acid are added
and the bombs are returned to the oven for another 12 hr. Solution volume is
determined, and a 20-fold dilution is made for FAAS analysis of Al, Fe, Mn, Si,
and Zn. For analysis of Hg, sediment samples are digested using a modified
version of EPA method 245 5. Samples were analyzed using the following
instrumentation:
Analyte Method
Hg Cold vapor atomic absorption (CVAA)
Al, Fe, Mn, Zn Flame atomic absorption (FAA)
Ag, As, Cd, Cr. Cu. Ni. Pb, Graphite furnace atomic absorption
Se. Sn (GFAA)
Al, Cr, Fe, Mn Instrumental neutron activation
analysis (INAA)
ASTM Methods D1971, D3974, and D4698 and SW846 Method 3050B
describe various digestion methods for determination of metals in sediments
(ASTM. 2001 a).
Standard Method 3030K, ASTM Method D5258. and SW846 Method 3051
describe the microwave digestion method (APHA, 1999; ASTM, 2001 a).
Several methods describe the analysis of metals using various atomic
absorption methods, such as Standard Method 31 12 B for CVAA, 31 1 1 for
FAA, 3113B for GFAA and SW846 7000 series of methods.
Chemical screening of trace metals in sediments against contaminant
guidelines provides an indication that adverse effects may or may not be
occurring.
Tissue sample digestion in a Teflon™ bomb is a standard method for "clean"
digestion for metals analysis. The instrumental suite employed in this method
takes advantage of the know strengths of each instrument for trace analysis.
For example, GFAA is much more sensitive than FAA, requiring only a small
volume of sample for trace analysis, and CVAA is very sensitive for mercury.
Processing of samples for trace levels required for risk assessments requires
class-100 clean room, or other suitable environment.
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Website
2.2.2-2 (contd.)
NOAA. 1998. Sampling and Analytical Methods of the National Status and
Trends Program, Mussel Watch Project: 1996 Update, NOAA Technical Memo
NOS ORCA 130. National Oceanic and Atmospheric Administration, Silver
Spring, MD. 233 pp.
http //ccma nos noaa qov/publications/
lm130 odf
Last Accessed: 1/30/2003
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Method Summary
Data
Uses/Application
Advantages
Limitations
2.2.2-3
Analysis of Marine Sediment and Bivalve Tissue by X-Ray Fluorescence, Atomic
Absorption and Inductively Coupled Plasma Mass Spectrometry
To determine the concentration of 17 metals in sediment and biological tissue
samples utilizing atomic absorption, inductively coupled plasma mass spectrometry
(ICP-MS). and energy dispersive X-ray fluorescence (XRF).
Sediment samples are weighed and freeze-dried. The dried sample is ground in a
ball mill. 0.5 g aliquots are used directly for XRF analysis or are further digested for
AA or ICP-MS analysis.
200 mg of dried sediment is placed in a Teflon™ bomb, to which 1 ml of 4:1
HNOa/HCI04 is added. The bombs are heated in a 130°C oven for4 hours. After
cooling, 3 mL of concentrated HF are added to the bomb, and the bombs are
heated again in a 130°C oven for 8 hours. After cooling, the digestates are diluted to
approximately 20 mL with deionized water. Solution volumes are calculated, and the
digestates are analyzed directly by GFAA or CVAA. For ICP-MS analysis, a 10-mL
aliquot of the digestate is dried in a perchloric acid hood. The dried digestate is
dissolved in 1 mL of 10% HNO3 and dried again. The dried digestate is dissolved
again in 1 mL of 10% HNO3 and 9 mL of deionized water.
AnalyteMethod
Hg Cold vapor/gold foil amalgam
Cd, Se, Ag Graphite furnace atomic
absorption(GFAA)
Ag, Al. Cr, Cd, Ni, Pb, Sb, Sn ICP-MS
Al, As, Cr. Cu, Fe, Mn, Ni, Pb, Si, Zn XRF
Standard Method 3030K, ASTM Method D5258, and SW846 Method 3051 describe
the microwave digeston method (APHA, 1999; ASTM, 2001 c). Selected methods
for the analysis of metals include: Standard Methods 31 12B for CVAA. 31 13B for
GFAA. and 3120B for ICP-MS; SW846 Method 6020 for ICP-MS and SWB46 7000
series for atomic absorption (APHA, 1999).
Chemical screening of trace metals in sediments against contaminant guidelines
provides an indication that adverse effects may or may not be occurring.
XRF analysis does not require digestion of the sample. Crustal elements such as
Al, Cr, Fe, Ni, and Si, that can be difficult to dissolve from sediment, can be
quantified by XRF. ICP-MS has the advantage of simultaneous analysis of many
elements with detection limits much lower than the XRF and similar to those of
GFAA. ICP-MS is particularly sensitive for Al, Cr, Ni, Ag. Cd, Sn, Sb, and Pb.
CVAA is very sensitive and reliable for Hg analysis.
Leakage at high pressure can cause loss of Hg from the sample during digestion.
Analysis of GFAA requires the use of matrix modifiers and standardization of the
instrument by method of addition to the sample matrix to provide accurate results.
XRF and total HF digestion measure total metals, which may not reflect levels that
are bioavailable.
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Website
2.2.2-3 (contd.)
NOAA. 1998. Sampling and Analytical Methods of the National Status and Trends
Program, Mussel Watch Project: 1996 Update, NOAA Technical Memo NOS ORCA
130. National Oceanic and Atmospheric Administration, Silver Spring, MD. 233 pp.
htto //ccma nos.noaa aov/oublications
/tm130odf
Last Accessed: 1/30/2003
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Method Summary
Data
Uses/ Application
Advantages
Limitations
Reference
Website
2.2.2-4
Determinaton of Acid Volatile Sulfide and Selected Simultaneously Extractable
Metals in Sediment
For the determination of acid volatile sulfide (AVS) and for selected metals that are
solublized during the acidification step (simultaneously extracted metal, SEM).
Sediment samples must be protected from exposure to oxygen during collection and
storage. If possible, the head space in the sample container should be filled with
oxygen-free nitrogen or argon. Appropriate storage conditions: frozen (preferred if
sediments to be used for chemical analyses only) or refrigerated to 4 degrees .
Celsius (if sediments to be used for biological tests as well); glass containers if
refrigerated, but plastic is acceptable if frozen. About 10 gm of sediment is acidified
with hydrochloric acid at room temperature to convert the AVS to hydrogen sulfide.
The H2S is then purged from the sample and trapped in an aqueous solution, which
varies depending upon the analytical method being used. Using the color imetric
method, the H2S is trapped in sodium hydroxide. The sulfide reacts with N-N-
dimethyl-p-phenylenediamine to form methylene blue, which is then measured
colorimetrically at 670 nm. Using the gravimetric method, the sulfide is trapped in
silver nitrate, forming a silver sulfide precipitate. The silver sulfide is isolated onto a
1.2 micron filter by filtration. The filter is dried and the amount of silver sulfate is
weighed. Using the third method, the sulfide is trapped in an anttoxidant buffer, and
the sample is analyzed using an ion-selective sulfide electrode.
After the determination of AVS, the acidified sediment sample is filtered through a
0.2u membrane fitter. The filtrate is analyzed for SEM (commonly, cadmium,
copper, lead, silver, nickel, and zinc) by atomic absorpton or inductive coupled
plasma spectrometric methods.
Both AVS and SEM are expressed on a umole per gram dry sediment basis. The
ratio of SEM to AVS is the sum of the concentrations of SEM metals divided by the
acid volatile sulfide concentration.
Sulfide is Important in controlling the bioavaitability of metals in anoxic sediments.
The amounts of SEM and AVS are important in predicting the bioavailability of
metals.
The gravimetric procedure can be used with samples that have a moderate or high
AVS concentration. The colonmetric method is capable of determining AVS
concentrations over a range of 0.01-1000 umoles/gram dry weight. The sample
purging and trapping apparatus may consist of either Erlenmeyer flasks (less costly)
or ground glass stoppered flasks (better sealing).
Sulfide ion is unstable in the presence of oxygen. Sulfide can be formed or lost due
to biological activity during storage Leakage of the Erlenmeyer flasks may cause
low recovery of AVS.
USEPA. 1 991 . Draft Analytical Method for Determination of Acid Volatile Sulfide in
Sediment, EPA-821-R-91-100. Office of Water, U.S. Environmental Protection
Agency, Washington, DC. Proper storage of samples will mitigate these limitations.
N/A Last Accessed:
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Advantages
Limitations
Reference
Website
2.2 2-5
Photovac GC Analysis for Soil, Water, and Air/Soil Gas, OSWER SOP# 2109
This method is designed as a field screening procedure for the tentative
identification of various volatile organic compounds.
Soil samples are collected in 40-mL VOA vials with Teflon™-lined silicons septum
screw caps. A 5 gm aliquot of sample is weighed into a second, clean VOA vial.
Reagent water is added to the sample to bring the volume in the vial to 20 mL. The
vial is capped, shaken vigorously for one minute, and allowed to stand at room
temperature for at least one hour for vapor phase equilibration. An aliquot of the soil
head space is then removed from the vial and injected into the GC using a gas-tight
syringe. The GC uses an ultraviolet light source and photoionization detector.
Concentrations are reported as ug/kg.
Typical MDLs for this method range from 1 ppb to 5 ppb.
SO Ps # 2108 and #2107 describe the operation of specific models of Photovac Gas
Chromatographs.
Site assessment/characterization and health and safety surveys.
The data generated with this method allows for rapid evaluation of site conditions.
Pollutant identification is only tentative.
USEPA. 19945. SOP # 2109: Photovac GC Analysts for Soil, Water, and Air/Soil
Gas Compendium of Emergency Response Team Standard Operating Protocols.
Office of Solid Waste and Emergency Response, U.S. Environmental Protection
Agency, Edison NJ.
htto //www.ert.ora/oroducts/21 09 .PDF
Lasfcccessed: 1/30/2003
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Method Summary
Data Uses/Application
Advantages
Limitations
2.2.2-6
Extraction and Clean-Up of Sediments for Semi-volatile Organics Following the
Internal Standard Method, LMMB 040
To prepare the sediment samples for the measurement of organic
contaminants, such as polychlorinated biphenyls, polynuclear aromatic
hydrocarbons, and chlonnated pesticides.
Following Method LMMB 040 (USEPA 1997d: EPA 905-R-97-012c). 15 - 30 g
of sediment are chemically dried with sodium sulfate, spiked with surrogate
standards, and extracted with DCM using a 30°C sonication bath (sonicate for
60 minutes, let stand in bath overnight [24 hours] and sonicate again for 60
minutes). During a silica/alumina column clean-up, two separate fractions are
collected. The first fraction, which is eluded with hexane, contains RGBs,
HCB, 4, 4'-DDE, aldrin, and heptachlor. The second fraction, which is eluded
with 10% diethyl ether in hexane, contains alpha- and gamma-BHC,
chlordanes, 4,4'-DDT, 4,4'-DDD, and all PAHs. The two fractions are
concentrated. The first fraction is treated with activated copper and frozen at -
15*C until analysis. The second fraction is solvent exchanged into hexane and
refrigerated until analysis.
Following NS&T procedures, samples are stored frozen at approximately -
15°C until extraction. A 10 - 30 gram aliquot of the homogenized sediment
sample is chemically dried with sodium sulfate, spiked with surrogate
standards, and extracted with dichloromethane (DCM) using a Soxhlet
apparatus for 8 hours. The extract is concentrated, filtered if necessary, and
solvent changed to hexane. The sample is cleaned-up using purified silica
gel/alumina column chromatography before instrumental analysis. Activated
copper in the column removes elemental sulfur that may be present. The
sample is concentrated to 1 mL in hexane for analysis. Chemical surrogates
are used to monitor extraction and cleanup efficiency.
Several methods for sample extraction and clean-up are described in SW846
Methods 3500B and 3600C. ASTM Method D3976 describes the preparation
of sediment samples for volatile, semi-volatile, and nonvolatile analyses
(ASTM, 2001 c).
Polychlorinated biphenyls and high molecular weight PAHs are primary risk
factors in many contaminated sediments and are measured as part of the
chemical assessment of a site characterization and to assess remediation
effectiveness.
Both of the above listed methods, or variations based on performance, are
sufficient for the analysis of PCB by GC-ECD or GC/MS (low resolution) or the
analysis of PAH by GC/MS (low resolution).
Method interferences may be caused by contaminants in solvents, reagents,
glassware, and other sample processing hardware. Matrix interferences result
from co-extraction of compounds other than the analytes of interest, such as
elemental sulfur and lipids.
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Reference
Website
2.2 2-6 (contd.)
USEPA. 1997d. Method LMMB 040: Extraction and Clean-Up of Sediments for
Semi-volatile Organics Following the Internal Standard Method in Lake Michigan
Mass Balance Study Methods Compendium, Volume 2: Organic and Mercury
Sample Analysis Techniques, EPA 905-R-97-012c. Great Lakes National Program
Office, U.S. Environmental Protection Agency, Chicago, IL.
http://www eoa aov/qlnDo/lmmb/methods/soD-
401 pdf
Last Accessed: 1/30/2003
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Method Title
Purpose
Method Summary
Data
Uses/ Application
Advantages
Limitations
Reference
Website
2.2.2-7
Quantitative Determination of Polynuclear Aromatic Hydrocarbons by Gas
Chromatography/Mass Spectrometry (GC/MS) - Selected Ion Monitoring (SIM)
Mode
To determine low concentrations of Polycyclic aromatic hydrocarbons (PAHs) and
their alkylated homologues in extracts of water, sediments and biological tissues.
Just prior to analysis, an aliquot of internal standard solution is added to the sample
extract producing a final internal standard concentration of approximately 40 ng/mL.
The analytical system includes a temperature programmable gas chromatography
with a fused silica capillary column. Helium is used as the carrier gas, and the
samples are handled by an auto sampler capable of making 1 - 4 ul injections. A
five point calibration curve is established to demonstrate the linear range of the
detector. The effluent from the GC capillary column is routed directly into the ion
source of the mass spectrometer (MS). The MS is operated in the SIM mode using
appropriate windows to include the quantization and confirmation masses for target
PAHs. For all compounds detected at a concentration above the MDL, a
confirmation ion is checked to confirm its presence. The response factors of the
surrogate relative to each of the calibration standards are calculated, followed by the
calculation of the sample extract concentration. The sample concentration for each
compound is calculated by dividing the sample extract concentration by the sample
amount
PAH concentrations are primary risk factors associated with contaminated
sediments. PAH data obtained from this analysis are used for site characterization
and risk assessments.
GC/MS in the SIM mode provides unambiguous and sensitive detection for PAHs.
The PAH quantization method is very rigorous because PAHs have very strong
molecular ion peaks under the mass spectrometric conditions used. Alkylated PAH
homolog data can be used for source identification. Also, the availability of labeled
surrogates internal standards of many of the analytes makes very accurate
determinations of analyte concentrations possible.
GC/MS in SIM mode cannot be used for simultaneous screening for other organic
contaminants of similar polarity or volatility; cannot be used to identify tentatively
identified compounds (TICs).
NOAA. 1998. Sampling and Analytical Methods of the National Status and Trends
Program, Mussel Watch Project: 1996 Update, NOAA Technical Memo NOS ORCA
130. National Oceanic and Atmospheric Administration, Silver Spring, MD. 233 pp.
http //ccma nos noaa qovfpublications Last Accessed: 1/30/2003
/tm30 odf
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Method Summary
Data
Uses/Applicator
Advantages
Limitations
Reference
Website
2.2 2-8
Analysis of Polychlonnated Biphenyls and Chlorinated Pesticides by Gas
Chromatography with Electron Capture Detection, LMMB 041
To quantify chlorinated hydrocarbons (i.e., chlorinated pesticides and PCBs) in
sample extracts.
This method is based on high resolution, capillary gas Chromatography using
electron capture detection (GC/ECD). Extracts normally have a holding time of 40
days. The instrument's detector is calibrated before the sample in injected.
PesticidePCB calibration is done also as part of the analytical run. If the response
for any peak exceeds the highest calibration solution, the extract is diluted, a known
amount of surrogate and TCMX solution added, and the sample reanalyzed for
those analytes that exceeded the calibration range. Concentrations in the samples
are calculated based on the internal standard method. Data is reported as ng/g dry
weight.
Other methods describing the analysis of PCBs and pesticides by GC/ECD are
NS&T methods. ASTM Method E697. and SW846 Methods 8081 A and 8082
(NOAA. 1998; ASTM. 2001d).
PCBs and persistent pesticides (particularly DDT and metabolites) are two of the
primary risk factors of contaminated sediments. Data are used in site
characterization and in risk analysis.
The ECD is very sensitive and allows for detection of the chlorinated hydrocarbons
at trace concentrations (ppb).
The detector does not have a linear response over a wide concentration
range and must be used by sufficiently trained personnel. Second column analysis
must be performed to provide unequivocal compound identification. These methods
do not measure the 12 World Health Organization PCB congeners, which may be
desired data in some risk assessments. A separate analysis using a different GC
column is required for peak confirmation.
USEPA. 1997d. Method LMMB 041: Analysis of Polychlorinated Biphenyls and
Chlorinated Pesticides by Gas Chromatography with Electron Capture Detection, in
Lake Michigan Mass Balance Study Methods Compendium, Volume 2: Organic and
Mercury Sample Analysis Techniques, EPA 905-R-97-012C. Great Lakes National
Program Office, U.S. Environmental Protection Agency, Chicago, IL.
httpV/www epa qov/qlnpo/lmmb/methods/
sop-501 pdf
Last Accessed: 1/30/2003
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Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.2.2-9
Screening for Polychlonnated Biphenyls by Immunoassay. SW846 Method 4020
This method is used to screen soils and non-aqueous waste liquids for the presence
of polychlorinated biphenyls (PCBs).
This method is used to determine when PCBs are present at concentrations above
5, 10 or 50 mg/kg. The method is most often performed using a sample extract.
Determining the presence of PCBs above concentrations other than 5. 10 or 50
mg/kg is possible by dilution of the sample extract. The sample extract and an
enzyme conugate reagent are added to immobilized antibody. The enzyme
conjugate "competes" with PCB present in the sample for binding to immobile anti-
PCB antibody. Test kits are commercially available for this method. Each
commercially-available test kit will supply or specify the apparatus and materials
necessary for successful completion of the test. The manufacturer's directions
should be followed. Method 4020 provides an estimate for the concentration of
PCBs by comparison with a standard.
Site characterization, screening.
Test kits are commercially available for this method.
This method does not provide information regarding congener or Aroclor
concentrations. High levels of chemically-similar compounds may register a false
positive. Method is intended for screening, not for quantitative analysis. In cases
where the exact concentrations of PCBs are required, quantitative techniques
should be used. If the proportions of PCB congeners in the calibration standard are
not similar to the proportions present at the site, accuracy can be compromised.
USEPA. 1996h. Screening of Polychlorinated Biphenyls by Immunoassay, SW846
Method 4020. Office of Solid Waste, U S. Environmental Protection Agency,
Washington, DC.
http //www epa qov/epaoswer/hazwaste/ Last Accessed: 2/13/03
test/odfs/4020 odf
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Method Summary
Data
Uses/ Application
Advantages
Limitations
Reference
Website
2.2.2-10
Tetra- through Octa-Chlorinated Dioxins and Furans by Isotope Dilution
HRGC/HRMS, EPA Method 1613
This method is for determination of tetra- through octa-chlorinated dibenzo-p-dbxins
(CDDs) and dibenzo furans (CDFs) in solids (not tissue).
This method is "performance-based". The labeled compounds are spiked into a
sample containing 10 g (dry weight) of solids. Samples containing multiple phases
are pressure filtered and any aqueous liquid is discarded. Coarse solids are ground
or homogenized. Any non aqueous liquid from multi phase samples is combined
with the solids and extracted in an extractor. The extract is concentrated for cleanup.
After extraction. 37CI4-labeled 2,3,7 ,8-TCDD is added to each extract to measure the
efficiency of the cleanup process. Sample cleanups may include back-extraction
with acid and/or base, and gel permeation, alumina, silica gel, Florisil and activated
carbon chromatography. High-performance liquid chromatography (HPLC) can be
used for further isolation of the 2,3,7,8-isomers or other specific isomers or
congeners. After cleanup, the extract is concentrated to near dryness. Immediately
prior to injection, internal standards are added to each extract, and an aliquot of the
extract is injected into the gas chromatography. The analytes are separated by the
GC and detected by a high-resolution (^1 0,000) mass spectrometer.
CDD/CDF Minimum Level (ng/kg) CDD/CDF ML(ng/kg)
2.3,7,8-TCDF 1 1,2,3.4 ,7 ,8-HxCDD 5
2,3,7,8-TCDD 1 1, 2,3,6,7 ,8-HxCDD 5
1,2,3,7,8-PeCDF 5 1 ,2,3,7 ,8,9-HxCDD 5
2,3,4,7,8-PeCDF 5 1,2.3.4 ,6,7 ,8-HpCDF 5
1, 2,3,7 ,8-PeCDD 5 1,2,3,4 ,7 ,8,9-HpCDF 5
1, 2.3.4 ,7,8-HxCDF 5 1,2,3,4 ,6,7 ,8-HpCDD 5
1,2,3,6,7,8-HxCDF 5 OCDF 10
1 ,2,3,7 ,8,9-HxCDF 5 OCDD 10
2.3,4,6,7,8-HxCDF 5
This method is also described in SW846 Method 8290 and NS&T methods (NOAA
1998).
The method is for use in EPA's data gathering and monitoring programs associated
with the Clean Water Act, the Resource Conservation and Recovery Act, the
Comprehensive Environmental Response, Compensation and Liability Act, and the
Safe Drinking Water Act.
Method 1613 is able to meet detection limits required for human health and
ecological risk assessments.
The GC/MS portions of this method are for use only by analysts experienced with
HRGC/HRMS or under the close supervision of such qualified persons
USEPA. 1994c. Method 1613: Tetra- through Octa-Chlorinated Dioxins and Furans
by Isotope Dilution HRGC/HRMS, EPA 821-B-94-005. Office of Water, U S.
Environmental Protection Agency, Washington, DC.
http //www epagov/waterscience/methods/1613 odf L^t Accessed- 1/30/2003
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Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.2.2-11
Toxic Polychlonnated Biphenyls by Isotope Dilution High Resolution
Gas Chromatography/High Resolution Mass Spectrometry, EPA Method 1668
This method is for determination of the toxic polychlorinated biphenyls (PCBs) in
solids (not tissue).
This method is performance-based. The labeled compounds are spiked into a
sample containing 10 g (dry weight) of solids. Samples containing multiple phases
are pressure filtered and any aqueous liquid is discarded. Coarse solids are ground
or homogenized. Any non-aqueous liquid from multi-phase samples is combined
with the solids and extracted in an SDS extractor. The extract is concentrated for
cleanup. After extraction, samples are cleaned up using back-extraction with
sulfuric acid and/or base, and gel permeation, silica gel, Florisil and activated carbon
chromatography. High-performance liquid chromatography (HPLC)can be used for
further isolation of specific isomers or congeners After cleanup, the extract is
concentrated to near dryness. Immediately prior to injection, internal standards are
added to each extract, and an aliquot of the extract is injected into the gas
chromatography. The analyles are separated by the GC and detected by a high-
resolution (2 10, 000) mass spectrometer.
Extract
IUPAC EMDL(ngAg) EML(ngfkg) EML (pg/|JL)
77 0.5 2 1
123 4 10 5
126 10 4 5
118/167/15&157/169/1WV170/189 6 20 10
114 60 200 100
105 40 100 50
EMD: = Estimated Method Detection Limit; EML = Estimated Minimum Level
The method is for use in EPA's data gathering and monitoring programs associated
with the Clean Water Act, the Resource Conservation and Recovery Act, the
Comprehensive Environmental Response, Compensation and Liability Act, and the
Safe Drinking Water Act.
Method 1668 provides data for most, but not all. of the "dioxin-like" PCBs, including
those with the highest TEFs, as determined by the World Health Organization. This
method provides detection limits frequently required in risk assessments.
The GC/MS portions of this method are for use only by analysts experienced with
HRGC/HRMS or under the close supervis on of such qualified persons. Method
1668 does not provide data for all of the •dioxin-like" PCBs, as does Method 1668A.
USEPA. 1997e. Method 1668: Toxic Polychlorinated Biphenyls by Isotope Dilution
HRGC/HRMS. EPA-821-R-97-001. Off ice of Water, U.S. Environmental Protection
Agency, Washington, DC.
http://www epa gov/clanton/clhtml/pubtitl Last Accessed: 1/30/2003
eOW.html
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2.22-12
Chlorinated Biphenyl Congeners in Water. Soil, Sediment, and Tissue by
HRGC/HRMS, EPA Method 1668 Revision A
This method is for congener-specific determination of more than 150 chlorinated
biphenyl (CB) congeners in solids (not tissue).
This method is performance-based. The labeled compounds are spiked into a
sample containing 10 g (dry weight) of solids. Samples containing multiple phases
are pressure filtered and any aqueous liquid is discarded. Coarse solids are ground
or homogenized. Any non-aqueous liquid from multi phase samples is combined
with the solids and extracted in a Soxhlet/Dean-Stark extractor. The extract is
concentrated for cleanup. After extraction, a labeled cleanup standard is spiked into
the extract which is then cleaned up using back-extraction with sulfuric acid and/or
base, and gel permeation, silica gel, or Florisil chromatography. Activated carbon
and high-performance liquid chromatography (HPLC) can be used for further
isolation of specific congener groups. After cleanup, the extract is concentrated to
20 uL. Immediately prior to injection, labeled injection internal standards are added
to each extract and an aliquot of the extract is injected into the gas chromatography
(GC). The analytes are separated by the GC and detected by a high-resolution
(a 10,000) mass spectrometer.
Without interferences, EMDLs and EMLs will be, respectively, 0 5 and 1.0 ng/kg for
soil, tissue, and mixed-phase samples, and EMLs for
extracts will be 0.5 pg/uL.
EMD: = Estimated Method Detection Limit; EML = Estimated Minimum Level
This Method is for use in data gathering and monitoring associated with the Clean
Water Act, the Resource Conservation and Recovery Act, the Comprehensive
Environmental Response, Compensatbn and Liability Act, and the Safe Drinking
Water Act.
Method 1668A provides congener data that can be used for source identification.
Listed PCBs include the 12 World Health Organization "dioxin-like" PCBs. The
HRMS method provides lower EMDLs compared to ECD or low resolution MS
analyses and provides unequivocal congener identification.
The GC/MS portions of this method are for use only by analysts experienced with
HRGC/HRMS or under the close supervision of such qualified persons. Solvents,
reagents, glassware, and other sample processing hardware may yield artifacts,
elevated baselines, and/or lock mass suppression causing misinterpretation of
chromatograms.
USEPA. 1999c. Method 1668, Revision A: Chlorinated Biphenyl Cogeners in Water.
Soil, Sediment, and Tissue by HRGC/HRMS, EPA-821-R-00-002. Office of Water,
U.S. Environmental Protection Agency, Washington, DC.
http //www epa gov/region08/water/wast
ewater/biohome/biosohdsdown/methods
/1668a5odf
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2.2.2-13
Butyltin in Sediments
The extraction and analysis of organotin compounds in soil and sediment.
A 15 g aliquot of freeze-dried sediment sample is spiked with surrogate standards
and shaker extracted four times with 0.2% tropolone in dichloromemane. The
extract is concentrated by Kuderna-Damsh technique and solvent exchanged to
hexane. Organotin compounds are hexylated with hexybnagnesium bromide
(Grignard reagent) by adding the reagent to the sample and heating the sample at
70°C for 30 minutes. The excessive reagent is removed with HCI and the organic
phase of the sample removed. The remaining aqueous phase is extracted twice
with pentane: CH2CI2 (3/1, v/v). The combined hexylated extract is dried with
sodium sulfate and concentrated. The sample is loaded onto a silica gel/alumina
column and eluded with pentane. The cleaned sample is concentrated and
analyzed by high resolution, capillary gas chromatography using flame photometric
detection (GC/FPD). This method quantitatively determines Tetra butyltin (4BT),
tributyltin (TBT), dibutyltin (DBT), and monobutyltin (MBT). Results are reported as
ng Sn/g.
Butylin is a principal risk factor in many freshwater and marine harbor sediments.
FPD is a sensitive detector that is specific to tin. Hexylatton of the organotin anions
provides compounds amenable to the GC/FPD technique and provides reliable
quantization of organotins at low concentrations (ng Sn/g).
Organotins are ubiquitous laboratory contaminants. Clean methods must be
observed.
NOAA. 1998. Sampling and Analytical Methods of the National Status and Trends
Program, Mussel Watch Project: 1996 Update, NOAA Technical Memo NOS ORCA
130. National Oceanic and Atmospheric Administration, Silver Spring. MD. 233 pp.
http //ccma nos noaa qovfpublications
/tm130 Ddf
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2.2.2-14
Procedures for Sediment Total Organic Carbon (TOC) Determination
Determination of the TOC content in a sample by combustion.
This method describes TOC determination by combusting preacidified samples at
high temperature and measuring the volume of carbon dioxide gas produced.
Samples are homogenized and 5 g wet weight subsamples dried for approximately
48 hours in a covered evaporation dish. The dried sediment sample is then ground
with a porcelain pestle. Approximately 20 to 30 mg of the dried and ground
sediment sample are placed in small beakers and acidified to remove-sources of
inorganic carbon. Samples are then dried again and then exposed to a pre-
com busted stream of oxygen. The C02 evolved is measured by an infrared gas
analyzer and the resulting gas peak is integrated. Integrator units are compared to a
standard curve to convert to organic carbon.
Alternatively, using the NS&T method, 0 1 to 0.5 ± 0.001 g of oven-dried, finely
ground homogenized sediment is weighed into a combustion crucible (NOAA,
1998). Approximately 1.4 g each of copper and iron chip accelerators are added to
the crucible. The crucible is placed and sealed within the oven combustion tube.
Total carbon compounds in samples are decomposed by pyrolysis in the presence
of oxygen, and the CO2 that is formed is quantified by infrared detection. Total
organic carbon (TOC) is determined by acidifying the sample with 10% HCI and
drying the sample overnight at 50*C. Acidification converts carbonate carbon to
carbon dioxide, which is purged from the acidified sample prbr to analysis.
Carbonate carbon, or total inorganic carbon (TIC), is determined by the difference
between total carbon and total organic carbon.
TOC is used to normalize the concentration of nonionic organic contaminants in the
development of equilibnum partitioning sediment guideines (ESGs), and this is an
important chemical parameter for sediment quality.
The EMAP method is one of several combustion methods for TOC determination.
The TOC determination is not a substitute for the determination of biological oxygen
demand or chemical oxygen demand, should those parameters be needed.
USEPA. 1995. Environmental Monitoring and Assessment Program Laboratory
Methods Manual, Estuaries, Volume 1 -Biological and Chemical Analyses,
EPA/620/R-95/008. Environmental Monitoring and Assessment Program , U S.
Environmental Protection Agency, Washington DC.
http //www epa qov/emap/html/pubs/docs/qrou Last Accessed: 1/30/2003
pdocs/estuarv/freld/lab man odf
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2.2.2-15
Determination of the Activity of Lead-210 in Sediments and Soils, LMMB 084
This procedure measures the activity of the Pb-210 granddaughter, Po-210.
Sediment is collected with a gravity or box corer. The samples are extruded at
known intervals and placed into preweighed bottles. The samples are dried in a
60°C oven, and the dry weight calculated. The samples are then ground to a fine
powder and stored until used. 0.50 g of dried sediment is digested with a
combination of HCI and hydrogen peroxide. During the digestion, the sample is
heated on a hot plate to 90-95°C for a total of four hours. After sitting overnight, the
sample is filtered through a Whatman No. 42 filter paper into a flask. The sample is
heated until its volume is reduced to 5 mL. The pH of the sample is adjusted to 0.5
to 1.0. Ascorbic acid is added to prevent interference from ferric iron. A copper disk
is added to the sample, which is heated overnight in a 95°C oven. The Po-210
concentration on the disk is determined by alpha spectrometry using silicon surface
barrier detectors . A yield monitor, Po-208, is added to each sample to determine
the exact activity of Po-210.
The activity of Pb-210 can be used to estimate dates of sediment deposition. Such
dating can be used in establishing chronologies of sediment contamination, rates of
sediment accumulation and rates of contaminant attenuation.
Straightforward and accurate analytical method.
Pb-210 has a half life of 22 years, limiting age dating using Pb-210 to approximately
the last 100 years. If sediments have been disturbed (e.g.. by past dredging,
scouring, bioturbation), accurate dating may not be possible. It should be noted that
other analyses may be more accurate for dating sediment deposition which occurred
more recently than the last 100 years. For example, analysis for Cesium-137 may
be suitable for dating sediments deposited in the previous 50 years, while Beryllium-
7 can date sediments deposited in the previous two years. Using more than one
dating method can provide added assurance in date estimates.
USEPA. 1997c. Method LMMB 084: Determination of the Activity of Lead-210 in
Sediments and Soils. Lake Michigan Mass Balance Study Methods Compendium,
Volume 3. Metals, Conventional, Radio chemistry, and Biomonitoring Sample
Analysis Techniques. EPA 905-R-97-01 2c. U.S. Environmental Protection Agency,
Washington, DC.
http //www epa qov/qlnpo/lmmb/methods/lead- Last Accessed: 1/30/2003
210pdf
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Fact Sheet No.
2.2.2-16
Sediment Gram Size Analysis, NHEERL-AED SOP 1.01.005
To determine the percentages by weight of sand, silt, and clay in sediment samples
15 - 20 gm of sediment is treated with 50 - 100 ml of 30% hydrogen peroxide for 12
hours to oxidize any organic matter present. The sample is then washed with
distilled water to remove salts. 400 ml of sodium hexametaphosphate solution is
used to disperse the particles in the sediment. The sample is shaken for 24 hours.
The gravel/sand fraction is wet-sieved through a .063 mm sieve into an underlying
evaporation dish to separate the sands (>.063 mm} from the silt and the clay
(<. 063mm). The material remaining on the sieve(gravel/sand) is washed into a pre-
weighed beaker. This fraction is dried at 100 - 130*0 for 24 hours and then weighed
to the nearest 0.1 g.
The sill and clay in the evaporation dish is then transferred to a graduated cylinder
and 10 ml of dispersant from stock solution of sodium hexametaphosphate is
added. The solution is stirred and stored for 12 hours. If flocculation occurs, the
sample is treated with more dispersant and mixed. The silt and clay fractions are
measured using the pipette method (Folk, 1974) The solution is stirred and aliquots
are pipetted out at specified times and depths. Silt and clay fraction: After 20
seconds of stirring, the pipette is inserted to 20 cm and at the end of 20 seconds, 20
ml is removed. This fraction is placed into a beaker. Clay fraction: After 2 hours
and 3 minutes, the pipette is inserted to a depth of 5 cm and 20 ml is withdrawn.
This fraction is placed into a beaker.
The removed fractions are dried in an oven at 100 - 130*C for at least 24 hours.
Total dry weight = wt. sand + wt. silt + wt. clay. The weight of silt+clay is multiplied
by 50 and the weight of one dispersant is subtracted to obtain the total weight of
silt+clay. This process is repeated for the clay fraction. Total dry weight = wt. sand
+ wt. silt + wt clay. The respective percentages of sand, silt and clay are derived by
dividing the individual weights by the total weight and multiplying by 100.
Grain size analysis is also described in ASTM Method D422, NOAA NS&T, and
EMAP Lab methods (ASTM, 2001 e; NOAA, 1998).
Grain size is an important characteristic of sediments that may be correlated with
contaminant concentrations. Data may also be used in sediment transport methods.
This is one of several methods derived from Folk (1974) that has gained wide
acceptance for grain size determination.
This method does not provide 4> classification data; these data are important in
some transport models.
USEPA and the Naval Construction Battalion Center. 1992. Standard Operating
Procedures and Field Methods Used for Conducting Ecological Risk Assessment
Case Studies. Technical Document 2296. Naval Command, Control and Ocean
Surveillance Center, RDT&E Division, San Diego, CA.
http //www duxbury battelle org/compend Last Accessed:
lum/methods/NHEERL-AED-SOP-
1 01 005 odf
2.2.2-17
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Procedures for Water Content Determination
Determine the percent water content of sediment samples.
Sediments are placed in a 250 ml glass beaker and homogenized. Approximately
5-10 grams wet weight of sediment will be placed in a clean, tared 50 mL glass
beaker and the weight are recorded. The sample is dried for 24 hours and then
reweighed. Percent water content is then calculated.
Alternatively, using the NS&T method, sediments are homogenized using a solvent
rinsed spatula (NOAA, 1998). Approximately five grams of sample is placed in a
pre-weighed scintillation vial (combusted for 4 hr at 400°C) and the weight recorded.
The samples are dried for 24 hours in a drying oven set at 63-65°C. Samples are
placed in a desiccator and albwed to cool to room temperature for at least 30
minutes. The samples are weighed. The samples are put back in the oven for at
least 2 hr after which they are removed from the oven and albwed to cool for at
least 30 m in in a desiccator. The sample is reweighed. If the difference between
the first and second weighting wis less than ± 0.02 g, the dry weight percent is
calculated based on the last weighing.
[Vial wt. + Drv sample wt.l - [Vial wt.]
Percent dry weight = [Vial wt. + Wet sample wt.] - [Vial wt.] X 100
The percent water content is calculated as 100 - percent dry weight.
Dry weight measurements are used to calculate sediment analyte concentrations on
a dry weight basis. In addition, water content is one of a suite of parameters
typically used in settlement calculations for contaminated sediment capping studies.
The EPA Region 1 functbnal guidelines use percent solids data as follows. If the
percent solids content of a soil/sediment sample falls below 30%, all positive and
non-detect results in that sample are qualified (J for positive results, R for non-
detects). When the percent solids content of a soil/sediment sample falls below
10%, all results in that sample are rejected (R).
Dry weight measurements determined in this manner can be compared directly to
NOAA NS&T database.
This method has not been widely accepted as the method for drying to constant
weight at 1 05" C.
USEPA. 1995. Environmental Monitoring and Assessment Program Laboratory
Methods Manual, Estuaries, Volume 1 -Biological and Chemical Analyses,
EPA/620/R-95/008. Environmental Monitonng and Assessment Program , U.S.
Environmental Protection Agency, Washington DC.
htto //www epa qov/emaD/html/pubs/docs/qrou Last Accessed: 1/30/2003
odocs/estuarv/field/lab man pdf
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Advantages
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Reference
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2.2.2-18
Standard Test Method for Field Vane Shear Test in Cohesive Soil. ASTM Method
D2573
To determine the shear strength of cohesive soils.
A four-bladed vane is placed in the undisturbed soil and is rotated from the surface
to determine the torsional force required to cause a cylindrical surface to be sheared
by the vane. Friction of the vane rod and instrument must be accounted for, so as
not to record friction as soil strength. Shear is calculated as torque multiplied by the
inverse of a constant, depending on the dimensions and shape of the vane.
Field vane shear testing measures the in situ undramed shear strength of sediments
underlying the surficial low- bearing capacity sediments. In-situ contaminated
sediments to be capped are predominately fine-grained, and may have high water
contents and low shear strengths. The shear strength of sediments will influence
their resistance to localized bearing capacty or sliding failures, which may cause
localized mixing of capping and contaminated materials.
There are cost and schedule advantages to performing this procedure in the field.
This test should not be performed in any soil such as sand or silt that will permit
drainage during the test period or in soils where stones or shells are encountered by
the vane.
ASTM. 2001e. ASTM Book of Standards. Volume 04.08. American Society for
Testing and Materials, West Conshocken, PA.
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2.2.2-19
Standard Test Method for Specific Gravity of Soil Solids by Water Pycnometer,
ASTM Method D854
To determine the specific gravity of soil solids that pass the 4.75-mm sieve, by
means of a water pycnometer..
Two alternative methods exist for measuring specific gravity: procedure for moist
specimens and procedure for oven-dry specimens. Guidelines exist that
recommend the dry soil mass versus soil type and pycnometer size. After these
guidelines have been consulted and the sample size selected, the pycnometer
volume Is calbrated. The pycnometer is then weighed. Following the procedure for
moist samples, the water content of the sample is determined, and the sample is
mixed with 100 mL of water to form a slurry. The slurry is transferred into the
pycnometer. Following the procedure for oven-dry specimens, the sample is dried
to a constant mass in a 100°C oven and then transferred to the pycnometer.
Water is then added to the pycnometer to form a slurry, and the slurry is deaired
using either heat, vacuum, or a combination of both. The pycnometer is filled with
deaired water and placed into an insulated container, where it is left overnight to
thermally equilibrate. The following day, the mass of the pycnometer, soil, and water
are determined, and the temperature of the slurry is measured. The soil slurry is
transferred to a tared pan and dried to a constant mass at 110*0. The specific
gravity of soil solids at test temperature is calculated using the following equation:
Gr= Mt
(M^r-fM^-M^.vitere
Ms = the mass of the oven dry soil solids (g)
Mp*,t = the mass of pycnometer and water at the test temperature (g)
Mpws.i - the mass of pycnometer, water, and soil solids at the test temperature (g)
The specific gravity of soil solids at 20°C is calculated by multiplying the specific
gravity at the test temperature by a temperature coefficient.
Specific gravity is used to calculate the phase relationship of soils, such as void ratio
and degree of saturation, and soil solid density. In addition, specific gravity is one of
a suite of parameters typically used in settlement calculations for contaminated
sediment capping studies.
This is the standard, accepted method for measuring specific gravity in soil.
This analysis cannot be performed on soil solids that may be altered by this method
or on highly organic soil solids.
ASTM. 2001e. ASTM Book of Standards. Volume 04.08. American Society for
Testing and Materials. West Conshocken, PA.
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2.2.2-20
Standard Test Method for Permeability of Granular Soils (Constant Head), ASTM
Method D2434
To determine the coefficient of perm eability by a constant-head method.
A representative sample of soil is analyzed for particle size before the permeability
test. Any particles larger than 19 mm are separated out by sieving and the
percentage of oversize material is recorded. Of the sieved sample, a subsample of
approximately twice the amount required to fill the parameter chamber is selected by
the method of quartering. First, the cross-sectional area of the sample is calculated.
A subsample of the soil is analyzed for water content. The air-dried soil sample is
spread and compacted in successive layers into the parameter until the device is
filled to the proper level. The unit weights.
void ratio, and relative density of the test
specimen are calculated. Air adhering to soil particles and present in the voids is
removed wilh a vacuum pump or aspirator. The sample is then saturated with
water, preferably native water. The inlet valve from the filter tank is opened and
time, head, quantity of flow and water temperature are recorded when a stable head
condition is attained. Test runs are repeated at heads increasing by 0.5 cm in order
to accurately establish the region of laminar flow with velocity directly proportional to
hydraulic gradient. The coefficient of permeability is calculated as follows:
k = QUAth. where
k = coefficient of permeability,
0 = quantity of water discharged,
L = distance between manometers,
A = cross-sectonal area of specimen,
t = total time of discharge, and
h = difference in head on manometers.
The permeability is corrected to that for 20°C.
Permeability measurements are needed for engineering sediment capping
alternatives.
This is the standard and accepted method
for measuring permeability in soil.
This procedure ts limited to disturbed granular soils containing not more than 10%
soil passing the 75-um sieve.
ASTM. 2001 e ASTM Book of Standards. Volume 04.06. American Society for
Testing and Materials, West Conshocken,
N/A
PA.
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2.2.2-21
Standard Test Method for One-Dimensional Consolidation Properties of Soil, ASTM
Method D2435
To determine the magnitude and rate of consolidation of soil.
This test procedure is usually performed on undisturbed samples of fine grained
soils naturally sedimented in water. The sample is trimmed and placed in the tared
consolidation ring. The sample is then trimmed flush with the plane ends of the ring.
The initial wet mass, height, volume, and water content of the sample are
determined. The sample is loaded into the consolidometer. The standard loading
schedule consists of a load increment ration (LIR) of one which is obtained by
doubling the pressure on the soil to obtain values of approximately 12, 25, 50, 100,
200, etc. kPa. The standard unloading schedule is selected by halving the pressure
on the soil. Before each pressure increment is applied, the height or change in
height of the sample is recorded Two alternative procedures exist for the analysis
of soil consolidation. Test Method A is performed with constant load increment
duration of 24 hours, or multiples thereof. Time-deformation readings are required
on a minimum of two load increments. Test Method B requires time-deformation
readings on all load increments. Successive load increments are applied after
100% primary consolidation is reached, or at constant tme increments as described
in Test Method A. The deformation results are plotted (void ratio or strain), and the
plot is used to determine the value of the preconsolidation pressure.
The data from the consolidation test are used to estimate the magnitude and rate of
both differential and total settlement of a structure or earthfill.
This is the standard and accepted method
for measuring consolidation in soil.
The test results can be greatly affected by sample disturbance and greatly
dependent on the competence of the personnel performing the test.
ASTM. 2001 e. ASTM Book of Standards. Volume 04.08. American Society for
Testing and Materials, West Conshocken, PA.
N/A
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2.2.2-22
Standard Test Method for Classification of Soils for Engineering Purposes (Unified
Soil Classification System), ASTM Method D2487
To classify mineral and organo-mineral soils based on laboratory determination of a
variety of parameters.
This classification system identifies three major soil divisions: coarse-grained soils,
fine-grained soils, and highly organic soils. These three divisions are further
subdivided into a total of 15 basic soil groups.
The minimum amount of test sample required for this test method depends on which
of the laboratory tests need to be performed. The laboratory tests include particle-
size determination, liquid limit, and plasticity index. The percentage of fines found in
the sample dictates which tests are required. The results of these tests are used to
classify soils by group.
Soil classification is used to describe a soil and to aid in the evaluation of its
significant properties for engineering use.
Provides visual classification of soils for engineering purposes
This classification system is dependent on the competence of trained personnel.
ASTM. 2001e. ASTM Book of Standards. Volume 04.08. American Society for
Testing and Materials, West Conshocken, PA.
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2.2.2-23
Standard Test Method for Liquid Limit, Plastic Limit, and Plasticity Index of Soils,
ASTM Method D431 8
To determine the liquid limit, plastic limit, and plasticity index of soils.
The liquid and plastic limits of soils (collectively referred to as Atterberg limits)
distinguish the boundaries of the several consistency states of plastic soils. These
analyses are performed only on the portion of soil that passes through the 425-um
(No. 40} sieve. Two alternative methods exist for determining the liquid limit: the
multipoint test (the recommended method) and the one-point test. The liquid limit is
determined by conducting trials in which a portion of the sample is spread in a brass
cup, divided in two by a grooving tool, and allowed to flow together which the cup is
repeatedly dropped in a standard mechanical device. In the multipoint test, three or
more trials are conducted over a range of water contents. In the one-point test, two
trials at one water content is conducted
The plastic limit is determined by alternately pressing and rolling a portion of plastic
soil into a 3.2 mm diameter thread until its water content is reduced to a point at
which the thread crumbles and can no longer be pressed together and recoiled.
The water content of the soil at this point is reported as the plastic limit. The
plasticity index is calculated as the difference between the liquid limit and the plastic
limit.
Results from these analyses are used in the soil classification process to
characterize the fine-grained fractions of soils.
This is the standard, accepted method for measuring the plasticity of soils.
The one-point test is not recommended for inexperienced analysts. The one-point
test may not be valid for certain types of soil, such as organic or marine soils.
ASTM. 2001 e. ASTM Book of Standards. Volume 04.08. American Society for
Testing and Materials. West Conshocken, PA.
N/A
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.2.2-24
Field Portable X-Ray Fluorescence Spectrometry for the Determination of Elemental
Concentrations in Soil and Sediment
Site characterization, screening
Under this method, inorganic analytes of interest are identified and quantified
directly by a field portable X-Ray fluorescence spectrometer. Radiation from one or
more radioisotope sources or an electrically excited X-Ray tube is used to generate
the characteristic X-Ray emissions in a sample. Each source emits a specific set of
primary x-rays that excite a corresponding range of elements in a samples. When
more than one source can excite the element of interest, the source is selected
according to its excitation efficiency for the element of interest.
For measurement, the sample is positioned in front of the probe window. Samples
may be analyzed in one of two manners: m situ or intrusive. If in situ mode, the
probe window is placed in direct contact with the soil or sediment In the intrusive
mode, the sample is collected, prepared, and placed in a sample cup, which is then
placed on top of the probe window inside a protective cover for analysis.
Most FPXRF instruments are menu-driven from software developed by the
manufacturer. The measurement time for each source is user-selectable. Shorter
source measurement times (30 seconds) are used for initial screening or hot spot
delineatbn. Longer times (up to 300 seconds) are used to meet higher precision
and accuracy requirements.
Twenty-six elements can be measured by this method. Field-based detection limits
established for Sb, As, Ba, Cr, Co, Cu, Pb, Mn, Mo, Ni, Rb, Sr, Sn, Zn, and Zr. Field
screening of Cu, Pb, and Zn at metal contaminated sites has been demonstrated by
the Navy (NFESC, 2000). Method 6200 is intended for dry samples. The Navy has
demonstrated good results on unprepared, wet sediment (NFESC. 2000).
Rapid on-site screening for selected elements allows rapid characterization of many
metal-contaminated sites.
High levels of V and Fe will interfere with the quantttation of Cr and Co, respectively.
A high ratio of Pb to As may result in no As being reported regardless of actual
concentration. Trained operators must understand the limitations of the method.
Confirmatory laboratory analysis required.
USEPA 2000c Method 6200, Field Portable X-Ray Fluorescence Spectrometry for
the Determination of Elemental Concenlratons in Soil and Sediment. Office of Solid
Waste, U.S. Environmental Protection Agency, Washington DC.
http //www epa qov/epaoswer/hazwaste/ Last Accessed: 1/30/2003
test/Ddfs/6200 Ddf
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Applicaton
Advantages
Limitations
Reference
Website
2.22-25
Sediment Age Dating Using Cesium-137
To determine chronological timescales in sediments using the radioisotope Cesium-
137
Sediment is collected with a coring device, as warranted by the sampling location.
The samples are extruded from the corer in 5-cm segments and collected in
sampling jars. A 100g aliquot is used for 137Ce analysis. The sediment is
homogenized, weighed and an aliquot is freeze-dried prior to analysis to determine
percent solids. Sediment for analysis can be either wet or dry and does-not require
any special storage conditons. Sediment for 137Ce analysis is gamma counted on a
Ge-diode detector. The sample is placed in front of or on top of the detector,
depending on the configuration of the system. The sample is placed in exactly the
same position as the standard and this position remains constant for all samples in
the batch. The sample is generally counted for 24 hours, depending on the size and
activity of the sample.
The activity of Cesium 137 can be used to estimate dates of sediment deposition.
Such dating can be used to establish chronologies of sediment contamination, rates
of sediment accumulation and rates of contaminant attenuation.
Cesium 137 has a relatively short residence time in natural waters.
Cesium 137 is a thermonuclear byproduct. Its presence in natural systems is
directly related to thermonuclear activity and therefore its useful in detecting effects
since the 1950's only (onset of aboveground nuclear weapons testing). Particle size
distribution (PSD, or grain size analysis) should be conducted concurrently to
support the assumption that uniform sediment processes were occurring during the
time of interest.
Battelte. 2001 . Natural Recovery of Persistent Organics in Contaminated Sediments
at the Sangamo-Weston/Twelvemile Creek/Lake Hartweil Superfund Site. US EPA
National Risk Management Research Laboratory Cincinnati. OH.
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.22-26
Beryllium- 7 as a Tracer of Short Term Sediment Deposition
To aid in the estimation of particle resuspension and deposition rales in sediments.
Sediments are collected in the field with the appropriate sampler (e.g. core, grab, or
sediment trap). Sediments are returned to the lab for analysis within 48 hours of
collection In the lab, the samples are dried to constant weight, ground, and
homogenized using a mortar and pestle. The dried sediments are then compressed
into pellets, weighed, and measured. The activity of 7Be is determined on either a
lithium-drifted or intrinsic germanium detector coupled to a multichannel
autoanalyzer. The sample prep and analysis should take place in a shielded clean
room. Prior to sample analysis the detectors are calibrated and a calibration curve
is generated based on the sample size (in height). Measured counts per minute
(cpm) are divided by the detector efficiency yielding disintegrations per minute
(dpm) The activity is converted to picocuries per gram of dry weight and corrected
for the detector efficiency.
7Be is a naturally occurring, atomosphencally derived radioisotope that can help
provide actual rates of short-term deposition and resuspension of sediments. 7Be
can be used to elucidate types and rates of processes that directly affect the cycling
of certain contaminants in the sediments, such as PCBs.
Because of it's relatively short half-life, 7Be
and resuspension rates.
allows definition of short-term deposition
7Be tracer analysis is useful in describing processes (short-term deposition and
resuspension rates), and not particle type and composition.
Fitzgerald, S.A., J Val Klump, PW Swarzenski, RA Mackenzie, and KD Richards.
2001 . Berylhum-7 as a Tracer of Short-Term Sediment Deposition and
Resuspension in the Fox River, Wisconsin. Environmental Science and Technology
351 300-305.
N/A
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2.2.3 Biological Analysis (Methods
Section 2.2.3 provides a compendium of sediment-related biological analyses. Table 2.2-1 lists
numerous acute freshwater, chronic freshwater, acute marine, chronic marine and
bioaccumulation tests that can be used to assess the effects that sediments may have on
endemic organisms. Attention was paid to include '"reference all standard test species, different
periods, endpoints. After performing physical analyses, the Superfund managers may select the
test that best suits the physical, chemical and biological parameters at their site. These tests are
performed to determine the lethal (acute) and sub-lethal (chronic) effects of the sediment on
resident organisms. These results are then compared with chemistry data to identify and
compare effects data with contaminant exposure data to determine the sediment's risk to -
ecological or human health.
The advantages and limitations associated with each test are provided in their respective fact
sheet. However, there are general limitations and interferences associated with all
active/chronic/freshwater/marine solid-phase toxicity tests. These potential interferences are
identified by some of the source documents (ASTM Method E1706 (ASTM, 2001 b), USEPA,
2000d). They are listed below:
Sediment collection handling and storage may alter bioavailability;
Natural geochemical characteristics of sediment may affect the response of test
organism;
Indigenous animals may be present in field-collected sediments;
Route of exposure may be uncertain and data generated in sediment toxicity tests
may be difficulty to interpret if factors controlling the bioavailability of contaminants
in sediments are unknown;
Tests applied to field samples may not discriminate effects of individual chemicals;
Few comparisons have been made of methods or species;
Only a few chronic methods for measuring sublethal effects have been developed
or extensively evaluated; and
Laboratory tests have inherent limitations in predicting ecological effects.
The toxicity test fact sheets provide methods described in USEPA guidance documents, Dredging
Manuals, and ASTM reports from the following agencies and offices:
The USEPA's Office of Water
The USEPA's Office of Research and Development
The USEPA and USACOE Dredging Teams
The Puget Sound Water Quality Action Team
The Puget Sound Dredged Disposal Analysis Program
The USEPA's EMAP Program
ASTM
The USEPA's Environmental Research Laboratory-Narragansett,
The USEPA's Great Lakes Program Office
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Table 2.2.3-1. A Summary of Tost Types and Toxlcologlcal Endpolnts for Solid-Phase Toxlelty
Test Type
Acute Freshwater
2.2.3-1
2.2.3-2
2.2.3-3
Acute Freshwater
2.2.3-4
Acute Freshwater
2234
Chronic
Freshwater
2.2.3^
Chronic
Freshwater
2.2.3-5
Acute Marine
25.3-7
Acute Marine
2.2.3-7
Acute Marine
2.234
Acute Marine
22.34
Acute Marine
2234
Acute
Estuanne/Marine
2.2.3-9
Acute Estuanne/
Manne
2.23-9
Test Organism
Amphipod
Crustacean
Crustacean
other than
amphipods
Insect Larvae
Amphipod
Crustacean
Insect Larvae
Bivalve
Bivalve
Echmoderrn
Echmoderm
Crustaceans
other than
amphipods
Crustaceans
other than
amphipods
Scientific Name
Ceriodaphnia dub/a
Hyallela azteca
Chmnomus
tentans
Hyallela azteca
Chironomus
tentans
Mytilus adults
Crassostrea gigas
Strongylocentrotus
purpuratus
Strongyhxentrotus
droebachtensis
Dendrasfer
excentrfcus
Mysidopsis bahia
Penaeussp
Endpolnts
Survival
Survival and
growth
Survival and
growth
Survival growth
and reproduction
growth
Survival, growth,
reproduction
emergence of
adults, egg
number, and
hatching success
Larval Survival
Larval survival,
abnormal shell
development
Embryonic
survival
Acute/Embryonic
survival
Embryonic
survival
Survival
Survival
Test
Specifics
Static, Flow
through and in
situ, 48 hours
10 days
10 days
42 days
Up to 60 days
48 hours
48 hours
48-96 hours
48-96 hours
48-96 hours
96 hours
96 Hours
Comments
Commonly used for bbassays
Short generation time, contact
with sediment
Short generation time, contact
with sediment
Short generation time, contact
with sediment
Short generation lime, contact
with sediment
May need to substitute if
sediments contain greater than
60% fines. Recommended a)
dredged material sites
May need to substitute if
sediments contain greater than
60% fines Recommended at
dredged material sites
Recommended at dredged
material sites
Recommended at dredged
material sites
Recommended at dredged
material sites
Wide tolerance to grain size,
salinity and temperature.
Epibenthos Filter-feeder,
deposit-feeder
Deposit-feeder, burrower
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Table 2.2.3-1. (contd.)
Test Type
Acute Marine
2.2.3-10
Acute
Manne/Estuarine
22.3-10
Acute Manna
2.2.3-10
Acute Marine
2.23-11
Test Organism
Amphipod
Crustacean
Amphipod
Crustacean
Amphipod
crustacean
Polychaete
Scientific Name
Ampelsca abd/ta
Eohaustorius
estuamis
Rhepoxynius
abronius
Neanthes
arenaceodentata
Endpoints
Survival
Survival
Survival
Survival
Test
Specifics
10 days
10 days
10 days
10 days
Comments
Wide tolerance to grain size.
salinity and temperature. May
be used If test sediment
contains greater than 60%
fines Tube dweller, deposit-
feeder, bunower.
Recommended at dredged
material sites
Wide tolerance to grain size,
salinity and temperature. May
be considered for use over
grain size distributions ranging
from 100% sand to 0 6% sand.
as long as the day fraction
<30%; Free burrowing, deposit-
feeder. Recommended at
dredged material sites
Preferred species for coarser-
grained sediments (i.e., fines
<60%) Free bumming, deposi-
feeder. Recommended at
dredged material sites
Size class must be uniform for
biomass estimates Tube
dweller. Deposit-feeder.
burrower. Recommended at
dredged material sites
Identified for bioaccumulation
studies based on feeding type,
biomass, salinity tolerance,
pollution tolerance, culture
potential, bioaccumulation
toxicity information, commercial
availability, and historic use in
other programs.
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Table 2.2.3-1. (contd.)
Test Type
Acute Marine
223-11
Chronic Marine
2.2.3-12
Chronic Marine
2.2.3-13
Bioaccumulation
Freshwater
22.3-17
Bioaccumulation'
Marine
2.2 3-17
Bioaccumulation '
Marine
2.2.3-17
Bioaccumulabon '
Marine
223-17
Test Organism
Polychaete
Amphipod
crustacean
Polychaete
Oligochaete
Bivalve
Bivalve
Bivalve
Scientific Name
Neanthes wrens
Leptocheirus
plumulosus
Neanthes
arenaceodentata
Lumbrculus
vanegatus
Mamma baltHca
Mamma nasuta
Yoldialimatula
Endpolnts
Survival
Survival, Growth.
and Reproduction
Survival
Bioaccumulation
Bioaccumulation
Bioaccumulation
Bioaccumulation
Test
Specifics
10 Days
28 days
28 days
28 days
28 days
28 days
28 days
Comments
Must be held under flow-
through conditions. Deposit-
feeder, burrower.
Identified for bioaccumulation
studies based on feeding type,
biomass, salinity tolerance,
pollution tolerance, culture
potential, bioaccumulation
toxicity information, commercial
availability, and historic use in
other programs.
Deposit-feeder, burrower
same as above
Easy to culture and handle,
tolerant of a wide range of
sediment characteristics, and it
is adaptable to long-term test
exposures.
Identified based on feeding
type, biomass. salinity
tolerance, pollution tolerance,
culture potential,
bioaccumulation toxicity
information, commercial
availability, and historic use in
other programs
Identified based on feeding
type, biomass. salinity
tolerance, pollution tolerance,
culture potential,
bioaccumulation toxicity
information, commercial
availability, and historic use in
other programs
Identified based on feeding
type, biomass. salinity
tolerance, pollution tolerance,
culture potential,
bioaccumulation toxcity
information, commorcial
availability, and historic use in
other programs.
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Table 2.2.3-1. (contd.)
Test Type
Bioaccumulataon'
Marine
2.2.3-17
Bioaccumulataon'
Marine
2.2.3-17
Test Organism
Polychaete
Polychaete
Scientific Name
Neanthes wrens
Nereis diversicolor
Endpolnts
Bioaccumulataon
Bioaccumulataon
Test
Specifics
28 days
28 days
Comments
Must be held under flow-
through conditions. Deposit-
feeder, burrower
Identified for bioaccumulation
studies based on feeding type.
biomass. salinity tolerance.
pollution tolerance, culture
potential, bioaccumulation
toxerty information, commercial
availability, and historic use in
other programs.
Identified for bioaccumulation
studies based on feeding type,
biomass. salinity tolerance.
pollution tolerance, culture
potential, bioaccumulation
toxerty information, commercial
availability, and historic use in
other programs
1 For bioaccumulatjon tests, it is recommended that a deposit-feeding bivalve mollusk and a burrowing polychaete are used.
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Applicaton
Advantages
Limitations
Reference
Website
2.2.3-1
Acute Freshwater Crustacean Sediment Bioassay: Flow-through
This test is used to determine the effects of a 48-hour exposure of the freshwater
crustacean. Ceriodaphnia dubia, to sediments in a laboratory flow-through system.
200-mL aliquots of sediment (by weight) are placed in 1-L glass beakers, and 800
mL of site water is added slowly. Ceriodaphnia neonates are then placed in
sediment exposure chamber (SEC) units and the units are placed in one of the test
beakers containing sediment. The inlet port of the SEC unit connects to a reservoir
(20 L) of site water. The flow-through rate is controlled by-a metering pump
calibrated to match the retention time of water flowing through the chambers in the
field. Survival of Ceriodaphnia neonates is determined at the end of the 48-hour test.
The flow-through test allows investigators to better assess sediment contamination
by simulating field conditions with water flow and controlling parameters such as pH
and dissolved oxygen to examine for direct effects from contaminants.
Ceriodaphnia dubia have been used widely as a test species. It has shown to be a
sensitive and useful test species for assessments of sediment toxicity.
Please note the list of general limitations for all solid-phase toxicity tests in the
introduction to this section.
Sasson-Bnckson, G. and G.A. Burton, Jr.
Toxicity Testing with Ceriodaphnia Dubia.
Chemistry. Vol 10. P 201 -207.
N/A
1991. In Situ and Laboratory Sediment
Environmental Toxicology and
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.2.3-2
Acute Freshwater Crustacean Sediment Bioassay: In Situ Exposures
This test is used to determine the effects of a 48-hour exposure of the freshwater
crustacean. Ceriodaphnia dubia, to sediments in situ.
Ceriodaphnia dubia are transported to the test location and placed in one of five
sediment exposure chambers (SEC). These acrylic chambers are tied together and
placed onto the sediment surface. The inlet port of the SEC is directed upstream,
so that it receives water that flows into the chamber, circulates and then exits via the
outlet port, which is directed downstream.
The SEC units are collected after 48-hours, placed in a polyethylene bucket
containing site water, covered, and transported back to the laboratory, where
surviving organisms were enumerated within 1.5 hours.
Test-site water toxicity is differentiated from sediment toxicity by placing SEC units in
situ with a plastic barrier between the unit base and the sediment surface. Water
samples are also collected simultaneously in high-density polyethylene bottles and
returned to the laboratory for toxicity testing.
In situ sediment exposures prove to be sensitive indicators of both degraded and
nondegraded stream conditions. These types of experiments provide a way to
compare and validate laboratory results to determine the accuracy of these
laboratory experiments.
Ceriodaphnia dubia have been used widely as a test species. It has shown to be a
sensitive and useful test species for assessments of sediment toxicity.
It is more difficult in the field to test effects exclusively from contaminants, since the
investigators are unable to control all other parameters such as temperature, pH,
and dissolved oxygen levels. Although the test is more representative of actual
conditions, it is less definitive in correlating contaminant presence and ecological
effects.
Please note the list of general limitations for all solid-phase toxicity tests in the
introduction to this section.
Sasson-Brickson. G. and G.A. Burton, Jr. 1991. In Situ and Laboratory Sediment
Toxicity Testing with Ceriodaphnia Dubia. Environmental Toxicology and
Chemistry. Vol 10. P 201 -207.
N/A Last Accessed:
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Method Title
Purpose
Method Summary
Data
Uses/Applicaton
Advantages
Limitations
Reference
Website
2.2.3-3
Acute Freshwater Crustacean Sediment Bioassay: Static Laboratory Exposures
This test is used to determine the effects of a 48-hour exposure of the freshwater
crustacean, Ceriodaphnia dubla, to sediments in a static laboratory system.
To assess the partitioning of sediment-bound toxicants, the sediment is tested as
solid phase, interstitial phase and elutriate phase. For solid-phase tests, sediments
are homogenized in the laboratory with a hand paddle for approximately 5 minutes.
The solid-phase test is prepared by placing 30 mL of wet sediment (by weight) into
test beakers, then slowly adding 120 mL of reconstituted hard water with a syringe.
Test beaker contents are allowed to settle for one hour prior to adding the test
organisms.
For interstitial phase tests. 400 to 450 mL of wet sediment is placed into a 500 mL
polycarbonate bottle. The samples are centrifuged at 9000 rpm for 15 minutes. The
resultant interstitial water is immediately siphoned off and placed in the test beakers.
For elutnate phase tests, sediment and water are mixed in a 1:4 ratio by volume.
Sediment is placed in a 500-mL polycarbonate bottle; 300 mL of reconstituted water
is added to the bottle. The bottles are shaken on a Eberback shaker table for 30
minutes. After the mixture has settled, the liquid portion is siphoned off and
centnfuged at 9000 rpm for 15 minutes. The supernatant water is siphoned off the
top and added to the test beakers.
Ceriodaphnia neonates are then exposed to test media (i.e., whole sediment,
interstitial water or elutriates) in 250-mL glass beakers containing 150-mL of the test
solution. Beakers are maintained at 25 +/- 1" C. Survival numbers are recorded at
24 and 48 hours. Tests were considered valid when control mortality was < 1 0%.
This test method may be useful in assessing sediment contamination, registration
of pesticides, assessments of new and existing chemicals, Superfund site
assessment, and assessment and cleanup of hazardous waste treatment, storage,
and disposal facilities.
Ceriodaphnia dubia have been used widely as a test species. It has shown to be a
sensitive and useful test species for assessments of sediment toxicity.
Please note the list of general limitations for all solid-phase toxicity tests in the
introduction to this section.
Sasson-Bnckson, G. and G.A. Burton, Jr
Toxicity Testing with Ceriodaphnia Dubia.
Chemistry. Vol 10. P 201-207.
N/A
1991. In Situ and Laboratory Sediment
Environmental Toxicology and
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
2.2.3-4
Acute Freshwater Amphipod and Freshwater Insect Larvae Sediment Bioassay, EPA
Method 100.1
This test measures the survival and growth of the estuarine amphipod crustacean.
Hyallela azteca, and the freshwater midge, Chironomus tentans after exposure to
sediments for 10 days in the laboratory.
Hyalella azteca and/or Chironomous tentans are exposed to sediments for 10-days
in a 300 mL test chamber containing 100 mL of sediment and 175 mL of overlying
water that is renewed. Test temperature is 23 "+/- 1 "C. There are 10 organisms per
chamber. The endpoints are survival and growth. Minimum mean control survival
must be 70% and measurable growth of test organisms. Test organisms are fed
daily.
ASTM E 1706-00 describes similar methods for conducting whole sediment toxicity
tests with Cladocerans, mayflies, Chironomus riporius, Diporeia spp and Tubifex
(ASTM Method E1706, ASTM 2001 b).
Environment Canada also describes a similar method using the test species Hyalla
azteca in EPS/ 1/RM/33 and Chironomus riparies in EPS/1/RM/32.
Sediments tests can be used to determine the relationship between toxic effects and
bioavailabihty, investigate interactions among chemicals, compare the sensitivities of
different organisms, determine spatial and temporal distribution of contamination,
evaluate hazards of dredged material, measure toxicity as part of product licensing or
safety testing, rank areas for clean up and estimate the effectiveness of remediation
or management practices.
Amphipods and midges are commonly used as appropriate test species to determine
acute toxicity because they are relatively sensitive to contaminants associated with
sediments, they have a short generation time, they have lots of contact with the
sediment (i.e., they are both deposit-feeders and burrowers). they are relatively easy
to culture in the laboratory and they tolerate varying physico-chemical characteristics
of sediment.
Both the amphipod and midges are considered benchmark organisms by the USEPA
and USACE Inland Testing Manual Standards (1998) and testing data comprise a
substantial database. The organisms represent the sensitive range in a variety of
ecosystems. These organisms provide comparative data on the relative sensitivity of
local test species.
The amphipod, Hyallela azteca, can also be used for estuanne toxicity studies; they
are tolerant to salinities up to 25ppt.
Please note the list of general limitatbns for all solid-phase toxicity tests in the
introduction to this section.
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Fact Sheet No.
Reference
Website
2.2.3-4 (contd.)
USEPA. 2000d. Methods for Measuring the Toxicity and Bioaccumulaton of
Sediment-Associated Contaminants with Freshwater Invertebrates. EPA/600/R-
99/064. Office of Science and Technology, U.S. Environmental Protection Agency,
Washington, D.C.
http //www eoa oov/waterscience/cs/freshmanua
|_pdf
Last Accessed1 1/31/2003
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.2.3-5
Chronic Freshwater Am phipod Sediment Bioassay. EPA Method 100.4
This test measures the survival, growth and reproduction of the freshwater
crustacean, Hyalella azteca, after exposure to sediments for 42 days in the
laboratory.
The freshwater invertebrate, Hyalella azteca, is exposed to sediments for 42-d ays in
a 300 ml container containing 100 ml of sediment and 175 ml of overlying water.
Test temperature is 23 +/- 1°C. 100 ml of overlying water will be renewed every 12
hours. The organisms are fed daily. The endpoints are 28-day survival and growth,
35-day survival and reproduction; and 42-day survival, growth and reproducton.
Survival is measured by counting the number of alive vs. dead amphipods at 28, 35
and 42 days. Reproduction is measured by exposing amphipods up until a few days
before the release of the first brood. The amphipods are then sieved from the
sediment and held in water to determine the number of young produced. Length
and weight are measured to provide data for the growth end point.
This is a laboratory method for determining the chronic toxicity of contaminants
associated with sediments collected from freshwater environments.
The amphipod, Hyaltela azteca, is considered benchmark organism by the USEPA
and USAGE Inland Testing Manual Standards (1998) and testing data comprise a
substantial database. The amphipod sensitivity corresponds to the sensitive range
in a variety of ecosystems. This organism provide comparative data on the relative
sensitivity of local test species.
The methodology recommended for measuring reproduction may not be accurate;
the amphipods may recover from effects of sediment exposure during the holding
period in clean water.
Please note the list of general limitations for all solid-phase toxicity tests in the
introduction to this section.
USEPA. 2000d. Methods for Measuring the Toxicity and Bioaccumulaton of
Sediment-Associated Contaminants with Freshwater Invertebrates, EPA/600/R-
99/064. Office of Water, U.S. Environmental Protection Agency, Washington, D.C.
httpV/www epa gov/waterscience/cs/freshman
ual pdf
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Reference
Website
2.2.3-6
Life-Cycle Freshwater Midge Sediment Bioassay, EPA Method 100.5
This test measures the survival, growth and reproduction characteristics of the
freshwater midge, Chironomus tentans, after exposure to sediments for 40 or 50
days in the laboratory.
Chironomus tentans, a freshwater invertebrate, is exposed to sediments for up to 60
days in a 300 ml beaker containing 100 ml of sediment and 175 ml of overlying
water. Test temperature is 23 +/- 1 "C. The endpoints are 20-day and end of test
(50-60 days) survival, 20-day growth, and reproduction is monitored daily after day
23, examining endpoints such as emergence of adults, egg number and hatchlmg
success.
The end of the life-cycle test depends upon the sediments being evaluated. In clean
sediments, the test typically requires 40 to 50 d from initial setup to completion.
However, test duration will increase in the presence of environmental stressors
which act to reduce growth or delay emergence. Where a strong gradient of
sediment contamination exists, emergence patterns between treatments will likely
become asynchronous, in which case each treatment needs to be ended separately.
This is a laboratory method for determining the chronic toxicity of contaminants
associated with sediments collected from freshwater environments.
C. tentans is a good candidate for long-term toxicity testing because it has a short
life cycle and a variety of developmental (growth, survivorship) and reproductivity
(fecundity) endpoints can be monitored.
The midge, C. tenlans, is considered a benchmark species by the USEPA and
USAGE Inland Testing Manual Standards (1998) and midge testing data form a
substanSal database Midge sensitivity is in the range of a many ecosystems, and
midges provide comparative data on the relative sensitivity of local test species.
They are burrowers and deposit-feeders.
Please note the list of general limitations for all solid-phase toxicity tests in the
Introduction to this section.
USEPA 2000d. Methods for Measuring the Toxicity and Bioaccumulabon of
Sediment-associated Contaminants with Freshwater Invertebrates, EPA/6007R-
99/064. Office of Water, U.S. Environmental Protection Agency, Washington, D.C.
http //www eoa qov/waterscience/cs/freshmanu Last Accessed: 1/31/2003
alpdf
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Advantages
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Reference
Website
2.2.3-7
Acute Larval Bivalve Sediment Bioassay
This test measures the survival of the marine bivalve larvae. Crassosfrea g/gas, and
Mytilus edulis, after exposure to sediments for 48 hours in the laboratory.
Adult bivalves, conditoned as necessary in the laboratory, are induced to spawn
with selected thermal and biological (i.e., sperm) stimulation. Selected densities of
the resulting embryos are exposed to the test or reference area sediments for 48
hours, during which the embryos normally will develop into prodtssoconch I larvae.
Exposure time should not exceed 60 hours for an acceptable test. Toxicity test
endpoints are based on abnormal shell development and larval death.
This toxicity test can be used to assess the toxicity of marine sediments, especially
dredged material. It may be used alone as a screening tool or in combination with
sediment chemistry and in situ biological indices, and in laboratory experiments
addressing a variety of sediment and water quality manipulations. These sediment
bivalve bioassays are performed as a part of the Dredged Material Evaluation and
Disposal Procedures in the Puget Sound (Puget Sound Dredged Disposal Analysis
(PSDDA) Program, 2000).
Refer to table 2.2.3-1 to compare alternative methods for acute sediment bioassays.
Data from tests with longer exposures (> 48 hours) may not be comparable to those
tests conducted using the standard 48-hour exposure.
Please note the list of general limitations for all solid-phase toxicity tests in the
introduction to this section.
PSWQAT. 1997. Recommended Guidelines for Sampling Marine Sediment, Water
Column, and Tissue in Puget Sound, Puget Sound Protocols and Guidelines. Puget
Sound Water Quality Action Team, Olympia, WA.
http //www.psat wa gov/Publicat Last Accessed: 1/31/2003
lons/orotocols/Drotocol odfs/field odf
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2.2.3-8
Acute Echmoderm Sediment Bioassay
This test measures the survival of the marine echinoderms, Dendraster excentricus,
Strongybcentrotus purpuratus and S. Droebachiensis, after exposure to sediments
for 48-96 hours in the laboratory.
Adult Echinoderms, Dendraster excentricus, Strongylocentrotus purpuratus and S.
droebachiensis, are induced to spawn with chemical stimulation. The resulting
embryos are exposed to test sediment for 48 to 96 hours during which the embryos
will devebp into the four-armed pluteus stage. The toxicity test endpomt is based on
failure to develop normal pluteus larvae. These sediment echinoderm bioassays are
performed as a part of the Dredged Material Evaluation and Disposal Procedures in
the Puget Sound. (USACE/WDNR/WDEC. 2000)
This toxicity test can be used to assess the toxicity of marine sediments, particularly
dredged material. It may be used alone as a screening tool or in combination with
sediment chemistry and in situ biological indices, and in laboratory experiments
addressing a variety of sediment and water quality manipulations.
Refer to table 2.2.3-1 to compare alternative methods for acute sediment bioassays.
The three species may show different levels of sensitivity; therefore, the results for
corresponding end points may not be comparable between the three species.
Please note the list of general limitations for all solid-phase toxicity tests in the
introduction to this section.
PSWQAT. 1997. Recommended Guidelines for Sampling Marine Sediment, Water
Column, and Tissue in Puget Sound. Puget Sound Protocols and Guidelines. Puget
Sound Water Quality Action Team, Olympia, WA.
http Mvww psat wa qov/Publications/pro Last Accessed 1/31/2003
tocols/orolocol odfs/field odf
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2.2.3-9
Acute Marine Crustacean Sediment Bioassay
This test measures survival of the marine mysid shrimp, Mysidopsis bahia and the
marine penaeid shrimp, Penaeus sp., after a 96-hour exposure to sediments in the
laboratory.
The mysid shrimp, Mysidopsis bahia, and Penaeid shrimp, Penaeus sp., are
placed in 1-L glass chambers containing 175 mL sediment and about 800 ml of
overlying water for 96-hours. Test temperature 20°C and the recommended
overlying water salinity is 20 ppt. The test chambers will be lightly aerated, but
water will not be renewed. Test species will be fed once daily. The end points in the
toxicity test are survival. Performance criteria established for this test include the
average survival of organisms in negative control treatment must be 2 90%.
A miniaturized method of this test also exists (Ho, 2000) and will be incorporated
into EPA's TIE guidance document.
This test method may be useful in assessing sediment contamination, registration of
pesticides, assessments of new and existing chemicals, Superfund site
assessment, and assessment and cleanup of hazardous waste treatment, storage,
and disposal facilities.
Mysid shnmp are filter- and deposit-feeders commonly found in marine sediments;
therefore, exposure to contaminated sediments is likely. Penaeid shrimp are
deposit-feeders and burrowers, so they are also likely exposed to contaminants
through there feeding regime. Mysid shrimp tolerate a wide range of salinities.
Amphipod crustaceans are more commonly used for short term sediment
bioassays. They are considered benchmark species by the USEPA and USACE
Inland Testing Manual (1998) in that they comprise a substantial database,
represent the sensitive range of a variety of ecosystems, and provide comparative
data on the relative sensitivity of local test species.
Please note the list of general limitations for all solid-phase toxicity tests in the
introduction to this section.
USEPA. 1995. Environmental Monitoring and Assessment Program Laboratory
Methods Manual, Estuaries, Volume 1-Biologicaland Chemical Analyses,
EPA/620/R-95/008. Environmental Monitoring and Assessment Program , U.S.
Environmental Protection Agency, Washington DC.
http //www epa gov/emap/html/pubs/doc
s/arouodocs/estuarv/field/lab man odf
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Method Title
Acute Marine Amphipod Crustacean Sediment Bioassay, EPA Method 100.4
Purpose
This test measures the survival of the marine amphipod crustaceans, Ampelisca
abdiia, Eohaustorius estuarius, Leptocheirus plumulosus or Rhepoxynius abronius,
after exposure to sediments for 10 days in the laboratory.
Method Summary
Infaunal amphipods. Ampelisca abdita, Eohaustorius estuarius, Leptochefrus
plumulosus and Rhepoxynius abronius are used in toxicity studies assessing
sediments from marine and estuarine environments. The toxicity test is conducted for
10 d in 1-L glass chambers containing 175 ml sediment and about 800 mL of
overlying water. Test temperature is 15"C for E. estuarius. 20°C for A. Abdita and
25°C for L. plumulosus, and the recommended overlying water salinity is 20 ppt for
E. estuarius and L plumulosus and 28 ppt for A. abdita and R. abronius. There will
be no feeding during the test and no renewal of overlying water. The endpoints in the
toxicity test are survival of amphipods. Performance criteria established for this test
include the average survival of amphipods in negative control treatment must be a
90%.
The Rhepoxynius abronius is the preferred species for coarser-grained sediments
(I e.r fines <60%) with a salinities >25 ppl. The Ampelisca abdita may be used when
test sediment contains > 60% fines and in a wide range of salinities. The
Eohaustorius estuarius may be used when grain size ranges from 0.6 % sand to
100% sand and salinities range from 1 ppt to 25 ppt.
Puget Sound Dredged Disposal Analysis Program (USACE/WDNR/WDEC, 2000)
also recommends a similar 10-day acute toxicity test with the marine amphipods,
Ampelisca abdita, Eohaustorius estuarius, and Rhepoxynius abronius. ASTM E1367
and NHEERL-AED SOP 1.03.002 also describe methods for sedimenl bioassays
with amphipods (ASTM, 2001b and USEPA and Naval Construction Battalion
Center. 1992, respectively).
A miniaturized method of this test also exists (Ho, 2000) and will be incorporated into
EPA's TIE guidance document. __
Data
Uses/Applicabon
This is a sediment toxicity method used to evaluate the effects (reduction in survival)
of marine and estuarine sediments on the marine amphipods. The test method may
be useful in assessing sediment contamination, registration of pesticides.
assessments of new and existing chemicals, Superfund site assessment, and
assessment and cleanup of hazardous waste treatment, storage, and disposal
facilities
The choice of these amphipod species as test organisms is based on sensitivity to
sediment-associated contaminants, availability and ease of collection, tolerance of
environmental conditions (e.g., temperature, salinity, grain-size), ecological
importance, and ease of handling in the laboratory. Either alone or in combination
they may be used to measure toxicity of any commonly encountered marine
sediment.
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2.2.3-10 (contd.)
Amphipods are among the first taxa to disappear from benthic communities impacted
by pollution, and have been shown to be more sensitive to contaminated sediments
than several other major taxa. All of these organisms are considered benchmark
species by the USEPA and USAGE'S Inland Testing Manual (1998) indicating that
they comprise a substantial database, represent the sensitive range of a variety of
ecosystems, and provide comparative data on the relative sensitivity of local test
species.
Please note the list of general limitations for all solid-phase toxicity tests in the
introduction to this section.
USEPA. 1994d. Methods for Assessing the Toxicity of Sediment-Associated
Contaminants with Estuarine and Marine Amphipods. EPA/600/R-94/025. Office of
Research and Development, U.S. Environmental Protection Agency, Washington,
D.C.
htto //www eDa.qov/waterscience/cs/freshmanua
Lpdf
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Advantages
Limitations
Reference
Website
2.2.3-11
Acute Marine Polychaete Sediment Bioassay. ASTM Method E1 61 1-00
This test measures the survival of the marine polychaetes, Neanthes
arenaceodentata and Neanthes virens, after exposure to sediments for 10 days in
the laboratory.
Infaunal polychaetes Neanthes arenaceodentata and Neanthes virens are used in
toxicity studies assessing sediments from marine and estuarine environments. The
toxicity test is conducted for 10 d in 1-L glass chambers with a sediment depth of 2
to 3 cm and aerated overlying water. Water is not renewed during the 10-day
exposure and there is no feeding. The end points in the toxicity test is survival of
polychaetes.
A negative control or reference sediment is used to give a measure of acceptability of
the test.
A similar method using the test species Polydora cornuta is described in
Environment Canada's method EPS/1 /RM/41
This is a sediment toxicity method used to evaluate the acute effects (reduction in
survival ) of marine and estuarine sediments on polychates. Polychaetes are an
important component of the benthic community and are sensitive to both organic and
inorganic chemicals. The results of this acute toxicity test can be used to predict
temporal or spatial distribution of sediment toxicity. The test method may be useful in
assessing sediment contamination, registration of pesticides, assessments of new
and existing chemicals, Superfund site assessment, and assessment and cleanup of
hazardous waste treatment, storage, and disposal facilities.
Polychaetes are burrowers and deposit-feeders; therefore, contaminant exposure is
likely.
A 10-day test provides data on the short-term effects that may be useful for
comparisons to other species but does not provide information on delayed effects.
Polychaetes are not considered benchmark species (USEPA and USAGE, 1998).
Please note the list of general limitations for all solid-phase toxicity tests in the
introduction to this section.
ASTM 2001 b. ASTM Book of Standards. Volume 1 1 .05. American Society for
Testing and Materials, West Conshocken, PA.
N/A
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2.2.3-12
Chronic Estuarine Amphipod Sediment Bioassay
This test measures the growth and reproduction of the estuarine amphipod
crustacean, Leptocheirus plumulosus, after exposure to sediments for 28 days in the
laboratory.
This is a laboratory method for determining the chronic toxicity of contaminants
associated with whole sediments collected from estuarine or marine environments
(or estuarine or marine sediment spiked with compounds in the laboratory). The
toxicity method uses an estuarine crustacean, the amphipod, Leptocheirus
plumulosus. The toxicity test is conducted for 28 d in 1-L glass chambers containing
175 mL sediment and about 725 ml of overlying water. Test temperature is 25° ± 2',
and the recommended overlying water salinity is 5 ppt ± 2ppt (for test sediment with
pore water at 1 ppt to 10 ppt) or 20 ppt ± 2 ppt (for test sediment with pore water >10
ppt). 400 mL of overlying water is renewed three times a week, at which times test
organisms are fed. The endpoints in the toxicity test are survival, growth, and
reproduction of amphipods. Performance criteria established for this test are that the
average survival of amphipods in negative control treatment must be a 80% and
there must be measurable growth and reproduction in all replicates of the negative
control treatment.
This is a sediment toxicity method used to evaluate the sublethal effects (reduction in
growth and reproduction) of marine and estuanne sediments on the marine
amphipod, Leptocheirus plumulosus. The test method may be useful in assessing
sediment contamination, registration of pesticides, assessments of new and existing
chemicals, Superfund site assessment, and assessment and cleanup of hazardous
waste treatment, storage, and disposal facilities.
The marine amphipod, Leptocheirus plumulosus, is considered a benchmark species
which means that they comprise a substantial database, represent the sensitive
range of a variety of ecosystems, and provide comparative data on the relative
sensitivity of local test species. This organisms is a deposit-feeder and burrower
therefore exposure to sediment contaminants will occur through its feeding regime.
The test is applicable for use with sediments from oligohaline to fully marine
environments, with a silt content greater than 5% and a clay content less than 85%.
Please note the list of general limitations for all solid-phase toxicity tests in the
introduction to this section.
USEPA. 2001 e. Method for Assessing the Chronic Toxicity of Marine and Estuarine
Sediment-associated Contaminants with the Amphipod Leptocheirus plumulosus,
EPA 600/R-01/D20. Office of Research and Development, U.S. Environmental
Protecbon Agency, Washington, D.C.
http //www epa gov/waterscience/cs/guid Last Accessed: 1/31/2003
ancemanual odf
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Advantages
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Reference
Website
2.2.3-13
Chronic Marine Polychaete Sediment Bioassay, ASTM Method E1 611-00
This test measures the growth and reproduction of the marine polychaete, Neanthes
arenaceodentata, after exposure to sediments for 28 days in the laboratory.
This is a laboratory method for determining the chronic toxicity of contaminants
associated with whole sediments collected from estuarine or marine environments
(or estuanne or marine sediment spiked with compounds in the laboratory). The
toxicity method uses an estuarine polychaete, Neanthes arenaceodentata. The
toxicity test is-conducted for 28 d in 1-L glass chambers containing 2-3 cm of
sediment and aerated overlying water. This is a static renewal toxicity test and the
organisms are fed daily. The endpoints in the toxicity test are survival, growth, and
reproduction of amphipods. Performance criteria established for this test include the
average survival of amphipods in negative control treatment must be * 80% and
there must be measurable growth and reproduction in all replicates of the negative
control treatment.
Puget Sound protocols and guidelines recommend a juvenile polychaete bioassay
with a 20-day exposure time. Endpoints are mortality, total biomass, and average
individual biomass. It is a static renewal assay and organisms are fed.
This is a sediment toxicity method used to evaluate the sublethal effects (reduction in
growth and reproduction) of marine and estuarine sediments on the marine
polychates. The test method may be useful in assessing sediment contamination,
registration of pesticides, assessments of new and existing chemicals, Superfund
site assessment, and assessment and cleanup of hazardous waste treatment,
storage, and disposal facilities.
This type of worm is a deposit-feeder and burrower, therefore exposure to sediment
contaminants is likely through the feeding regime.
This organism is not considered a benchmark species (USEPA and USAGE, 1998).
The protocol may have to be modified for tests at salinities less than 20 ppt.
Please note the list of general limitations for all solid-phase toxicity tests in the
introduction to this section.
ASTM. 2001 b. ASTM Book of Standards. Volume 1 1 .05. American Society for
Testing and Materials, West Conshocken, PA.
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2.2.3-14
Ames Mutagenicity Assay
This test can be used to determine if a sample is mutagenic or cancer-causing. It
uses the induced reversion of bacterial mutants to detect DNA-damaging
substances.
Sediment samples are dried with anhydrous sodium sulfate, extracted with
methylene chloride, subjected to gel-permeation chromatography cleanup,
evaporated under nitrogen, and brought to volume in DMSO.
The Ames assay uses 100uL of cultured test strain (Salmonella typhimurium). 500 uL
of either phosphate buffer, and 100uL of (he sediment extract or DMSO mixture
(control). The entire mixture is incubated for 20 to 30 minutes in a dry block heater.
Following incubation, top agar is added containing trace histidine and biotin and the
mixture is poured into plates. Plates are then incubated and the resulting colonies
are counted at 72 hours.
A positive mutagenic response is indicated when the number of revertants on test
plates are greater than or equal to 2 times the number of colonies in the DMSO
solvent control plate.
Short-term bioassays generally identify specific genotoxic contaminants or those in
complex mixtures of contaminants, provide baseline data for monitoring changes in
environmental conditions, and predict potential long range genotoxic health effects.
The Ames test is relatively quick and inexpensive. It is useful for establishing
priorities for more definitive chemical analysis or lexicological testing.
Some chemicals that are mutagenic/carcmogenic, do not give a positive Ames Test
(/' e., dioxin). Because the strain of salmonella used is histidine negative, the test
may also give false positives if histidine is present in environmental samples.
Please note the list of general limitations for all solid-phase toxicity tests in the
introduction to this section.
USEPA. 1993b. Assessment and Remediation of Contaminated Sediments (ARCS)
Program: Biological and Chemical Assessment of Contaminated Great Lakes
Sediment. EPA 905-R93-006. Great Lakes National Program Office. U.S.
Environmental Protection Agency, Chicago, IL.
hltp-//www epa qov/qlnpo/arcs/EPA-905-
R93-006/EPA-905-R93-006 html
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Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
Website
2.2.3-15
Mutatox Genotoxicity Assay
This test can be used to determine if a sample is mutagenic or cancer-causing. It
uses the induced reversion of bacterial mutants to detect DMA-damaging
substances.
Sediment samples are dried with anhydrous sodium sulfate, extracted with
methytene chloride, subjected to gel-permeation chromatography cleanup,
evaporated under nitrogen, and brought to volume in DMSO.
The Mutatox assay uses rat liver S9 for exogenous metabolic activation of
progenotoxins and a dark mutant strain of the luminescent bacterium Photobacterium
phosphoreium for detection of genotoxins. DNA-damaging substances are detected
by measuring the ability of a test extract or specific chemical to restore the
luminescent state in the bacterial cells. The degree of light increase indicates the
relative genotoxicy of the sample. •
Short-term bioassays generally identify specific genotoxic contaminants or those in
complex mixtures of contaminants, provide baseline data for monitoring changes in
environmental conditions, and predict potential long range genotoxic health effects.
The test is relatively quick and inexpensive. It is useful for establishing priorities for
more definitive chemical analysis.
Comparative data may be limited.
Please note the list of general limitations for all solid-phase toxicity tests in the
introduction to this section.
USEPA. 1993b. Assessment and Remediation of Contaminated Sediments (ARCS)
Program: Biological and Chemical Assessment of Contaminated Great Lakes
Sediment, EPA 905-R93-006. Great Lakes National Program, U.S. Environmental
Protection Agency, Chicago, IL.
htlp //www epa gov/qlnpo/arcs/EPA-905-
R93-006/EPA-905-R93-006 html
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Method Title
V79 Sister Chromatid Exchange Assay, NHEERL-AED SOP 1.03.012
Purpose
These methods describes a test used to evaluate mutagenic effects of single
compounds and complex mixtures, including sediment extracts and their fractions.
Method Summary
The Sister Chromatid Exchange (SCE) first requires the preparation of media that is
used for plating, dosing and media change procedures. The media is then divided
and applied to toxicity plates and SCE plates. Cell suspensions are prepared and
then added to appropriate vials in a 1:10 dilution ratio. The number of cells per mL
in the cell suspensions are determined using a hemocytometer. Cell suspension
dilutions are then added to the toxicity plates and the SCE plates. These plates are
then incubated for 24 hours to allow for cell attachment.
Following incubation, media and solvents are mixed to prepare a dosed medium that
is then added to both the toxicity plates and the SCE plates: the toxicity plates
receive a minimum of 3 ml of dosed media and the SCE plates receive a minimum
of 7 ml of dosed media. The plates are then incubated for 5 hours. Media is renewed
with "clean media" on the toxicity plates and then the plates are returned to the
incubator for 6 days. The media is changed again and the plates are incubated for
20 hours.
Cells are harvested from both the toxicity plates and the SCE plates and slides are
made. On the toxicity slides, the number of colonies are counted. The SCE slides
are scanned for suitable chromosome spreads. The number of chromosomes and
the number of SCEs per spread are recorded, along with other observations.
Data
Uses/Application
The SCE Assay is commonly used to determine genetic damage and mutational
events by cytogenetic analysis.
The mean colony per dose determined on the toxicity test slides is used to find the
percent survival of a dose as compared to the control or blank for that test. The
number of SCE/number of chromosomes is evaluated statistically to find the mean
per dose which is compared to the control or blank for that test.
Advantages
The assay has been used to evaluate effects of single compounds (i.e., mitocmycin
C, benzo(a)pyrene) and to evaluate whole sediment extracts and sediment fractions
from sites with known contaminated sediment problems.
Limitations
The tests need to be monitored daily since contamination will skew the results. Any
contaminated plates should be removed, taped with autoclave masking tape,
wrapped in foil, and autoclaved.
There may also be problems with chromosome, staining and spreading quality.
Please note the list of general limitations for all solid-phase toxicity tests in the
introduction to this section.
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Website
2.2 3-16 (contd.)
USEPA and the Naval Construction Battalion Center. 1992. Standard Operating
Procedures and Field Methods Used for Conducting Ecological Risk Assessment
Case Studies. Technical Document 2296, Naval Command, Control and Ocean
Surveillance Center, RDT&E Division, San Diego, CA.
http //www duxburv battelle orq/compend
lum/methods/NHEERL-AED-SOP-
1.03 012 odf
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2.2.3-17
Method Title
Bioaccumulation Test for Marine, Estuarine and Freshwater Sediments, EPA Method
100.3
Purpose
This test measures bioaccumulation in the freshwater Lumbriculus variegatus after
exposure to sediments for 28 days in the laboratory.
Method Summary
The Lumbriculus variegatus is exposed to sediments for 28-days in a 4 to 6 L
container containing 1 to 2 L of sediment and 1 to 4 L of overlying water. Test
temperature is 23 +/-1 °C. 1 L of overlying water will be renewed every 12 hours.
No supplemental food will be added during the experiment. The endpoint is
bioaccumulation.
In some cases, body burdens will not approach steady-state body burdens in a 28-d
test (e.g., organic compounds with a log Kow >5, be metabolically refractory, or have
low depuaration rates). Depending on the goals of the study and the adaptability of
the test species to long-term testing, it may be necessary to conduct an exposure
longer than 28-d (or a kinetic study) to obtain a sufficiently accurate estimate of
steady-state tissue residues of these compounds. Use of long-term tests or
toxicokinetic approaches is recommended specifically for slowly accumulated
compounds and for a greater than 80 percent accuracy in test species achieving
steady state.
ASTM also provides guidance for bioaccumulabon tests with marine test species
such as the polvchaetes, Nereis dlverslcotor, Neanthes wrens and the bivalve
Macoma nasuta, Macoma batthica, and Yoldia limatula (ASTM Method E1688;
ASTM 2001 b), and freshwater test species such as the Diproeia spp and
Lumbriculus variegates. They recommend selecting at least one species
representing filter-feeding, deposit-feeding and burrowing species.
Data
Uses/Application*
This is a laboratory method for determining the bioaccumulation of contaminants
associated with sediments collected from freshwater environments. The data are
sometimes multiplied by an adjustment factor to accommodate for different steady-
state rates with different contaminant mixtures.
Data from bioaccumulation tests are used to derive bioaccumulation factors (BAFS)
and to determine biota-sediment accumulation factors (BSAFS) in equilibrium
partitioning models.
Bioaccumulation data is needed in ecological or human health risk assessments,
therefore the procedures are designed to generate quantitative estimates of steady-
state tissue residues. These tests are also used to assist in the development of
sediment quality criteria and to assess the potental impacts of disposal of dredged
materials. Biota-sediment accumulation factors (BSAFS) are often compared
between laboratory-exposed and field-exposed organisms to determine the validity of
laboratory experiments and to better predict contaminant-specific lipid partitioning
tendencies.
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2.2.3-1 7 (contd.)
Previous bioaccumulatoon tests used 10-day exposures. A 28-day exposure is a
practical compromise between cost, data accuracy and data utility. Observed
steady-state tissue levels were reached in 28-days in 69% of the tests. The data
should be sufficiently accurate for quantitative risk analysis in most cases. In cases
in which more accurate estimates are required, either a long-term exposure or an
alternative approach can be used.
Additional research is needed on the standardization of bioaccumulation procedures
with sediment. Steady-state is reached at different times with different contaminants,
thus 28-day is an approximate period of time that may prove inaccurate with the
wrong mixture of contaminants.
Specifically, the 28-day time period appears to underestimate steady-state of DDT
and dieldrin, so it may be necessary to use adjustment factors for sites with
significant DDT and dieldrin concentrations.
Please note the list of general limitations for all solid-phase toxicity tests in the
introduction to this section.
USEPA. 2000a. Bioaccumulation Testing and Interpretation for the Purpose of
Sediment Quality Assessment: Status and Needs, EPA 823-R-00-001. Office of
Water and Office of Solid Waste, U.S. Environmental Protection Agency,
Washington, DC.
http//www epa qov/clanton/clhtml/Dubtitl
eOW html
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2.3 Biota
The health and community structure of endemic-organisms are often evaluated in order to assess
the impacts of chemical contamination on the environment. At Superfund sites containing
contaminated sediments, phytoplankton, zooplankton, benthic invertebrates and fish can all be
monitored. These organisms can potentially be exposed to contaminant stressors via ingestion
pathways or direct contact/absorption from the water column. Therefore, they are collected either
for identification and enumeration analyses to determine community structure or they are collected
for chemical tissue analyses to investigate contaminant uptake, bioaccumulation and potential
biomagnification in the food chain.
There are three common approaches to evaluating environmental risk to receptors: 1) the use of
literature screening values; 2) a "desk-top" risk assessment that can model existing site-specific
contaminant data to ecological receptors for subsequent comparison to literature toxteity values; or
3) field investigation/laboratory analysis that involves a site investigation and laboratory analysis of
contaminant levels in media and/or experimentation using bioassay procedures (USEPA, 1997a).
The methods provided in the following section provide a summary of those methods that would be
used in the third approach: field investigation and laboratory analyses. These fact sheets intend to
provide Superfund managers with a summary of the existing methods that may be applicable to
their site, the method's relative strengths, and the method's relative weaknesses. These analyses
will help to determine the relationship between the exposure of a contaminant and the response it
elicits.
2.3.1 Chemical and Physical Analyses
Section 2.3.1 presents field sample collection and processing methods for biota. Biota are
collected at Superfund sites for chemical residue studies, population/community studies, and
toxicity testing/bioassays; all directed at assessing exposure-response relationships at the site
(USEPA, 1997a). Methods are provided for sample collection and processing of phytoplankton.
zooplankton, periphyton, benthic invertebrates and fish. Biota methods were predominantly
gathered from the following sources:
• The USEPA's Office of Water
• The USEPA's EMAP program
• The USEPA's Great Lakes Program
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2.3.1-1
Phytoplankton Sample Collection and Preservation in the Great Lakes, LMMB 023t
This method describes the collection and preservation of phytoplankton samples for
community analyses
Water samples are collected using a Rosette sampler (see Fact Sheet 2.1.1-6). 1L
aliquots from each discrete sampling depth are composited, and approximately 1 L of
the composite sample is transferred to a sample bottle. The sample is preserved
with Lugol's Solution for analysis (final concentration 1%). Samples are stored in the
dark and refrigerated.
Phytoplankton community analyses are useful for bioassessments to determine
community disturbance as a result of contamination.
One of few standard methods for water column bioassessment
This collection method ts not suitable for chlorophyll a or productivity measurements.
Populations of phytoplankton are seasonal and highly variable. Use of one or more
reference stations is essential.
USEPA. 1997b. Method LMMB 023: Standard Operating Procedure for
Phytoplankton Sample Collection and Preservation. Lake Michigan Mass Balance
Study Methods Compendium, Volume V Sample Collection Techniques, EPA 9Q5-R-
97-01 2c. Great Lakes National Program Office, U.S. Environmental Protection
Agency, Chicago, IL.
http //www epa qov/glnpo/lmmb/methods/phyt Last Accessed: 1/31C003
ocol odf
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Purpose
Method Summary
Data
Uses/ Application
Advantages
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Reference
Website
2.3.1-2
Chlorophyll-a Sampling Method and Preservation: Field Procedure in the Great
Lakes, LMMB015
This method is used to filter chlorophyll-a samples.
Water samples are collected using Niskin bottles or other suitable sampling device.
The water samples are transferred from the Niskin bottles to opaque sample bottles
for storage. The water sample for chlorophyll-a analysis is vacuum filtered through a
47 mm diameter glass fiber filter (see Fact Sheet 2.3.1-3). The entire procedure is
conducted in subdued (green) light to prevent photodecomposition. During filtration,
the samples are treated with a solution of MgC03 to prevent acid induced
transformation of chlorophyll to its degradation product, Phaeophytin. Sample filters
are stored in aluminum foil pouches and frozen until analysis.
Often used as a surrogate for productivity or standing crop measurements,
chlorophyll a measurements are also used to monitor plankton blooms. Also used to
calibrate SeaWiFS or other remote sensing images.
Simple collection, extraction, and analysis methods albw economical spatial and
temporal variations to be monitored.
Filters must be extracted and analyzed within 28 days.
USEPA. 1997b. Method LMMB 015: Standard Operating Procedure for Chlorophyll-
a Sampling Method: Field Procedure. Lake Michigan Mass Balance Study Methods
Compendium, Volume 1: Sample Collection Techniques. EPA 905-R-97-01 2c. Great
Lakes National Program Office, U.S. Environmental Protection Agency, Chicago, IL.
htto //www eoa qov/qlnDO/lmmb/methods/chlf Last Accessed: 1/31/2003
ield.pdf
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Method Summary
'Data
Uses/Application
Advantages
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Reference
Website
2.3.1-3
Chlorophyll a and Phaeophytin Field Filtering Protocols
This method describes the methods used for the immediate processing of water
samples analyzed for Chlorophyll a and Phaeophytin.
Chlorophyll a and Phaeophytin samples must be filtered no more than 4 hours after
collection. Samples that cannot be filtered immediately after collection must be held
at 4°C until filtered. Filtering can be accomplished by the use of a vacuum pump or
by using positive pressure, as described below
Vacuum Filtration: Filter the water onto two 47 mm diameter glass fiber filter pads.
Do not exceed a vacuum of 15 psi or a filtration duration of greater than 5 minutes.
Add 1 ml of saturated MgC03 solution during the last few seconds of filtering after
the nutrient filtrate has been removed.
Record the volume filtered on the data sheet. The filtrate should be saved for
dissolved nutrient analyses. Approximately 40 mL of filtrate will be collected into a
pre-labeled, clean 60 mL Nalgene screw-capped bottle and stored on dry ice.
Carefully remove the filters using forceps, fold in half, and wrap in aluminum foil.
Label the samples and place package on dry ice.
Positive Pressure: The alternative method is to use positive pressure to push a
sample through the filter. A disposable, graduated 50-cc polypropylene syringe fitted
with a stainless steel or polypropylene filtering assembly is used to filter the site water
through 25 mm diameter glass fiber filter pads, the volume of water must be
documented. If conditions allow, up to 200 mL of site water should be filtered for
each chlorophyll sample. After filtering, add 1 mL of MgC03 solution to the syringe
and pass through the filter pad. Remove the filter, fold and place in aluminum foil.
Again, approximately 40 mL of filtrate will be collected into a pre-labeled, clean 60 mL
Nalgene screw-capped bottle and stored on dry ice.
Methods LMMB 085 and 086 describe similar filtering protocols (USEPA. 1997b).
Chlorophyll a measurements are indicative of the primary producer's relative
abundance and composition in the water column sample.
Simple collection, extraction, and analysis
temporal variations to be monitored.
methods allow economical spatial and
If filtration cannot occur in under 4 hours, the phytoplankton cells can possibly lyse.
The sample on the filter paper may degrade over time, and must be extracted and
analyzed within 28 days.
USEPA. 2000b. Coastal 2000 Northeast Component: Field Operations Manual,
Environmental Monitoring and Assessment Program (EMAP), EPA/620/R-00/002.
Office of Research and Development, U.S. Environmental Protection Agency,
Washington, DC.
N/A
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2.3.1-4
Primary Productivity Using UC: Field Procedure in the Great Lakes. LMMB 016
This method is used to determine primary productivity and primary productivity
parameters from water.
Water samples are collected using Niskin bottles or other suitable samplers. When
there is a thermal stratification in the water column, samples are collected from both
the hypolimnion and the epiEmnion. The water samples are transferred from the
Niskin bottles to opaque sample bottles for storage in a light-tight, insulated
container.
The following procedures are conducted in subdued {green) light to avoid
photodegradation. Water samples are carefully transferred to incubation bottles.
Water samples are inoculated with a known quantity of bircarbonate substrate, which
is labeled with the radiotracer 14C. Samples are incubated at various light intensities
for 2 - 4 hours. After incubation, a 100 mL aliquot of each sample is filtered through a
47 mm cellulose acetate filter (0.45 urn pore size). The filter is placed into a
scintillation vial and 0.5 N HCI is added. The vials sit at room temperature for 1 hour.
20 mL of liquid scintillation cocktail is added to each vial. The vials are stored until
they are analyzed by liquid scintillation counting to determine the quantity of carbon
fixed by the algae into organic matter.
Primary productivity is a key measurement in many site assessments, particularly
those affected with nutrient enrichment.
This method is the standard for productivity determination.
Use of >4C requires NRC License. Disposal of 14C waste is often problematic.
USEPA. 1997b. Method LMMB 016: Standard Operating Procedure for Primary
Productivity Using 14C: Field Procedure. Lake Michigan Mass Balance Study
Methods Compendium, Volume 1: Sample Collection Techniques. EPA905-R-97-
01 2c. Great Lakes National Program Office. U.S. Environmental Protection Agency,
Chicago, IL.
http //www epa aov/alnpo/lmmb/methods/c14 Last Accessed: 1/31/2003
field^df
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2.3.1-5
Zooplankton Sample Collection and Preservation in the Great Lakes, LMMB 024
This method describes the collection and preservation of zooplankton samples for
community analyses.
Water samples are collected using a plankton tow net that is maneuvered using a
winch on the starboard side of the vessel. The tow net has a flow meter and
screened sample bucket attached to the end. The flow meter should be calibrated
every survey season. For sampling, the net is lowered to the desired depth (usually
20 meters from the water surface) and raised at a constant slow speed until the rim is
above the water. In shallower waters, the samples are usually collected from 1 meter
above the bottom to the surface. The net is then lifted out of the water and rinsed
from the outside to free organisms from the side of the net, concentrating them into
the sample bucket. The sample bucket is removed, and the sample is rinsed into a
sample container. The organisms are then narcotized with 20 mL of soda water and
left to sit for 30 minutes. The samples are preserved with 20 mL of formalin solution.
Tow nets survey the biological community by collecting abundance and taxa
composition data from sampling locations. They are often used to gam information
on particular species of larval fish and an overall estimation of fish populations and
communities. Fish population and community data are used to measure the status
and trends of environmental pollution freshwater, estuarine and marine organisms to
assess water quality criteria and to monitor surface water quality.
The tow net is easy to handle and it is small enough for use on boats 4 m or larger in
length. The design reduces current vibrations in the water directly in front of the net.
Zooplankton populations are highly seasonal and within season can vary spatially
depending upon currents and microclimate. Effective use of reference areas
required.
USEPA. 1997b. Method LMMB 024: Standard Operating Procedure for
Zooplankton Sample Collection and Preservation. Lake Michigan Mass Balance
Study Methods Compendium, Volume 1: Sample Collection Techniques, EPA 905-R-
97-01 2c. Great Lakes National Program Office, U.S. Environmental Protection
Agency, Chicago, IL.
http //www epa qov/qlnpo/lmmb/methods/zoo
fid pdf
Last Accessed' 1/31/2003
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2.3.1-6
Field-based Periphyton Survey in Wadeable Streams
To perform a quick semi-quantitative assessment of algal biomass and taxonomic
composition in the field.
This protocol describes a field-based rapid survey of periphyton biomass and coarse-
level taxonomic composition (e.g.. diatoms, filamentous greens, blue-green algae).
To perform a field-based periphyton survey, the investigator establishes three
transects across the habitat being sampled (preferably riffles or runs in the reach in
which benthic algal accumulation is readily observed and characterized). Three
locations are then selected along each transect. Algae are characterized in each of
the selected locations by immersing a bucket with a 50-dot grid in the water.
Macroalgal biomass and microalgal cover are then determined in the bucket.
EPA's EMAP field document describes similar field-based periphyton surveys
(USEPA, 1998, EPA/620/R-94/004F).
Species relative abundance and taxa richness are data derived from these protocols.
These data parameters provide information pertaining to the status and trends of
environmental pollution and its impacts on freshwater, marine and estuanne
communities.
Biological impairment resulting from pollution is often evaluated using metrics of
biotic integrity derived from the aforementioned data parameters that evaluate
community, population and functbnal parameters. Examples of metrics based on
species composition include species richness, total number of genera, total number
of divisions, shannon diversity (for diatoms), percent community similarity of diatoms,
pollution tolerance index for diatoms, and percent sensitive diatoms. Furthermore,
other metrices infer ecological conditions based on documented preferences. These
metrices include the percent aberrant diatoms, percent motile diatoms, simple
diagnostic metrics, inferred ecological conditions with simple autecological indices
(SAI), inferred ecological conditions with weighted average indices, and impairment
of ecological conditions.
The field-based periphyton survey requires less effort than the laboratory methods. It
is able to assess algal biomass over larger spatial scales than substrate sampling
and laboratory analysis. Coarse-level taxonomic characterization of communities is
also possible with this technique.
The field methods are not as accurate as the laboratory analysis.
Barbour et al. 1999. Rapid Bioassessment Protocols for Use in Streams and
Wadeable Rivers: Periphyton, Benthic Macroinvertebrates and Fish, Second Edition,
EPA 841-B-99-002. Office of Water, U.S. Environmental Protection Agency,
Washington, D.C.
http //www epa qov/owow/monitonnq/rbp/ Last Accessed: 1/31/2003
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Method Summary
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Reference
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2.3.1-7
Laboratory-Based Periphyton Survey: Single Habitat Sampling in Wadeable Streams
To determine the periphyton abundance and composition in area of interests.
Single habitat sampling protocol outlines a procedure for collecting periphyton from a
single substrate/habitat combination that characterizes the study reach. A
preliminary, visual habitat assessment should be performed prior to sample collection
to determine the percent cover of each substrate type and the estimated relative
abundance of organisms.
Collection techniques depend on the substrate type and the dominant periphyton.
Several subsamples should be collected from the same substrate/habitat
combination and composited into a single container. Periphyton samples should be
collected during periods of stable stream flow.
If the samples are going to be assayed for chlorophyll a, the samples should not be
preserved until they have been subsampled. Following subsampling and
preservation ( Lugol's solution, "M3" fixative, buffered 4% formalin. 2%
glutaraldehyde. or other preservative) the samples are transported back to laboratory
on ice.
EPA's EMAP field document describes similar protocols for periphyton surveys in
wadeable streams (USEPA. 1998).
Periphyton can be collected to: 1) determine taxonomic composition and relative
abundance. 2) determine chlorophyll. 3) determine biomass. and 4) determine
acid/alkaline phosphate activity.
Single habitat sampling provides periphyton biomass data.
Variability in habitat differences between streams may be reduced if periphyton
collection is performed from a single substrate/habitat combination.
Spatial variability can lead to samples not being representative of site. Adequate
replication and spatial coverage required.
Barbour et al. 1999. Rapid Bioassessment Protocols for Use in Streams and
Wadeable Rivers: Periphyton, Benthic Macroinvertebrates and Fish. Second Edition.
EPA 841-B-99-002. Office of Water;\\, U.S. Environmental Protection Agency;
Washington, D.C.
hlto //www eoa qov/owow/monitonng/rbD/ Last Accessed: 1/31/2003
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Method Summary
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Advantages
Limitations
Reference
Website
2.3.1-8
Laboratory-Based Rapid Periphyton Survey:
Streams
Multi habitat Sampling in Wadeable
Algae sampling methods for subsequent laboratory assessments of species
composition.
Multi-habitat sampling is a procedure developed to sample periphyton from wadeable
streams. It should be conducted at the reach scale (30-40 stream widths) to ensure
sampling the diversity of habitats that occur in the stream. The protocol first calls for
visual estimates or quantitative transect-based assessments to determine the
percent cover of each substrate type and the estimated relative abundance of
macrophytes, macroscopic filamentous algae, diatoms and other microscopic algal
accumulations, and other biota. Following preliminary investigations, algae are
collected from all available substrates and habitats roughly in proportion to their areal
coverage in the reach. Periphyton samples should be collected during periods of
stable stream flow. Small amounts of subsample (about 5 ml or less) are usually
sufficient. The objective is to collect a single composite sample that is representative
of the periphyton assemblage present in the reach. Collection techniques depend on
the substrate type and the dominant macroinvertebrates. However, this protocol
recommends that specimens of macroalgae be collected by hand in proportion to
their relative abundance in the reach. Samples are combined into single, water-tight,
unbreakable, wide-mouth containers. After adding the appropriate preservative,
(Lugol's soluton. "M3" fixative, buffered 4% formalin. 2% glutaraldehyde, or other
preservative), the samples are transported back to laboratory on ice.
EPA's EMAP field document describes similar protocols for periphyton surveys in
wadeable streams (USEPA, 1998).
Multi-habitat sampling will provide information pertaining to species composition.
Changes in species composition among habitat are often evident as changes in color
and texture of the periphyton. These data provide information pertaining to the
effects of pollution on environmental communities.
Multi habitat sampling can also be conducted to collect periphyton for chlorophyll
determination, biomass determination and acid/alkaline phosphate activity.
The investigators may get a better sense of how habitat changes may impact
different benthic communities.
There may be variability of data due to differences in habitat between streams. The
results may not be sensitive to subtle water quality changes because of habitat
variability between reaches.
Barbour et al. 1999. Rapid Bioassessment Protocols for Use in Streams and
Wadeable Rivers: Periphyton, Benthic Macroinvertebrates and Fish, Second Edition,
EPA 841-B-99-002. U.S. Environmental Protection Agency; Office of Water;
Washington, D.C.
http //www epa.gov/owow/monitoring/rbp/
Last Accessed: 1/31/2003
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2.3.1-9
Method Title
Artificial Substrate Samplers of Macroinvertebrates in Wadeable Streams
Purpose
These methods describe the use of artificial substrate samples that have long been
used in algal investigations and in situations where bottom substrate sampling is not
possible due to physical obstacles. The Rapid Bioassessment Protocols (RBPs) list
artificial substrates as a sampling methodology to collect both periphyton and benthic
macroinvertebrates.
Method Summary
Artificial substrate samplers typically use glass slides as substrate, but also are
deployed with glass rods, ceramic tiles and other substances.
The samplers are positoned in the euphotic zone of good light penetration for
maximum abundance and diversity of macroinvertebrates. Optimum time for
substrate colonization is six weeks. At least two to three samplers should be
installed at each collecting site.
To retrieve the samplers, they are approached from downstream, lifted quickly and
placed in a polyethylene jug or bag containing 10% formalin or 70-80% ethanol.
The organisms can be removed in the field by disassembling the sampler in a tub or
bucket partially filled with water and scrubbing the rocks or plates with a soft-bristle
brush to remove clinging organisms. The contents of the bucket are poured through
a No. 30 or 60 sieve and the contents of the sieve are washed into a jar and preserve
with 10% formalin or 70-80% ethanol.
The use of artificial substrate samplers in macroinvertebrate field and laboratory
studies is also presented in USEPA, 1990b.
Data
Uses/Application
The benthic composition and abundance data from artificial substrate samplers are
used to measure the status and trends of environmental pollution, and effects on
freshwater, estuarine, and marine macroinvertebrates, and to assess surface water
quality.
The RBP protocols caution that artificial substrates should only be used for benthic
macroinvertebrates when other collection devices fail. The substrate used must be
representative of the natural habitat.
Advantages
Artificial substrates allow sample collection in locations that are typically difficult to
sample effectively. As a passive sample collection device, artificial substrates permit
standardized sampling by eliminating subjectivity in sample collection techniques.
Sample collection using artificial substrates may require less skill and training than
direct sampling of natural substrates.
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Limitations
Reference
Website
2.3.1-9 (contd.)
The limitations commonly encountered when using the artificial substrate sampler
include susceptibility to vandalism, sampling bias for insects, difficulty in anchoring
the device, and the lengthy time from initiation to conclusion of sampling (up to 8
weeks). Furthermore, the material of the substrate will influence the composition
and structure of the community. Orientation and length of exposure of the substrate
will influence the composition and the structure of the community.
Barbour, et al. 1999. Rapid Bioassessment Protocols for Use in Streams and
Wadeable Rivers- Periphyton, Benthic Macroinvertebrates and Fish, Second Edition.
EPA 841-B-99-002. U.S. Environmental Protection Agency,- Office of Water;
Washington, D.C.
httoV/www eoa aov/owow/monitorina/rbp/ Last Accessed: 1/31/2003
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Reference
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2.3.1-10
Algae and Macroinvertebrate Sampling with Frames
To delineate the percent coverage of the colonial forms of algae and
macroinvertebrates.
A 0.1 m2 or 1m2 square-shaped metal frame can be laid flat along rocky shores,
beaches etc. and be used to delineate the percent coverage of colonial frames. At
least ten frames should be used for counting organisms to characterize species
abundance and distribution adequately. Samples of the algae and
maeroinvertebrates should be removed from a measured area for species
identification and weighed for biomass determination.
An investigator can gather macrobenthos data using frames from locations where
conventional sampling devices are not practical. Macrobenthos data are used in
benthic community analyses to measure the status and trends of environmental
pollution, and its effects on freshwater, estuarine, and marine macroinvertebrates,
and to assess water quality criteria and monitor surface water quality.
This method is useful for sampling beach infauna.
Frames delineate organisms present on the surface, however all organisms
burrowed beyond the investigator's line of site will not be counted. Rely upon
statistics to derive species abundance and distribution for the entire region.
USEPA. 1990b. Macroinvertebrate Field and Laboratory Methods for Evaluating the
Biological Integrity of Surface Waters, EPA/600/4-90/030. Office of Research and
Development, U.S. Environmental Protection Agency, Washington, D.C.
http //www epa qov/clanton/clhtml/pubtitleORD ht Last Accessed- ?m/na
m!
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Fact Sheet No.
2.3.1-11
Benthic Organism Collection from a Marine Environment, NHEERL-AED SOP
1.02.001
This procedure describes the methods required to collect infaunal and epibenthic
marine organisms for tissue analyses or for use in toxicologfcal evaluation.
Benthic macroinvertebrates: Sediments are frequently collected with grab samplers,
such as the Young-modified Van Veen grab. This particular sampler is constructed
entirely of stainless steel and can be Kynar-coated to make it suitable for collecting
sediment samples for both biological and chemical analyses. The samples should
be numbered and the depth of the sediment at the middle of the sampler should be
recorded on the data sheet. The sampler should be at least half full. The data sheet
should also include a general description of the grab such as the presence or
absence of surface floe, color and smell of surface sediments, and visible fauna.
Worms: Sediments from grab samples are emptied into a tub and then passed
through sieves. The appropriate sieve size could be selected based on sediment
type and organisms to be collected. Worms are picked from the sieves, rinsed free
of sediment, and placed in sample jars.
Quahogs- Quahogs should be collected with the aid of a professional quahog
fisherman. The fisherman should be provided with one extra individual for
assistance, a sampling location chart, and prelabelled and organized sample bags.
Mytilus: Mussels are collected with a scalbp dredge towed at 2-3 knots for 5-10
minutes. The catch is then hauled back, dumped on board, and sorted.
Oysters: Hand collection in shallow water is recommended.
Soft-shell clams: Soft-shelled clams should be collected by hand at low-tide. After
locating siphon holes on the tidal region of the flat, the clams can be dug out, taking
care to avoid breaking the "soft-shell" during excavation.
USEPA's Coastal and Northeast EMAP document describes similar protocols for
benthic organism collection (USEPA, 2000b).
Benthic organisms can be collected to determine species composition and
abundance in a particular sampling reach, or the organisms may be used for tissue
residue analyses in toxicological evaluation.
All activities can be performed by hand or from a small boat.
While the use of sediment grab samplers for collecting macroinvertebrates and
worms is almost unanimously recommended, the application of other methods is
highly site-specific.
USEPA and the Naval Construction Battalion Center. 1992. Standard Operating
Procedures and Field Methods Used for Conducting Ecological Risk Assessment
Case Studies. Technical Document 2296. Naval Command, Control and Ocean
Surveillance Center, RDT&E Division, San Diego, CA.
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Benthic Macromvertebrate Protocols in a Wadeable Stream: Single Habitat
Approach, 1 -Meter Kick Net
To determine macroin vertebrate diversity and abundance in wadeable streams.
The single habitat approach to benthic macroinvertebrate sampling emphasizes
sampling a single, dominant habitat (i.e., riffles or runs) as a way of standardizing
assessments.
Benthic macroinvertebrate samples are collected systematically using aim kick
net. Once the net is in position on the substrate, a rectangular quadrant that is
approximately 0.5 m2is visually defined. The net is held securely while the substrate
is kicked vigorously for 20 seconds. After 20 seconds, the net is removed with a
quick upstream motion to wash the organisms to the bottom of the net. The kicks
collected from different locations in flowing water habitats will be composited to
obtain a single homogeneous sample. Kick net samples collected from pool habitats
are combined into a separate composite sample. The percentage of habitat type is
recorded along with observations of aquatic flora and fauna and a habitat
assessment will be performed.
The samples composited from the kick nets will be preserved in 95% ethanol. The
samples are then returned to the laboratory for species enumeration and
identification.
The USEPA EMAP field document describes similar methods for using a
1-m kick net (USEPA, 1998).
Species relative abundance and taxa richness are data derived from these protocols.
These data parameters provide information pertaining to the status and trends of
environmental pollution and its impacts on freshwater, marine and Estuanne
communities.
Biological impairment resulting from pollution is often evaluated using metrics of
biotic integrity derived from the aforementioned data parameters that evaluate
community, population and functbnal parameters.
The 1-m kick net method provides a rapid, reproducible, and inexpensive method for
the collection of macroinvertebrates from suitable environments.
Single habitats (i.e., cobble substrates) cannot be solely analyzed in reaches where
the substrate represents less than 30% of the sampling reach
Barbour et al. 1999. Rapid Bioassessment Protocols for Use in Streams and
Wadeable Rivers. Periphyton, Benthic Macroinvertebrates and Fish, Second Edition,
EPA 841-B-99-002. Office of Water, U.S. Environmental Protection Agency.
Washington, D C.
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2.3.1-13
Benthic Macroinvertebrate Protocols in a Wadeable Stream: Multi-habitat Approach:
D -Frame Dip Net
To determine macroinvertebrate diversity and abundance in wadeable streams.
This method focuses on a multi-habitat scheme designed to sample major habitats in
proportional representation within a sampling reach. Benthic macroinvertebrates are
collected systematically from all available instream habitats by kicking the substrate
or jabbing with a D-frame dip net. A total of 20 jabs (or kicks) are taken from all
major habitat types in the reach resulting in sampling of approximately 3.1 m2 of
habitat.
The samples collected from this protocol will then be sent to the laboratory where
species enumeration and identification will be conducted.
Species relative abundance and taxa richness are data derived from these protocols.
These data parameters provide information pertaining to the status and trends of
environmental pollution and its impacts on freshwater, marine and estuarine
communities.
Biological impairment resulting from pollution is often evaluated using metrics of
biotic integrity derived from the aforementioned data parameters that evaluate
community, population and functbnal parameters.
It is important to use a multi-habitat approach when the stream under investigation
varies in gradient and substrate type.
Differences in sampling techniques can lead to variability and difficulty comparing
data among researchers.
Barbour et al. 1999. Rapid Bioassessment Protocols for Use in Streams and
Wadeable Rivers: Periphyton, Benthic Macroinvertebrates and Fish, Second Edition,
EPA 841-B-99-002. Office of Water, U.S. Environmental Protection Agency,
Washington, D.C.
htto //www.epa qov/owow/momtonnq/rbp/ Last Accessed: 1/31/2003
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Photographic Habitat Documentation of the Benthic Community
To document a habitat or alterations in a station over time (e.g., increase in canopy
cover, changes in channelization of a stream, and effects of flooding etc.)
Photography of aquatic environments usually involves SCUBA equipment. The
SCUBA diver will place a photographically identifiable 1.0 m2 area frame or marker in
the habitat to be photographed and an additional nearby marker on which the
camera is placed each time a photograph is taken to ensure consistency.
Photography is a tool used to characterize benthic composition and potential
alterations overtime in environments with sessile organisms that may change over
time in relation to a new stressor.
Photographic images of the abundance and diversity of sessile organisms over time
is a way in which to monitor the status and trends of environmental pollution, and its
effects on freshwater, estuarine, and marine organisms, and to assess surface water
quality.
Photographic documentation is a rapid and inexpensive tool to use to support benthic
bioassessments, particularly in areas with significant populations of sessile
organisms.
Photography is generally limited to environments with suitably clear water that are
inhabited by sessile animals and rooted plants (e.g., estuarine habitats containing
corals, sponges, and attached algal forms). Underwater photography generally
requires trained SCUBA divers.
USEPA. 1990b. Macroinvertebrate Field and Laboratory Methods for Evaluating the
Biological Integrity of Surface Waters, EPA/600/4-90/030. Office of Research and
Development, U.S. Environmental Protecton Agency, Washington, D.C.
http //www epa qov/clanton/clhtml/pubtitleORD ht
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2.3.1-15
Sediment Profile Camera
This method describes use of a sediment profile camera to evaluate the in situ
macroinvertebrate community.
Photographs are taken of the benthic community prior to any other benthic sampling
to avoid disruption of the surface. The sediment profiling index (SPI) system consists
of a digital camera enclosed in a waterproof, pressure resistant housing, a 45-degree
prism that penetrates the sediment to a depth of 25 cm, and a mirror that reflects an
image of the sediment profile through the camera lens and to the digital-camera. The
camera prism is mounted on an assembly that can be moved up and down by
producing tension or slack on the winch wire.
As the camera is lowered, tension on the winch wire keeps the prism in the 'up'
position until the support frame hits the bottom. At this point the tension on the winch
wire is reduced causing the inner frame to move to the 'down' position, penetrating
the undisturbed sediment water interface. The upper 25 cm of the sea floor, as seen
in profile, is then photographed in high resolution with a film or digital camera. An
additional camera mounted on the frame photographs the sediment surface before
the prism penetrates the sediment. After each image is taken, the camera is raised
two or three meters off the bottom and redeployed for taking another image
('sample').
SPI cameras are used to evaluate macrofauna community structure and assess the
benthic habitat. SPI technology can readily quantify over 20 physical, chemical, and
biological parameters including: sediment grain size; prism penetration; surface
pelletal layer; sediment surface relief; mud clasts; redox area; redox contrast; current
apparent redox boundary; relict redox boundaries; methane gas vesicles; apparent
fauna! dominants; voids; burrows; surface features (e.g., worm tubes, epifauna,
shell); dredged material; microbial aggregatons; and successional stage. SPI data
have been accepted in the United States by the by the U.S. Environmental Protection
Agency and by the U S. Army Corps of Engineers for describing baseline benthic
habitat conditions at proposed dredged material disposal sites, for monitoring
changes in sediment structure and the benthic community from dredged material
disposal, and for monitoring the recovery of disposal sites and their surrounding
environment.
Rapid photographic evidence of sediment conditions.
Provides only a partial picture of benthic community structure, and little information
on benthic macromfauna communities Generally, limited to screening in soft bottom
sediments.
USEPA. 1990a. Environmental Monitoring and Assessment Program: Near Coastal
Component, 1990 Demonstration Project, Field Operations Manual. DRAFT.
Contract # 68-C8-0066. Office of Research and Development. Narragansett, Rhode
Island.
http //www epa qov/emap/html/pubs/docs/groupd Last Accessed: 1/31/2003
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2.3.1-16
Macromvertebrate Drift Nets in Wadeable Streams
To collect macrobenthos inhabiting a wide range of habitat types from shallow
flowing streams or shallow areas in rivers for quantitative evaluations.
For synoptic surveys, one net set above each of the major areas of population
concentrations is usually adequate; but for definitive studies a minimum of two drift
nets should be set at each station so that drift from above a pollution source, drift
from the polluted reach and drift from the clean water downstream from the recovery
zone can be compared.
Use nets with a 929 cm2 upstream opening and mesh equivalent to the U.S.
Standard No. 30 screen (0.595 mm pore size). Set drift nets for any specified time
(usually 3 hours). Sampling between dusk and 1 AM is optimum. For definitive
studies, install four nets at each station two about 25 cm from the bottom and tow
about 10 cm below the surface in water not exceeding 3 meters in depth. At the end
of the specified sampling period, remove the net from the water by loosening the
cable clamps and raising the net over the top of the steel rods, taking care not to
disturb the bottom upstream of the net. Concentrate the material in the net in one
corner by swishing up and down in the water and then wash into a bucket half-filled
with water. Then sieve and handle the sample in the regular manner.
Standard methods 10500 describe similar collection methods (APHA, 1999).
Drift nets collect macrobenthos in order to characterize the composition and
abundance of macroinvertebrate biota that drift in the water column. A summary of
stream net samplers is presented in Table 2.3.1-1.
Macroinvertebrate data such as these are used to measure the status and trends of
environmental pollution and its effects on freshwater, estuarine, and marine
macroinvertebrates, to assess water quality criteria and to monitor surface water
quality.
Standard collection method used throughout United States.
It is unknown where the organisms come from; terrestrial species may make up a
large part of sample in summer and periods of wind and rain. Drift nets do not collect
non-drifting organisms.
USEPA. 1990b. Macroinvertebrate Field and Laboratory Methods for Evaluating the
Biological Integrity of Surface Waters. EPA/600/4-90/030. Office of Research and
Development, U S. Environmental Protection Agency, Washington, D.C.
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Table 2.3.1-1. A Summary of Stream Net Samplers Used to Collect Organisms from Flowing Water (USEPA, 1990b1)
Net Sampler
Surber Stream
Bottom
Sampler
Portable
Invertebrate
Box Sampler
Hess Sampler
Hess Stream
Bottom
Sampler
Stream -bed
Fauna
Sampler
Drift nets
Habitats and
substrates
Shallow, flowing
streams, less than 32
cm in depth with good
current, rubble
substrate, mud. sand
and gravel
Same as Surber
Same as Surber
Same as Surber '
Same as Surber
Flowing nvers and
streams; all substrate
types
Effectiveness of Device
Performance depends on
current and substrate
Same as Surber
Same as Surber
Same as Surber
Same as Surber
Effective in collecting all
taxa which drift In the
water column
Advantages
Encloses area sampled;
easily transported or
constructed, samples a
unit area
Same as Surber except
completely endosed with
stable platform; can be
used in weed beds.
Same as Surber except
completely endosed with
stable platform, can be
used in weed beds
Same as Surber except
completely endosed with
stable platform, can be
used in weed beds
Same as Surber except
completely enclosed with
stable platform; can be
used in weed beds.
Low sampling error; less
time, money and effort
collects
macroinvertebrates from
all substrates, usually
collects more taxa
Limitations
Difficult to set in some
substrate types, that is
large rubble, cannot be
used efficiently in still,
slow-moving streams
Same as Surber
Same as Surber
Same as Surber
Same as Surber
Unknown where
organsms come from,
terrestrial species may
make up a large part of a
sample in summer and
periods of wind and ram;
does not collect non-
drifting organisms
USEPA. 1990b. EPA/600/4-90/030.
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2.3.1-17
Stream-Net Samplers: Surber, Portable Invertebrate Box Sampler, Hess Sampler,
Hess Stream Bottom Sampler, and Stream-Bed Fauna Sampler
To collect macrobenthos inhabiting a wide range of habitat types from shallow
flowing streams or shallow areas in rivers for quantitative evaluations.
The sampler is positioned with its net mouth open, facing upstream. The samplers
are brought down quickly to reduce the escape of rapidly moving organisms. There
should be no gaps under the edges of the frame that would allow for washing of
water under the net -and loss of benthic organisms.
Remove the sample after a specified period of time, by inverting the net into the
sample container (wide-mouthed jar) with 10% buffered formalin fixative or 70-80%
ethanol. Examine the net closely for small organisms clinging to the mesh, and
remove them (preferably with forceps) for inclusion in the sample.
Standard method 10500 describe similar collection methods (APHA, 1999).
Stream-net samplers collect relatively quantitative and qualitative macroinvertebrate
samples from the water column of flowing streams and rivers. The
macroinvertebrates collected in the nets will be taxonomically identified and counted
to determine the macroinvertebrate composition and abundance in that reach of the
river. Composition and abundance data are used to measure the status and trends
of environmental pollution and its effects on freshwater, estuarine, and marine
macroinvertebrates, to assess water quality criteria, and to monitor surface water
quality.
Rapid, reproducible and inexpensive sampling technique for in-stream fauna.
It is difficult to set in some substrate types, such as large rubble. It cannot be used
effectively in still, slow moving streams. Organisms often wash under the bottom
edge of some samplers such as the Surber.
USEPA. 1990b. Macroinvertebrate Field and Laboratory Methods for Evaluating the
Biological Integrity of Surface Waters. EPA/600/4-90/030. Office of Research and
Development, U.S. Environmental Protection Agency, Washington, D.C.
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Mussel Collection Using Brails
To sample bivalve mussels in large (non-wadeable) rivers
A crowfoot brail will be dragged a measured distance of 100 meters. Each brail
sample is then brought on board the boat, sorted and counted. The area sampled is
calculated in square meters by multiplying the length of the brail by 100 m. Catch
success is expressed in terms of the average catch of mussels per square per drag.
Brail sampling is randomized within fishing areas and by time periods during two
complete harvest seasons. The crowfoot brails can often be made or rented from a
commercial fisherman.
A minimum of six 100 m long hauls (drags) should be accomplished where a single
brail is used. If a significant mussel population is found, then qualitative or
quantitative SCUBA samples should be taken.
All samples should be identified to species, growth cessation rings counted, and
measured for determination of population age structure.
Brail sampling provides both qualitative and quantitative data pertaining to mussel
abundance in a given region. Useful in estuarine areas where mussels comprise a
dominant benthic community.
Brail sampling is an inexpensive, bioassessment technique for those riverine
environments where mussels are an important component of the ecosystem.
Mussel fishing with brails is highly dependent on experience of the user; however,
they are very efficient in the hands of experienced users as attested to by almost 100
years of continuous use.
USEPA. 1990b. Macroinvertebrate Field and Laboratory Methods for Evaluating the
Biological Integrity of Surface Waters. EPA/600/4-90/030. Office of Research and
Development, U.S. Environmental Protection Agency, Washington, D.C.
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2.3.1-19
Electrofishmg
Fish collection method for environmental assessments
Electrofishing is a method for collecting fish using electricity. Most electrofishing in
freshwater is done with pulsed DC electrical current equipment. In a boat-rigged
shocker (boom shocker), one or two people net the fish and another operates the
boat and equipment. The fish are nearly always driven into cover as a result of
electric stimulus making them difficult to capture. Once driven from cover, the fish
are kept within effective range of the electrical field and are immobilized making it
possible to pick them up with long-handled dip nets.
Other USEPA documents and APHA Standard Method describe similar use of
electrofishing for sample collection methods (Barbour et al, 1999; USEPA, 1998;
APHA, 1999).
Electrofishing is a technique used to survey the biological community. As a result,
fish species will be identified and counted to determine the organism abundance and
composition in that region. Abundance and composition data are used to measure
the status and trends of environmental pollution and its effects on marine, estuanne
and freshwater organisms, to assess water quality criteria, and to monitor surface
water quality.
Efficient method that can be used to obtain reliable information on fish abundance,
length-weight relationships, and age and growth offish in most streams of order 6 or
less. Usually results in more consistent success under varying conditions than
ordinary seining. It allows greater standardization of catch per unit effort, it requires
less time and manpower than use of ichthyocides, and it is less selective than seining
(although it is selective towards size and species). If properly used, adverse effects
on fish are minimized, and it is appropriate in a variety of habitats.
Individuals involved in electrofishing must have completed a certified course in
electrofishing or have been trained by someone certified and experienced in
electrofishing. If target assemblage is a common species, then seining may be just
as effective. Cannot be used in water with high turbidity. Need very specific
conditions and equipment. Sampling efficiency is affected by turbidity, conductivity,
aquatic vegetation, depth etc; although it is less selective than seining, electrofishing
also is size and species specific. Effects of elctrofishmg increase with body size.
Species specific behavioral and anatomical differences also determine vulnerability to
electroshocking. Electrofishing is a hazardous operation that can injure field
personnel.
USEPA. 1993c. Fish Field and Laboratory Methods for Evaluating the Biological
Integrity of Surface Waters, EPA/600/R-92-1 1 1 . Office of Research and
Development, Washington, D.C.
http //www epa.gov/bioindicators/html/fish meth Last Accessed: 1/31/2003
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2.3.1-20
Chemical Fishing
Fish collection method for environmental assessments
Fish toxicants are used for sampling fish populations in impounded waters and
streams throughout the United States. Only registered fish chemical toxicants, such
as rotenone, cresol, copper sulfate, antimycin A and sodium cyanide, can be used to
collect fish in the U.S. The ideal icthyockJe is nonselective; easily, rapidly, and safely
used; readily detoxified: and not detected and avoided by fish. Chemical sampling is
usually employed on a spot basis (e.g., a short reach of river or an embayment of a
lake or reservoir). A concentration of 0.5 ppm active ingredient will provide good
recovery of most species of fish in acidic or slightly alkaline water. Emulsion
products are applied via manual pumps , spraying equipment, power-driven pumps,
or a drip spout coming from a flowing system.
Standard Method 10600 describes similar uses of chemical fishing for fish sample
collection (APHA. 1999).
Chemical fishing surveys are often used to gain information on particular species of
fish and an overall estimation of fish populations and communities. Fish population
and community data are used to measure the status and trends of environmental
pollution and its effects on freshwater, estuarine and marine organisms, to assess
water quality criteria, and to monitor surface water quality. Rotenoning provides
greater standardization of unit of effort than seining. Rotenoning has the potential, if
used effectively, to provide more complete censuring of the fish population than
seining or electrofishing.
Advantages of rotenone: The effective use of rotenone is independent of habitat
complexity.
Disadvantages of rotenone: Use of rotenone is prohibited in many states, application
and detoxification can be time and manpower intensive. Effective use of rotenone is
affected by temperature, light, dissolved oxygen, alkalinity, and turbidity. Rotenoning
typically has a high environmental impact; concentration miscalculations can produce
substantial fish kills downstream of the study site.
USEPA. 1993c. Fish Field and Laboratory Methods for Evaluating the Biological
Integrity of Surface Waters, EPA/600/R-92-1 1 1 . Office of Research and
Development, U.S Environmental Protecton Agency. Washington, D.C.
http //www epa gov/bioindicators/html/fish method
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2.3.1-21
Fish Collection Using Seme Nets
Fish collection method for environmental assessments
A strip of strong netting is hung between a stout float line and a strong, heavily
weighted lead line at the bottom. In deepwater, one end of the hauling lines is
anchored on shore and the boat plays out the line until it reaches the end. The boat
then lays out the net parallel to the beach. When all of the net is in the water, the
boat brings the end of the second hauling line ashore. The net is then beached as
rapidly as possible. In shallow waters, a person can lay out the one end of the
hauling line and replicate the role of the boat. There are many different types of
seines; selectng the appropriate seine depends on the study design, sampling
methods and habitat type.
Other USEPA documents and APHA Standard Methods describe the similar use of
seine nets for fish collection (Barbouret al, 1999; USEPA, 1998; Standard Method
10600. APHA. 1999).
Seine nets survey the biological community by collecting abundance and taxa
composition data from sampling locations. Organism abundance and composition
data are used to measure the status and trends of environmental pollution and its
effects on freshwater, estuanne and manne organisms, to assess water quality
criteria, and to monitor surface water quality. The Rapid Bioassessment Protocols
(RBPs) list seining as a viable way to collect fish samples.
Seines are lightweight and easily transported and stored. Seine repair and
maintenance are minimal and can be accomplished onsite. Seine use is not
restricted by water quality parameters Effects on the fish population are minimal
because fish are collected alive and are generally unharmed.
Not effective in deep water. Not effective in areas that have snags, large rocks and
boulders, or sunken debris that may tear or foul the net. Quantitative seining is very
difficult. Previous experience and skill, knowledge of fish habitats and behavior and
sampling effort are probably more important in seining than in the use of any other
approaches. Seining sample effort and results are more variable than sampling with
electrofishing and rotenonmg. Seine use is generally restricted to slower water with
smooth bottoms, and is most effective in small streams or pools without litter cover or
debris. Standardization of unit of effort to ensure data comparability is difficult
USEPA 1993c. Fish Field and Laboratory Methods for Evaluating the Biological
Integrity of Surface Waters. EPA/600/R-92-1 1 1 . Office of Research and
Development, U.S Environmental Protecton Agency, Washington, D.C
http//www epa qov/biomdicators/htm I/fish meth
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2.3.1-22
Entanglement Nets
Fish collection method for environmental assessments
Entanglement nets, including gill nets and trammel nets, are used to sample fish
populations in estuaries, lakes, reservoirs, and larger rivers. Gill nets are the more
commonly used entanglement nets. They are usually set as an upright, vertical
fence of netting and can have either a variable or uniform mesh size. Gill nets
selectively capture particular species of fish since the mesh size determines the size
range of the fish to be sampled. They can be set at the surface, mid-depth, or on the
bottom depending on the objectives of the study and target species within the fish
community. Trammel nets are used in all types of riverine habitat. If a river channel
is to be fished, the net is floated or drifted downstream. They are very efficient for
taking fish like carp, buffalo, shovelnose sturgeon and freshwater drum.
Entanglement nets survey the biological community by collecting abundance and
taxa composition data from sampling locations. They are often used to gain
information on particular species offish and an overall estimation offish populations
and communities. Fish population and community data are used to measure the
status and trends of environmental pollution and its effects on freshwater, estuarine
and marine organisms, to assess water quality criteria, and to monitor surface water
quality.
This method describes an effective way to sample fish populations. The results are
expressed as the number or weight of fish taken per length of net per day (catch per
unit effort).
Entanglement nets need to be monitored for by-catch. Non-target species may be
caught and will not survive long in the net. Tidal currents, predation, optimum fishing
time and types of anchors, floats and line must be considered when setting
entanglement nets in estuaries.
USEPA. 1993c. Fish Field and Laboratory Methods for Evaluating the Biological
Integrity of Surface Waters, EPA/600/R-92-1 1 1 . Office of Research and
Development, U.S. Environmental Protection Agency, Washington, D.C.
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2.3.1-23
Entrapment Devices
Fish collection method for environmental assessments
With entrapment devices, fish enter an enclosed area (which may be baited) through
a series of one or more funnels. They are set in structurally complex areas where
fish movement and density are anticipated to be highest in order to maximize net
catches. Common entrapment devices include the hoop net, fyke net, and minnow
trap.
Entrapment devices survey the biological community by collection abundance and
taxa composition data from sampling locations. They are often used to gain
information on particular species of fish and an overall estimation of fish populations
and communities. Fish population and community data are used to measure the
status and trends of environmental pollution and its effects on freshwater, estuarine
and marine organisms, to assess water quality criteria, and to monitor surface water
quality.
They are used to sample reservoirs and wide river channels with slow velocity
conditions. The catch is recorded as numbers of weight per unit of effort, usually fish
per net day.
Entrapment devices are generally deployed overnight, requiring separate filed activity
for deployment and retrieval. Traps are often vandalized in unsecured areas.
USEPA. 1993c. Fish Field and Laboratory Methods for Evaluating the Biological
Integrity of Surface Waters, EPA/600/R-92-1 1 1 . Office of Research and
Development, U.S. Environmental Protection Agency, Washington, D.C.
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2.3.1-24
Pop Nets
Fish collection method for environmental assessments
Pop nets are rectangular devices, constructed of mesh netting used for the collection
of fish. They are designed to be deployed from the surface and released with a
mechanical device. They are set and received by two individuals and are easily
dissembled for transport.
Pop nets survey the biological community by collecting abundance and taxa
composition data from sampling locations. They are often used to gain information
on particular species of fish and an overall estimation of fish populations and
communities. Fish population and community data are used to measure the status
and trends of environmental pollution and its effects on freshwater, estuarine and
marine organisms, to assess water quality criteria, and to monitor surface water
quality.
Useful for sampling fish in shallow, riverine waters in heavily vegetated areas and
nonvegetated areas where seining or electroshocking may be difficult.
Pop nets will sample a relatively small area/volume of surface water. Thus.
representativeness may be a concern if used for population studies.
USEPA. 1993c. Fish Field and Laboratory Methods for Evaluating the Biological
Integrity of Surface Waters. EPA/600/R-92-1 1 1 . Office of Research and
Development, U.S. Environmental Protection Agency, Washington. D C.
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Trawls
Fish collection method for environmental assessments
Trawls are designed like seines; however, they are much larger and intended to be
towed behind boats in large, open water areas. There are four types of trawls
available: beam trawls, used to capture bottom fish; otter trawls, used to capture
near-bottom and bottom fish; mid-water trawls, used to collect schooling fish at
various depths; and surface tow nets, used to collect fish at or near the surface. The
trawls are deployed behind the boat, often with power winches and large motors.
Under the Coastal EMAP Program, fish are specifically collected with a high rise
sampling trawl with a 13.5 meter footrope with a chain sweep. Tow duration is 10
minutes with a towing speed of 2-3 knots against the prevailing current. Speed over
the bottom should be 1-3 knots (USEPA. 2000b).
The trawl is retrieved used hydraulics and the contents of the net are often emptied
onto sorting tables. Fish are sorted, enumerated and examined for gross
pathological examinations. Selected specimens are retained and properly processed
for tissue chemical analyses.
The APHA Standard Method describe similar trawl methods to collect fish (Standard
Method 10600 (APHA, 1999).
Trawl nets survey the biological community by collecting samples that will be
analyzed for species composition, relative abundance, chemical analysis, and
pathological examination. They are often used to gain information on particular
species offish and an overall estimation offish populations and communities. Fish
population and community data are used to measure the status and trends of
environmental pollution and its effects on freshwater, estuarine and marine
organisms to assess water quality criteria, and to monitor surface water quality.
Trawl nets are very effective in large, open water areas and can effectively sample
selected bottom, mid-water, and surface oriented species at specific life history
stages.
Not effective in deep water. Not effective in areas that have snags, large rocks and
boulders and sunken debris that may tear or foul the net. Quantitative trawling is very
difficult. Previous experience and skill, knowledge of fish habitats and behavior and
sampling effort are probably more important in seining than in the use of any other
approaches. Trawling sample effort and results are more variable than sampling with
electrofishing and rotenonmg. Trawl use is generally restricted to slower water with
smooth bottoms, and is most effective in small streams or pools without litter cover or
debris. Standardization of unit of effort to ensure data comparability is difficult
USEPA. 1993c. Fish Field and Laboratory Methods for Evaluating the Biological
Integrity of Surface Waters. EPA/600/R-92-1 1 1 . Office of Research and
Development, U.S. Environmental Protection Agency, Washington, D.C.
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Fish Processing Method in the Great Lakes, LMMB 025
This method describes the aging, compositing, and grinding method for fish.
Whole fish are collected (intact, with all body fluids and no incisions), wrapped in
aluminum foil, placed in 4 mil thick polyethylene bags, tagged, and frozen as soon as
possible on board the vessel. Fish should be transferred in coolers and stored at -
20°C. To age the fish, scales were removed from the fish, and the annual rings on
the scales are read to determine the age. Some fish that have been stocked may
contain coded wire tags (CWT) or clipped fins. Stocking or tagging records may
provide useful information in aging such fish.
For homogenization, fish are removed from the freezer and allowed to thaw in their
bags over an 8 - 12 hour period. The contents of the bags are weighed and
recorded. Fish may be composited based on species, location, size and season
sampled. Fish are measured (millimeters) on a measuring board and weighed to the
nearest gram. The measuring board, scalpel, and balance are cleaned between
each group. Each composite sample is homogenized, using various size vertical
cutters or Robot Coupe cutter. Subsamples of the homogenized tissue are placed in
clean sample containers and frozen (-20°C) until analyzed.
Standard Method 10600D.3 also discusses the field processing offish, including
length, weight, and age measurements (APHA, 1999).
Fish are often collected for chemical analyses of tissue to determine whether
contaminants are accumulating in biological populations.
These are standard methods and are performed fairly consistently to prepare tissue
for chemical analyses which enhances data consistency in resultant data.
Study design should consider advantages/limitations of homogenates of whole body,
fillet, or offal.
USEPA. 1997b. Method LMMB 025: Fish Processing Method. Lake Michigan Mass
Balance Study Methods Compendium, Volume 1: Sample Collection Techniques,
EPA 905-R-97-012C. Great Lakes National Program Office, Chicago, IL.
http.//www epa.gov/glnpo/lmmb/methods/fpml
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2.3.1-27
Fish Processing
To determine fish diversity and abundance
Once a catch is brought on deck, fish are identified to species, measured, counted,
examined for external pathology and processed for chemical analysis.
The fish are measured with a measuring board, the fork length to the nearest
millimeter. Coastal EMAP procedures specify that the first 30-50 individuals of each
species should be measured. The remaining fish will be identified to species and
counted (USEPA, 2000b, EPA/620/R-00/002).
All individuals that are measured, will be examined for evidence of gross external
pathology. The examination is intended to be a rapid scan of the surface of
individual.
Fish should be cut the entire length of the abdominal cavity. The later musculature is
removed from one side of the animal's visceral cavity to facilitate the fixation of the
internal organs. The opercula is removed and immersed in fixative. The sample
(whole fish or head, visceral cavity and abnormalities excised) is placed in a plastic
bag with many perforations. This bag is then placed in the fixative. Specimen's
should be fixed in Dietrich's fixative for one or two days . Samples may be
transferred to another preservative, such as ethyl alcohol (70-75%) or isopropanol
(40-45%), for storage.
Samples for fish tissue contaminant analysis or electrophoresis must be iced, placed
in dry ice, or liquid N2 for temporary storage or shipping. Special preservation
techniques must be used for histological, histochemical, or biomarker analyses.
Samples are then identified to the species level. Data recorded include species
composition and diversity, populaton density and biomass, and physiological
conditon of indigenous communities of aquatic organisms.
Species relative abundance and taxa richness are data derived from these protocols.
These data parameters provide information pertaining to the status and trends of
environmental pollution and its impacts on freshwater, marine and estuanne
communities.
Biological impairment resulting from pollution is often evaluated using metrics of
biotic integrity derived from the aforementioned data parameters that evaluate
community, population and functional parameters. Fish metrics commonly
determined from this data include species richness, trophic composition, and fish
abundance and condition. Matrices are collectively evaluated in indices such as the
Index of Biotic Integrity (IBI) which aggregates 12 biological metrics to assess fish
assemblage data.
These are considered basic and standard methods for fish processing.
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2.3.1 -27 (contd.)
As with any tissue processing, care must be taken to avoid laboratory and cross-
contamination.
Barbour era/. 1999. Rapid Bioassessment Protocols for Use in Streams and
Wadeable Rivers: Periphyton, Benthic Macroinvertebrates and Fish, Second Edition,
EPA 841-B-99-002. Office of Water, U.S. Environmental Protection Agency,
Washington. D.C.
httpV/www epa qov/owow/monitonnq/rbp/
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2.3.1-28
Swallows: Sampling Procedures
This method describes the use of tree swallows at contaminated sites to quantify
population level impacts and population level chemistry data.
Approximately 60 swallow boxes, 30 at each of 2 sites, will be attached to posts or
other suitable structures in suitable habitat. Boxes will be placed approximately 20-
30 meters apart, but this can vary depending on the structure of the habitat. Each
nest box will be visited approximately once per week until egg laying begins. After
that time, nests may be visited more often to collect egg or just hatched young
samples. After the eggs have been hatched, boxes will be visited at least once per
week until the young reach 12 days of age. Whether eggs or young are present in
the nest box, the number of eggs and young present will be recorded on a data
sheet. A sample of 2-3 eggs and/or just-hatched eggs (pippers) and a sibling 12-day-
old tree swallow nestling will be collected from a minimum of 5-10 boxes at each site.
Food samples from the stomachs of tree swallow nestlings will be removed at the
time that they are collected and dissected. A pooled food sample from each site,
along with the pipperand nestling samples may be analyzed for organochlorine
chemicals, including total PCBs and a full dioxm scan if sufficient mass is available.
Nestling tree swallows may be ligatured to obtain additional food samples for insect
species identification and for chemical analysis of food. Ligatures, black electrical zip
ties, will be placed on all nestlings in a nest box and left in place for 1 hour. Care will
be taken that the zip ties are loose enough to allow normal breathing. After 1 hour,
the food boli will be removed from the throats of the nestlings using a pair of blunt-
nosed forceps and the ligatures removed.
Swallows are collected for determining population impacts (ie., reproductive
successes, deformities etc) and for chemical analyses.
Evaluation of population level impacts is important to determine potential exposures
and effects over the long term.
Chemical analyses of swallow tissue indicate whether or not bioaccumulative
chemicals are present and whether they are being transferred up the food chain.
Sampling bird species is less precise since their mobility allows them to forage in a
great range of areas. Therefore, population level and tissue contaminant level
results may not always be indicative of the conditons at the site of concern.
Single species tests sometimes skew results since species will react differently to
contaminant exposures due to various biochemical or physiological traits.
USGS. 1998. Tree Swallow Sample Collection and Processing Procedures,
Technical Operating Procedure WE-410.0. Upper Mississippi Science Center, U.S.
Geological Survey, LaCrosse, Wl.
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Sample Processing of Swallows
This method describes the use of tree swallows at contaminated sites to quantify
population level impacts and population level chemistry data.
Pippers or 12-day old nestlings will be removed from the nest box and weighed.
Pippers and nestlings will be visually examined for gross abnormalities. Nestlings will
be decapitated with a pair of sharp scissors, contents in the upper gastrointestinal
tract removed with forceps after an incision is made along the length of the stomach,
and the carcass remainder placed in a chemically clean jar, which has been
purchased in that condition. The above will be done within 2 hours after removal
from the nest box. The carcass remainders and food samples will be maintained
frozen until transported to the storage in a freezer. Samples will be shipped to an
analytical laboratory for processing.
Swallows are collected for determining population impacts (i.e., reproductive
successes, deformities etc) and for chemical analyses used in ecological risk
assessments. Evaluation of population level impacts is important to determine
potential exposures and effects over the long term. Chemical analyses of swallow
tissue indicate whether or not bioaccumulatitve chemicals are present and whether
they are being transferred up the food chain.
Swallows are often used in ecological risk assessments at freshwater ponds
because of their exclusive insect diet and comparative ease of collection.
Sampling bird species is less precise since their mobility allows them to forage in a
great range of areas. Therefore, population level and tissue contaminant level
results may not always be indicative of the conditions at the site of concern.
Single species tests sometimes skew results since species will react differently to
contaminant exposures due to various biochemical or physiological traits.
Ouster. C.M., T.W. Custer, P.O. Allen, K.L. Stromborg, and M J. Melancon. 1998.
Reproduction and environmental contamination in tree swallows nesting in the Fox
River drainage in Green Bay, Wisconsin, USA. Environmental Toxicology and
Chemistry. 17:1786-1798.
N/A
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2.3.2 Chemical and Physical Analysis
Section 2.3.2 contains methods for sample preparation and the chemical analysis of biota. These
methods characterize the chemical composition of biota samples collected by methods described
in Section 2.3.1. Samples are often analyzed for the presence of inorganic and organic
contaminants that may pose a threat to human or ecological health. Analyzing biological tissue
provides a direct measure of the uptake and bioaccumulatbn of pollutants from the environment
and can be used to correlate environmental concentrations of contaminants with body residues.
Many of the methods described have been developed over time to optimize the detection,
identification, and quantification of potential chemicals of concern. Several are performance-based
and may be further modified to enhance the accuracy and precision of the method. Special
preparation and clean up procedures are utilized when analyzing biological tissue, due to the often
high lipid content of the samples. Lipids tend to concentrate environmental pollutants, but they can
also interfere with the analysis of these contaminants.
The chemical methods for the analysis of biological tissue are less routinely performed than for the
analysis of water and sediment. NOAA's National Status and Trends Program (1998) developed
many methods for the chemical analysis of biota and was a main source of information in the
preparation this compendium. Other sources of information presented in Section 2.3.2 included:
• The USEPA's Office of Water
• The USEPA's Lake Michigan Mass Balance Study Methods Compendium, 1997v
• The USEPA's Fish Field and Laboratory Methods for Evaluating the Biological Integrity
of Surface Waters, 1993
• The USEPA's Test Methods for Evaluating Solid Waste, Physical/Chemical Methods
(SW846 Methods)
• Standard Methods for Examination of Water and Wastewater, 1999
• ASTM
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2.3.2-1
Sample Preparation for Metal Contaminants in Tissue
This method describes how fish tissue is processed and prepared for metal
contaminant analyses in the laboratory.
Prior to use, utensils and bottles should be thoroughly cleaned with a detergent-free
solution, rinsed with tap water, soaked in acid, and then rinsed with metal-free water.
Sample size requirements vary with tissue type and detection limit requirements.
When filleting the fish, special care should be taken to avoid contaminating target
tissues (especially muscle) with slime and/or adhering sediment from the fish skin.
The procedure previously outlined for the preparation of fillet samples should
generally be followed. Unless specifically sought as a sample, the dark muscle
tissue that may exist in the vicinity should not be separated from the light muscle
tissue.
Samples should be frozen after resection and kept at -20°C. Samples may or may
not be homogenized before acid digesbon and subsequent preparation before
analysis.
ASTM Method D4309 also describes the preparation of biological samples for
inorganic chemical analysis (ASTM, 2001 a).
This method is followed by investigators preparing fish tissue for trace metal analysis.
Control of metal contamination is addressed in this
method.
The major difficulty in trace metal analyses of tissue samples is controlling
contamination of the sample after collection. In the field, sources of contamination
include sampling gear, grease from winches or cables, engine exhaust, dust or ice
used for cooling. Sample resection and any subsampling of the organisms should be
carried out in a controlled environment (i.e.. a Class 100 clean room).
USEPA. 1993c. Fish Field and Laboratory Methods for Evaluating the Biological
Integrity of Surface Waters, EPA-600-R-92-11 1 . Office of Research and
Development, U.S. Environmental Protection Agency, Washington, DC.
http.//www epa qov/bioindicators/html/fish metho
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2.3.2-2
Total Mercury in Tissue, Sludge, Sediment, and Soil by Acid Digestion and BrCI
Oxidatbn, Appendix to Method 1631
These procedures may be used in conjunction with EPA Method 1631 B for
determination of mercury in tissue, sludge, sediment, soil, industrial samples, and
certified reference materials.
Digestion I— This procedure is preferred for matrices containing organic materials,
such as sludge and plant and animal tissues, because the organic matter is
completely destroyed. In this procedure, a 0.2 - 1.5 g sample is digested with
HNOj/H2SO4. The digestate is diluted with BrCI solution to destroy the remaining
organic material.
Digestion II— This procedure is preferred for geological materials because of rapid
and complete dissolution of cinnabar (HgS), which is otherwise more slowly
attacked by the BrCI in Digestion I. In this procedure, a 0.5 - 1.5 g sample is
digested with aqua regia (HCI/HNO3 ) to solubilize inorganic materials.
The Hg concentration in the digestate is determined using EPA Method 1631 B.
These procedures, in conjunction with Method 1631B, allow determination of Hg
at concentrations ranging from 1.0 to 5000 ng/g in solid and semisolid matrices.
The method detection limit for Hg has been determined to be in the range of 0.24
to 0.48 ng/g when no interferences are present. The minimum level of
quantization (ML) has been established as 1.0 ng/g. These levels assume a
sample size of 0 5 g.
Using Method LMMB 053 (USEPA, 1997d) to measure total mercury in fish, the
fish tissue is digested in nitric acid for 30 minutes at room temperature then in a
bomb at 190°C for 15 minutes. The digestate is diluted to 25 mL using Milh-Q
water and sample ahquots are analyzed using the CVAFS purge and trap method.
Specific procedures for the measurement of mercury in plankton are described in
Method LMMB 051 (USEPA, 1997d).
The extent of mercury bioaccumulation is an important parameter to support
human health, ecological risk assessments and bioaccumulation models.
The dual amalgam trap system and fluorescence detector provide greater
sensitivity and specificity in the presence of interferences, and this system must
be used to overcome interferences, if present, and to achieve the sensitivity
required, if necessary.
This method does not measure methyl mercury, which may need to be monitored
separately in contaminated sediments.
USEPA. 2001 d. Appendix to Method 1631: Total Mercury in Sludge, Sediment,
Soil, and Tissue by Acid Digestion and BrCI Oxidation, EPA-821-R-01-013. Office
of Water. U.S. Environmental Protection Agency, Washington, DC.
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2.3.2-3
Versatile Combustion-Amalgamation Technique for the Photometric Determination of
Mercury in Fish and Environmental Samples, LMMB 052
For the direct detection of total mercury in fish and environmental samples.
0.05 - 0.1 g fish tissue is heated in a stream of 02 for 3.5 minutes in an induction
furnace. The released mercury vapor passes through a series of traps, and the
mercury is collected in a 10 mm diameter column of 24-gauge gold wires. This
amalgam is heated in the induction furnace and volatilized mercury is measured with
a mercury vapor meter.
The detection limit is less than 0.002 ug.
The extent of mercury bioaccumulation is an important parameter to support human
health, ecological risk assessments and bioaccumulation models.
This analytical system is easily converted to handle biological materials, water, and
sediments. Total analysis time is about B minutes per sample and a single analyst
can make up to 40 determinations in eight hours. The method has high sensitivity,
precision, and accuracy. Also, a small sample size is required.
For analysis of samples outside the range of 0.02 - 5.0 ppm mercury, a change of
operating procedure is required. Frequent changes in attenuation of the mercury
vapor meter are required. The sample must be well homogenized, due to the very
small sample size analyzed with this method. Detection limits may not be sufficiently
low for ecological or human health risk assessments.
USEPA. 1997d. Method LMMB 052: Versatile Combustion-Amalgamation
Technique for the Photometric Determination of Mercury in Fish and Environmental
Samples, Lake Michigan Mass Balance Study Methods Compendium, Volume 2:
Organic and Mercury Sample Analysis Techniques, EPA 905-R-97-012c. Great
Lakes National Program Office, U.S. Environmental Protection Agency, Chicago, IL.
http //www epa qov/qlnpo/lmmb/methods/s
can odf
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2.32-4
Trace Element Quantification Techniques
To determine major and trace elements in sediment and biological tissue samples
utilizing atomic absorption and neutron activation techniques.
Tissue samples are homogenized and freeze dried, and a dry aliquot is
homogenized and transferred to a Teflon™ bomb. Samples are digested by adding 3
ml HNOj and leaving the bombs at room temperature overnight. The bombs are
then placed in a 130°C oven for approximately 20 hours. After cooling, 18 ml of
quartz distilled water are added, and the solution volume is determined, and a 20-fold
dilution is made for FAAS analysis of Al, Fe, Mn, Si, and Zn. For analysis of Hg,
sediment samples are digested using a modified version of EPA method 245.6.
Samples were analyzed using the following instrumentation:
Analvto Method
Hg Cold vapor atomic absorption (CVAA)
Cu, Fe, Zn Flame atomic absorption (FAA)
Ag, As, Cd, Cr, Cu, Ni, Pb, Se, Sn Graphite furnace atomic absorption
(GFAA)
AT, Cr, Fe. Se, Ag, Zn Instrumental neutron activation
analysis (INAA)
ASTM Method D1971 describes the digestion of samples for determination of metals
by Flame Atomic Absorption (ASTM, 2001 a).
Standard Method 3030K describes the microwave digestion method (APHA, 1999).
Several Standard Methods describe the analysis of metals using various methods:
SM 31 12 B for CVAA; SM 31 1 1 for FAA; SM31 13B for GFAA.
Methods provide low detection limits needed for measuring ambient concentrations
at uncontaminated sites, or reference sites.
Tissue sample digestion in a Teflon™ bomb is a standard method for "clean*
digestion for metals analysis. The instrumental suite employed in this method takes
advantage of the know strengths of each instrument for trace analysis. For example,
GFAA is much more sensitive than FAA, requiring only a small volume of sample for
trace analysis.
Requires multiple instrument analyses for results on a complete suite of elements.
NOAA 1998. Sampling and Analytical Methods of the National Status and Trends
Program, Mussel Watch Project: 1996 Update, NOAA Technical Memo NOS ORCA
130. National Oceanic and Atmospheric Administration, Silver Spring, MO. 233 pp.
http.//ccma nos noaa qov/publications/tm Last Accessed: 1/31/2003
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2.3.2-5
Analysis of Marine Sediment and Bivalve Tissue by X-Ray Fluorescence,
Atomic Absorption and Inductively Coupled Plasma Mass Spectrometry
To determine the concentration of 17 metals in sediment and biobgical tissue
samples utilizing atomic absorption, inductively coupled plasma mass
spectrometry (ICP-MS), and energy dispersive X-Ray fluorescence (XRF).
Tissue samples are weighed and freeze-drted. The dried sample is ground in a
mill. 0.5 g aliquots are used directly for XRF analysis or are further digested for
AA or ICP-MS analysis.
500 mg of dried tissue is placed in a Teflon™ bomb, to which 5 mL of HCI and
3.5 mL of HN03 are added. The bombs are heated in a 60°C water bath for 3-4
hours. After cooling, the bombs are heated in a 130°C oven for 16 hours. After
cooling, the digestates are diluted to approximately 20 mL with deionized water.
Solution volumes are calculated, and the digestates are analyzed directly by
GFAA and CVAA or diluted 10:1 for ICP-MS analysis.
Analvte Method
Hg Cold vapor/gold foil amalgam
Al. Cd. Cr, Ni, Ag, Pb Graphite furnace atomic absorption (GFAA)
Ag, Al, Cr, Cd. Ni, Pb, Sb, Sn ICP-MS
As, Cu, Fe, Mn, Se, Si, Zn XRF
Several Standard Methods exist for the analysis of metals by a variety of
methods: 31 12B for CVAA; 31 13B for GFAA; 3120B for ICP-MS (APHA, 1999).
Metals contaminant data are used in both ecological and human health risk
assessments.
XRF analysis does not require digestion of the sample. Se and As. which can
be difficult to analyze in tissue by ICP-MS, are easier to analyze by XRF. The
digestion solution of HCI/HNO3 provide better recoveries for Ag. ICP-MS has
the advantage of simultaneous analysis of many elements with detection limits
much lower than the XRF and similar to those of GFAA. ICP-MS is particularly
sensitive for Al, Cr, Ni, Ag, Cd, Sn, Sb, P, and Tl. CVAA is very sensitive and
reliable for Hg analysis.
Leakage at high pressure can cause loss of Hg from the sample during
digeston. Analysis of GFAA requires the use of matrix modifiers and
standardization of the instrument by method of addition to the sample matrix to
provide accurate results.
NOAA. 1998. Sampling and Analytical Methods of the National Status and
Trends Program, Mussel Watch Project. 1996 Update, NOAA Technical Memo
NOS ORCA 130. National Oceanic and Atmospheric Administration, Silver
Spring, MD. 233 pp.
http://ccma nos noaa gov/publications/t Last Accessed- 1/3172003
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2.3.2-6
Chemical Speciation of Arsenic in Water and Tissue by Hydride Generation Quartz
Furnace Atomic Absorption Spectrometry, EPA Method 1632, Revision A
This method is for determination of inorganic arsenic (IA), arsenite (As +3 ), arsenate
(As +5 ), monomethylarsonic acid (MMA), and dimethylarsinic acid (DMA) in tissue
by hydride generation and quartz furnace atomic absorption detection. This method
is designed for measurement of As species in tissue in the range 0.10-500 ug/g dry
weight.
A 10- to 50-g wet weight sample is collected into a sample bottle. The tissue sample
is either freeze-dried and stored at room temperature or stored frozen at less than -
18°C. Prior to analysis, tissue samples are digested in HCI or NaOH at 80°C for 16
hours. An aliquot of tissue digestate is placed in a specially designed reaction
vessel, and 6M HCI is added. NaBH4 solution is added to convert IA. MMA. and DMA
to volatile arsines. Arsines are purged from the sample onto a cooled glass trap
packed with 15% OV-3 on Chromosorb ® W AW-DMCS, or equivalent. The trapped
arsines are thermally desorbed, in order of increasing boiling points and carried into
the quartz furnace of an atomic absorption spectrophotometer for detection. To
determine the concentration of As +3, another aliquot of water sample or tissue
digestate is placed in the reaction vessel and Tns-buffer is added. The procedure is
repeated to quantify only the arsine produced from As +3. The concentration of As
+5 is the concentration of As +3 subtracted from the concentration of IA
Analyte MDL ML
IA (As +3 +As +5 ) 0.03 ug/g 0.10 ug/g
Arsenite (As +3 ) 0.02 ug/g 0.10 ug/g
MMA 0.01 ug/g 0.05 ug/g
DMA . 0.04 ug/g 0.10 ug/g
The method is for use site characterizations and risk assessments.
The relative amounts of carcinogenic arsenite (As +3) to total arsenic varies with
surface water body and varies with pH. This method directly quantifies arsenite.
This method is far more costly than total arsenic determination and may only be
needed where speciation is required.
USEPA. 2001 c. Method 1632, Revision A: Chemical Speciation of Arsenic in Water
and Tissue by Hydride Generation Quartz Furnace Atomic Absorption Spectrometry,
EPA 821-R-01-006. Office of Water. U.S. Environmental Protection Agency,
Washington, DC
http //www brooksrand com/methods/1632a pdf Last Accessed: 1/31/2003
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2.3.2-7
Extraction and Lipid Separatbn of Fish Samples for Contaminant Analysis and Lipid
Determination, LMMB 043
To prepare tissue samples for the measurement of organic contaminants, such as
polychlorinated biphenyts, polynuclear aromatic hydrocarbons, and chlorinated
pesticides.
Using Method LMMB 043 (USEPA, 1997d), 10 g of tissue are combined with sodium
sulfate. The tissue mixture is transferred to a rinsed chromatography column that is
plugged with glass wool.. The tissue is extracted twice by eluting the column with 50
mL of a 90/10 petroleum ether/ethyl acetate mixture. The elutant is concentrated
using a Turbovap. A GPC column is used to remove lipids from the extract.
Samples are solvent exchanged into iso-octane and cleaned up using a silica gel
column. Extracts are eluted using a 5/95 ethyl acetate/hexane solvent mixture.
Samples are concentrated for analysis.
Using NS&T procedures (NOAA, 1998), a 0 5 - 1 5 gram (wet weight) aliquot of the
homogenized tissue sample is spiked with surrogate standards and extracted three
times with dichtoromethane in the presence of sodium sulfate by maceration with a
Tissumizer™, The extract is filtered through glass wool and sodium sulfate after
each extraction. The extract is concentrated using the Kuderna-Danish technique
and solvent changed to hexane. The sample is cleaned-up using alumina/silica gel
column chromatography before instrumental analysis. Tissue samples require
further purification by gel permeation chromatography (GPC) prior to instrumental
analysis for pesticides and PCBs. The sample is concentrated to 1 mL in hexane for
analysis.
US EPA's Fish Field and Laboratory Methods for Evaluating the Biological Integrity of
Surface Waters (USEPA, 1993c) also describe sample preparation methods for
organic contaminants in tissue.
Tissue contaminant data are used to delineate the spatial and temporal extent of
contamination and used in ecological and human health risk assessments.
This method provides quantitative extraction of most organic contaminants from
tissue samples, including those with high lipid contents.
These extraction methods have been validated for non-polar persistent organic
contaminants, such as PCBs, chlorinated pesticides, and PAHs. Methods may not
be applicable for more polar compounds or more reactive compounds.
USEPA. 1997d. Method LMMB 043: Extraction and Lipid Separatbn of Fish
Samples for Contaminant Analysis and Lipid Determination. Lake Michigan Mass
Balance Study Methods Compendium, Volume 2" Organic and Mercury Sample
Analysis Techniques. EPA 905-R-97-012c. Great Lakes National Program Office,
U.S. Environmental Protection Agency, Chicago, IL.
htlp //www epa gpv/glnpo/lmmb/methods/hc521a pdf
Last Accessed: 1/31/2003
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Method Summary
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Limitations
Reference
Website
2.3.2-8
Purification of Biobgical Tissue Samples by Gel Permeation Chromatography of
Organic Analyses
To purify tissue extract samples by separating out lipids and high molecular
weight components from target compounds.
The GPC/HPLC is calibrated to verify the instrument performance based on
retention time and area of each of the calibration standards. Sample extracts are
processed through a guard column and two size exclusbn columns connected in
series and the desired fraction is collected with a fracton collector. The collected
fracton is then concentrated and analyzed for polycyclic aromatic hydrocarbons,
pesticides, and polychlonnated biphenyls.
This method is a clean-up step used in the processing of organic contaminant
sample extracts for GC/MS or GC/ECD analysis.
A large amount of neutral lipids and high molecular weight components from
tissue samples can be eluded from an alumina/silica gel column
Chromatography clean up step. Size exclusion Chromatography can separate
the target analytes from these other components. Upon calibration, this method
is also suitable for the isolation of other classes or organic contaminants.
This method isolates organic contaminants from lipid matrix but does not
separate or isolate individual fractions of organic contaminants.
NOAA. 1998. Sampling and Analytical Methods of the National Status and
Trends Program, Mussel Watch Project: 1996 Update, NOAA Technical Memo
NOS ORCA 130 National Oceanic and Atmospheric Administration, Silver
Spring, MD. 233 pp.
http.//ccma.nos noaa qov/oublications/t
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Data Uses/Application
Advantages
Limitations
Reference
Website
2.3.2-9
Quantitative Determination of Polynuclear Aromatic Hydrocarbons by Gas
Chromatography/Mass Spectrometry (GO/MS) - Selected Ion Monitoring (SIM)
Mode
To determine low concentrations of polycyclic aromatic hydrocarbons (PAHs)
and their alkylated homologues in extracts of water, sediments and biological
tissues.
Just prior to analysis, an aliquot of internal standard solution is added to the
sample extract producing a final internal standard concentration of
approximately 40 ng/mL. The analytical system includes a temperature
programmable gas chromatography with a fused silica capillary column.
Helium is used as the carrier gas, and the samples are handled by an auto
sampler capable of making 1 - 4 ul injections. A five point calibration curve is
established to demonstrate the linear range of the detector. The effluent from
the GC capillary column is routed directly into the ion source of the mass
spectrometer (MS). The MS is operated in the SIM mode using appropriate
windows to include the quantization and confirmation masses for target PAHs.
For all compounds detected at a concentration above the MDL, a confirmation
ion is checked to confirm its presence. The response factors of the surrogate
relative to each of the calibration standards are calculated, followed by the
calculation of the sample extract concentration. The sample concentration for
each compound is calculated by dividing the sample extract concentration by
the sample amount.
PAH data obtained from this analysis are used for site characterization and site
assessment.
GC/MS in the SIM mode provides unambiguous and sensitive detection for
PAHs. The PAH quantization method is very rigorous because PAHs have
very strong molecular ion peaks under the mass spectrometric conditions
used. Also, the availability of labeled surrogates internal standards of many of
the analytes makes very accurate determinations of analyte concentrations
possible. Analysis of alkylated PAH homologues can provide site-specific
information that can be used in source identification or product identification.
GC/MS in SIM mode cannot be used for simultaneous screening for other
organic contaminants of similar polarity or volatility and cannot be used to
identify tentatively identified compounds (TICs).
NOAA. 1998. Sampling and Analytical Methods of the National Status and
Trends Program, Mussel Watch Project: 1996 Update. NOAA Technical Memo
NOS ORCA 130. National Oceanic and Atmospheric Administration, Silver
Spring, MD. 233 pp.
http.//ccma nos.noaa gov/publications/t Last Accessed. 1/31/2003
m130odf
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Reference
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2.3.2-10
Analysis of Polychlorinated Biphenyls and Chlorinated Pesticides by Gas
Chromatography with Electron Capture Detection, LMMB 041
To quantify chlorinated hydrocarbons (i.e., chlorinated pesticides and PCBs) in
sample extracts.
This method is based on high resolution, capillary gas Chromatography using
electron capture detection (GC/ECD). Extracts normally have a holding time of
40 days. The instrument's detector is calibrated before the sample in injected.
Pestbide/PCB calibration is done also as part of the analytical run. If the
response for any peak exceeds the highest calibration solution, the extract is
diluted, a known amount of surrogate and TCMX solution added, and the sample
reanalyzed for those analyles that exceeded the calibration range.
Concentrations in the samples are calculated based on the internal standard
method. Data is reported as ng/g dry weight.
Other methods describing the analysis of PCBs and pesticides by GC/ECD are
NS&T methods, ASTM Methods D5317 and D3S34, and SW846 Methods 8081 A
and 8082 (NOAA, 1998; ASTM, 2001 c)
Data are used in site characterization and in risk analysis
The ECD is very sensitive and allows for detection of the chlorinated
hydrocarbons at trace concentrations (ppb).
The detector does not have a linear response over a wide concentration
range and must be used by sufficiently trained personnel. Second column
analysis must be performed to provide unequivocal compound identification.
These methods do not measure the 12 World Health Organization congeners,
which may be desired data in some risk assessments.
USEPA. 1997d. Method LMMB 041 : Analysis of Polychlorinated Biphenyls and
Chlorinated Pesticides by Gas Chromatography with Electron Capture Detection.
Lake Michigan Mass Balance Study Methods Compendium, Volume 2: Organic
and Mercury Sample Analysis Techniques, EPA 905-R-97-012c. Great Lakes
National Program Office, U.S. Environmental Protection Agency, Chicago. IL.
http //www epa qov/qlnpo/lmmb/methods/sop- Last Accessed: 1/31/2003
501 Pdf
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Advantages
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2.3.2-11
Tetra- through Octa-Chlorinated Dioxins and Furans by Isotope Dilution
HRGC/HRMS. EPA Method 1613
This method is for determination of tetra- through octa-chlorinated dibenzo-p-
dioxins (CDDs) and dibenzo furans (CDFs) in tissue.
This method is 'performance-based." The sample is extracted by one of two
procedures:
LSoxhlet or SDS extraction— A 20 g aliquot of sample is homogenized, and
a 10 g aliquot is spiked with the labeled compounds. The sample is mixed with
sodium sulfate, allowed to dry for 12-24 hours, and extracted for 18-24 hours
using methylene chloride:hexane (1:1) in a Soxhlet extractor. The
extract is evaporated to dryness, and the lipid content is determined.
2.HCI digestion — A 20 g aliquot is homogenized, and a 10 g aliquot is placed in
a bottle and spiked with the labeled compounds. After equilibration, 200 ml of
hydrochloric acid and 200 mL of methylene chloride:hexane (1:1) are added,
and the bottle is agitated for 12-24 hours. The extract is evaporated to dryness,
and the lipid content is determined. After extraction, 37CI4-labeled 2,3,7 ,8-TCDD
is added to each extract to measure the efficiency of the cleanup process.
Sample cleanups may include back-extraction with acid and/or base, and gel
permeation, alumina, silica gel. Florisil and activated carbon chromatography.
High-performance liquid chromatography (HPLC) can be used for further
isolation of the 2,3,7,8-isomers or other specific isomers or congeners. After
cleanup, the extract is concentrated to near dryness. Immediately prior to
injection, internal standards are added to each extract, and an aliquot of the
extract is injected into the instrument. The analytes are separated by the GC
and detected by a high-resolution (al 0,000) mass spectrometer.
CDD/CDF ML(pg/pL) CDD/CDF ML(pg/uL)
2.3.7 ,8-TCDF 0.5 1. 2,3.4.7 ,8-HxCDD 2.5
2.3,7 ,8-TCDD 0.5 1, 2,3.6,7 ,8-HxCDD 2.5
1. 2,3,7 ,8-PeCDF 2.5 1, 2,3,7 ,8.9-HxCDD 2.5
2.3,4 ,7,8-PeCDF 2.5 1,2,3,4,6.7,8-HpCDF 2.5
1, 2,3.7 ,8-PeCDD 2.5 1, 2,3,4.7 ,8,9-HpCDF 2.5
1, 2,3,4 ,7,8-HxCDF 2.5 1,2,3,4 .6,7 ,8-HpCDD 2.5
1. 2,3.6.7 ,8-HxCDF 2.5 OCDF 5.0
1, 2,3,7 ,8,9-HxCDF 2.5 OCDD 5.0
2,3,4,6,7,8-HxCDF 2.5
This method is also described in SW846 Method 8290
The method is for use in EPA's data gathering and monitoring programs
associated with the Clean Water Act. the Resource Conservation and Recovery
Act, the Comprehensive Environmental Response, Compensation and Liability
Act, and the Safe Drinking Water Act.
Method 1613 is able to meet detection limits required for human health and
ecological risk assessments.
The GC/MS portions of this method are for use only by analysts experienced
with HRGC/HRMS or under the close supervision of such qualified persons.
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2.3.2-11 (contd.)
USEPA. 1994c. Method 1613: Tetra- through Octa-Chlorinated Dioxins and Furans
by Isotope Dilution HRGC/HRMS, EPA 821-B-94-005. Office of Water, U.S.
Environmental Protection Agency, Washington, DC.
http://www eoa qov/waterscience/methods/16
13pdf
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Advantages
Limitations
Reference
Website
2.3.2-12
Toxic Polychlorinated Biphenyls by Isotope Dilution High Resolution
Gas Chromatography/High Resolution Mass Spectrometry, EPA Method 1668
This method is for determination of the toxic polychlorinated biphenyls (PCBs) in
solids (not tissue).
This method is performance-based. A 20-g aliquot of sample is homogenized,
and a 10-g aliquot is spiked with the labeled compounds. The sample is mixed
with sodium sulfate, allowed to dry for 12- 24 hours, and extracted for 18-24
hours using methylene chloride: n-hexane (1:1) in a Soxhlet extractor. The
extract is evaporated to dryness, and the lipid content is determined. After
extraction, samples are cleaned up using back-extraction with sulfunc acid
and/or base, and gel permeation, silica gel, Florisil and activated carbon
chromatography. High-performance liquid chromatography (HPLC) can be used
for further isolation of specific isomers or congeners. After cleanup, the extract
is concentrated to near dryness. Immediately prior to injection, internal
standards are added to each extract, and an aliquot of the extract is injected
into the gas chromatography. The analytes are separated by the GC and
detected by a high-resolution (210,000) mass spectrometer.
Extract
IUPAC EMDL(ng/kg) EML (ng/kg) EML
(P9/HL)
77 0.5 2 1
123 4 10 5
126 10 4 5
118/167/156/157/169/180170/189 6 20 10
114 60 200 100
105 40 100 50
EMD: = Estimated Method Detection Limit; EML = Estimated Minimum Level
The method is for use in EPA's data gathering and monitoring programs
associated with the Clean Water Act, the Resource Conservation and Recovery
Act, the Comprehensive Environmental Response, Compensation and Liability
Act, and the Safe Drinking Water Act.
Method 1668 provides data for most, but not all, of the "dioxin-like" PCBs,
including those with the highest TEFs, as determined by the World Health
Organization. This method provides detection limits frequently required in risk
assessments.
The GC/MS portions of this method are for use only by analysts experienced
with HRGC/HRMS or under the close supervision of such qualified persons.
Method 1668 does not provide data for all of the "dioxin-like" PCBs, as does
Method 1668A.
USEPA. 1997e Method 1668: Toxic Polychlorinated Biphenyls by Isotope
Dilution HRGC/HRMS, EPA-821-R-97-001. Office of Water. U.S.
Environmental Protection Agency, Washington, DC.
http Wwww.epa gov/clanton/clhtml/pubtitl Last Accessed: 1/31/2003
eOW html
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Reference
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2 3.2-13
Chlorinated Biphenyl Congeners in Water, Soil, Sediment, and Tissue by
HRGC/HRMS. EPA Method 1668 Revision A
This method is for congener-specific determination of more than 150
chlorinated biphenyl (CB) congeners in solids (not tissue).
This method is performance-based. A 20-g aliquot of sample is homogenized,
and a 10-g aliquot is spiked with the labeled compounds. The sample is mixed
with anhydrous sodium sulfate, allowed to dry for 12 - 24 hours, and extracted
for-18- 24 hours using methylene chloride:hexane (1:1) in a Soxhlet extractor.
The extract is evaporated to dryness, and the lipid content is determined. After
extraction, a labeled cleanup standard is spiked into the extract which is then
cleaned up using back-extraction with su If uric acid and/or base, and gel
permeation, silica gel, or Florisil chromatography. Activated carbon and high-
performance liquid chromatography (HPLC) can be used for further isolation of
specific congener groups. Prior to the cleanup procedures cited above, tissue
extracts are cleaned up using an anthropogenic isolation column. After
cleanup, the extract is concentrated to 20 uL. Immediately prior to injection,
labeled injection internal standards are added to each extract and an aliquot of
the extract is injected into the gas chromatography (GC). The analytes are
separated by the GC and detected by a high-resolution (i 10.000) mass
spectrometer. Without interferences, EMDLs and EMLs will be, respectively,
0.5 and 1.0 ng/kg for soil, tissue, and mixed-phase samples, and EMLs for
extracts will be 0.5 pg/uL. EMD: = Estimated Method Detection Limit; EML =
Estimated Minimum Level
This method is for use in data gathering and monitoring associated with the
Clean Water Act, the Resource Conservation and Recovery Act, the
Comprehensive Environmental Response, Compensatbn and Liability Act,
and the Safe Drinking Water Act.
Method 1668A provides congener data that can be used for source
identification. Listed PCBs include the 12 World Health Organization "dioxin-
like" PCBs. The HRMS method provides lower EMDLs compared to ECD or
low resolution MS analyses and provides unequivocal congener identification.
The GC/MS portions of this method are for use only by analysts experienced
with HRGC/HRMS or under the close supervision of such qualified persons.
Solvents, reagents, glassware, and other sample processing hardware may
yield artifacts, elevated baselines, and/or lock- mass suppression causing
misinterpretation of chromatograms The natural lipid content of tissue can
interfere in the analysis of tissue samples for the CBs.
USEPA. 1999c. Method 1668. Revision A: Chlorinated Biphenyl Congeners in
Water, Soil, Sediment, and Tissue by HRGC/HRMS, EPA-821-R-00-002.
Office of Water, U.S. Environmental Protection Agency, Washington, DC.
http //www epa gov/region08/water/waste Last Accessed. 1/31/2003
water/biohome/biosolidsdown/methods/1
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Method Summary
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Limitations
Reference
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2.3.2-14
Determination of Percent Dry Weight for Tissues
To determine the percentages of dry weight and moisture in tissue samples.
A 0.5-1 g aliquot of homogenized sample is placed into a pre-weighed beaker
and weighed. The samples are dried for 24 hours in a drying oven set at 63-
65°C. Samples are placed in a desiccator and allowed to cool to room
temperature for at least 30 minutes. The samples are weighed. The samples
are put back in the oven for at least 2 hr after which they are removed from the
oven and allowed to cool for at least 30 min in a desiccator. The sample is
reweighed. If the difference between the first and second weighting is less than
± 0.02 g. the dry weight percent is calculated based on the last weighing. The
difference between the weight of the dried sample and that of the wet sample is
used to calculate the percent dry weight.
[Vial wt. + Drv samole wt.) - [Vial wt.l
Percent dry weight = [Vial wt. + Wet sample wt.] - [Vial wt.] X 100
Some exposure assessment models require concentration data on dry weight
basis.
National database of fish and contaminant data reported on dry weight basis
following this procedure.
None.
NOAA. 1998. Sampling and Analytical Methods of the National Status and
Trends Program, Mussel Watch Project: 1996 Update, NOAA Technical Memo
NOS ORCA 130. National Oceanic and Atmospheric Administration, Silver
Spring, MD. 233 pp.
http.//ccma nos noaa qov/publications/t
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Method Summary
Data Uses/Application
Advantages
Limitations
Reference
Website
2.3.2-15
Determination of Percent Lipid in Tissue
To determine the percent lipid (weight/weight basis) of a tissue.
An appropriate amount of sodium sulfate-dried tissue sample is extracted three
times with dichtoromethane (100 mL each time). An aliquot of 20 ml of the
extract is quantitatively removed for lipid determination. This aliquot is filtered,
further dried with sodium sulfate, and brought to a final volume of 1 ml in
dichloromethane. An aliquot of 100 uL was taken and evaporated to constant
weigh tr The residual weight of this dried 100 uL portion is used to calculate the
percent hpids of the sample based on the dry weight.
Lipid content has been found to be correlated to contaminant concentrations
for specific tissues and whole organisms.
National database of fish and bivalve contaminant data reported on lipid basis
following this procedure.
The Bligh and Dyer (1959) Method, using a different solvent system, provides
slightly different lipid values.
NOAA. 1998. Sampling and Analytical Methods of the National Status and
Trends Program, Mussel Watch Project: 1996 Update, NOAA Technical Memo
NOS ORCA 130. National Oceanic and Atmospheric Administration. Silver
Spring, MD. 233 pp.
http.//ccma nos noaa qov/Dublications/tm Last Accessed- 1/11/2003
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2.3.2-16
Method Title
Microwave Extraction of Marine Tissue for Semivolatile Organic Analytes, AED
LOP 2.03.030, Revisbn 0
Purpose
Microwave-assisted extraction of semi-volatile organic compounds from marine
tissue samples.
Method Summary
Homogenize the entire tissue sample using a tissue homogenizer. Determine dry
weight to wet weight ratio. Weigh approximately 1.0 g of homogenized sample into
preweighed aluminum pan. Place pan in drying oven and record weight at 24 and
48 hours. Using the dry/wet ratio, back-calculate the wet weight needed for each
sample, setting the dry weight constant between 0.8 and 1.0 g target dry weight.
Use the sample with the lowest dry/wet ratio (highest percent moisture) and back
calculate the wet weight for that sample (see A). Since the moisture content is not
the same for all the samples, the wet weight will also be different (see B). Adjust
the wet weight of all samples to be equivalent to the standardization samples by
adding hexane rinsed Dl water (see C).
A.: Target dry weight/(dry/wet ratio sample A) = grams wet sample A
B: Target dry weighV(dry/wet ratio sample B) = grams wet sample B
C: Grams wet sample A - Grams wet sample B = grams H20 added to
sample B.
Assemble and prepare extraction vessels according to operation manual (AED
uses a GEM MES-1000 microwave extraction system). Weigh samples directly
into the bottom of the liners. Standardize the wet weight for all samples by adding
hexane rinsed Dl water. Add internal standards (IS) as required. For samples < 1
g, grind sample with 5 g of sodium sulfate and transfer to extraction vessel. Add 30
mL of 20/80 hexane/acetone solvent mixture, stir gently with a Teflon spatula, and
insert the liner into a clean, dry, particle-free vessel body. Program the microwave
at 70% power, 200 psi, 30 minutes runtime; 15 minutes at pressure, and 115' C.
After the extraction, pour the top solvent layer from the extraction vessel into a pre-
solvent rinsed 250 ml separately funnel containing 80 ml of hexane rinsed Dl
water. Back extract the Dl/acetone; hexane phase in the separately funnel 3X with
hexane, using 10mL hexane for the first extraction and 5 mL each for the second
and third extractions. Combine the extracts and treat with sodium sulfate to
remove water.
Transfer the extract into a clean rinsed 200 mL Turbo-Vap® tube. Place the flask
into the Turbo-Vap® apparatus and turn on the unit. Adjust the associated
nitrogen pressure regulator to read approximately 5 psi. Reduce the sample
volume to approximately 1 mL. Adjust the Final volume to 1.0 mL with hexane.
Remove 0.1 mL into a preweighed aluminum pan forhpid weight determination.
Allow it to dry at room temperature for a minimum of 24 hours. Record the weight
of the pan plus sample.
Fractionate the sample using column chromatography with silicic acid.
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Website
2.3.2-16 (contd.)
Extracting semivolatile organic compounds from the tissue of aquatic fauna.
Extracts can be further processed by separation on silicic acid chromatography
procedures prior to analysis by gas criromatograpriy and/or
gas/chromatography/mass selective detector.
More time efficient and requires less solvent than other methods of semivolatile
organic compound extraction from tissue, such as sonicadon or maceration in
solvent
This procedure was written to meet the specific needs of the research program at
the U.S. EPS-Atlantic Ecology Division. It is not a U.S. EPA Standard Method and
must not be referred to as such. Mention of trade names or commercial products
does not constitute endorsement or recommendation for use.
Unpublished laboratory SOP. EPA NHEERL-AED, Narragansett Rl
N/A Last Accessed:
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2.3.3 Biological Analysis Methods
Section 2.3.3 provides a compendium of biota-related biological analyses. Biota data like these
are often used to measure the status and trends of environmental pollution on freshwater,
estuarine, and marine macroinvertebrates to assess water quality criteria and monitor surface
water quality. Thus, many of these methods pertain to the analysis of samples collected in the field
to determine species abundance and taxa richness. Biological impairments resulting from pollution
are often evaluated using indices derived from the sampling data that evaluate matrices such as
community, population and functionality parameters. Other fact sheets pertaining to
histopathological analyses are often included.
The sources of information for the biological analyses fact sheets come from the following
agencies and offices:
The USEPA's EMAP Program
The USEPA's Environmental Research Laboratory-Narragansett,
The USEPA's Great Lakes Program Office
NOAA's Status and Trends Program
The USEPA's Office of Water
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Fact Sheet No.
2.3.3-1
Method Title
Laboratory Identification. Enumeration and Biomass Measurements of Periphyton in
Wadeable Streams
Purpose
To determine periphyton species composition and/or biomass in the laboratory
Method Summary
The standard laboratory-based method provides the option of sampling natural
substrates in a few different ways. Regardless of the sampling strategy, the samples
are returned to the laboratory where they are homogenized, sorted, identified and
counted in order to derive relative abundance and taxa richness data. "Soft" (non-
diatom) samples are homogenized with a tissue homogenizer or a blender. These
thoroughly mixed samples are placed in Palmer counting cells. Approximately 300
algal "cell units" are counted and identified to the lowest possible taxonomic level at
400x magnification. Relative abundances of soft algae are determined by dividing the
number of cells counted for each taxon by the total number of cells counted.
Diatom samples are subsampled and oxidized. The diatoms are then mounted on a
high refractive index medium to make permanent slides. Diatom valves are counted
and identified to the lowest possible taxonomic level, which should be species and
perhaps variety level, under oil immersion at 1000X magnification. At minimum, count
600 valves (300 cells) and at least unbl 10 valves of 10 species have been observed.
Relative abundances of diatoms have to be corrected for the number of live diatoms
observed in the count of all algae. To determine the relative abundance of diatom
species in the algae assemblage, divide the number of valves counted for each
species by the total number of valves counted; then multiply the relative abundance of
each diatom taxon in the diatom count by the relative abundance of live diatoms in the
count of all algae.
USEPA's EMAP document describes a similar method for enumerating and measuring
periphyton from wadeable streams (USEPA, 1998).
Data
Uses/Application
Species relative abundance and taxa richness are data derived from these protocols.
These data parameters provide information pertaining to the status and trends of
environmental pollution and its impacts on freshwater, marine and estuarine
communities.
Biological impairment resulting from pollution is often evaluated using metrics of biotic
integrity derived from the aforementioned data parameters that evaluate community,
population and functional parameters. Examples of metrics based on species
composition include species richness, total number of genera, total number of
divisions, shannon diversity (for diatoms), percent community similarity of diatoms,
pollution tolerance index for diatoms, and percent sensitive diatoms. Furthermore.
other metnces infer ecological conditions based on documented preferences. These
metrices include the percent aberrant diatoms, percent motile diatoms, simple
diagnostic metrics, inferred ecological conditions with simple autecological indices
(SAI), inferred ecological conditions with weighted average indices, and impairment of
ecological conditions.
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Advantages
Limitations
Reference
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2.3.3-1 (contd.)
The laboratory-based survey is more accurate in assessing biotic integrity and in
diagnosing causes of impairment than the field-based survey.
The laboratory-based methods require more time and effort than the field evaluation.
Barbour era/. 1999. Rapid Bioassessment Protocols for Use in Streams and
Wadeable Rivers: Periphyton, Benthic Macroinvertebrates and Fish, Second Edition,
EPA 841-B-99-002. Office of Water, U.S. Environmental Protection Agency,
Washington, D.C.
htto //www eoa aov/owowwlrl/rnonitonna/rbp/inde
x html
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Method Title
Purpose
Method Summary
Data Uses/Application
Advantages
Limitations
Reference
Website
2.3.3-2
Laboratory Periphyton Biomass Determination
To determine periphyton biomass in the laboratory.
To quantify algal biomass, the area of the substrate sampled must be
determined. Periphyton biomass can be estimated with chlorophyll a, ash-free
dry mass, cell densities, and biovolume, usually per cm2. Each of these
measures estimates a different component of periphyton biomass.
Chlorophyll a: Extract in acetone and measure eh I concentration in the extract
with a spectrophotometer or fluorometer. Calculate the chlorophyll a density on
substrates by determining the proportion of original sample that was assessed
for chlorophyll a.
Ash-Free Dry Mass: A measurement of the organic matter in samples. At
detailed description of the process is beyond the scope of this fact sheet, but
standard methods are readily available (APHA, 1999. USEPA 1995). It is a
fairly simple analysis. It is recommended over dry mass measurements
because silt can account for a substantial proportion of dry mass in some
samples.
Area-Specific Cell Densities and Biovolumes: Cell densities are determined by
dividing the numbers of cells counted by the proportion of sample counted and
the area from which the samples were collected. Cell biovolumes are
determined by summing the products of cell density and biovolume of each
species counted and dividing that sum by the proportion of sample counted and
the area from which the samples were collected.
USEPA EMAP provides similar guidance for laboratory periphyton biomass
determination (USEPA, 1998).
Biomass may be especially important in studies that address nutrient
enrichment or toxicity.
Periphyton biomass provides information on standing crop, which is useful for
assessing the biobgical integrity of streams.
In many cases, sampling benthic algae misses peak biomass, which may best
indicate nutnent problems and potential for nuisance algae growths.
Barbour era/. 1999. Rapid Bioassessment Protocols for Use in Streams and
Wadeable Rivers: Periphyton, Benthic Macromvertebrates and Fish, Second
Edition. EPA 841-B-99-002. USEPA. Office of Water. Washington DC.
http.//www epa gov/owowwtr1/monitorinq/rbp/md Last Accessed- 1/31/2003
ex html
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Method Title
Purpose
Method Summary
Data Uses/Application
Advantages
Limitations
2.3.3-3
Laboratory Analysis of Benthic Macroinvertebrates in Wadeable Streams
To determine macroinvertebrate diversity and abundance.
Following sample collection, the sediment is sieved and preserved in a 10%
buffered formalin solution, however different mixtures should be used for soft-
bodied organisms (i.e., leeches, aquatic oligochaete, and other soft-bodied
organisms.
Samples are sorted by hand in the laboratory using a low power (2x) scanning
lens or a stereomicroscope. Approximately one or two tablespoonfuls of the
sample are placed in a white enamel pan filled about one-third full of water.
Ethanol-preserved organisms should float to the top and be removed from the
dish as a sub-sampling procedure. Various staining methods may also be used
for sub-sampling.
Microscope slide mounts are then prepared for all or parts of organisms for
identification purposes. These slides are then identified to a specific taxonomic
level. For water quality and pollution analyses, it is important that organisms are
identified to the species level. As organisms are identified, the individuals in
each taxonomic category are counted and the numbers are recorded in
laboratory bench sheets.
Subsampling of benthic samples is not a requirement and is often discouraged
by certain scientists. However, Rapid Bioassessment Protocols recommend a
fixed-count approach to subsampling and sorting the organisms based on the
sample matrix of detritus, sand and mud. This approach calls for sieving
samples as described above and then removing all material in four randomly
selected grids contained the sieved sample. The organisms in these four grids
are enumerated and identified to the lowest possible taxonomic level.
Several USEPA EMAP documents describe similar protocols to determine
macroinvertebrate diversity and abundance (USEPA, 1990b; USEPA, 2000b;
USEPA, 1995).
Macroinvertebrate data such as these are used to measure the status and
trends of environmental pollution. Biological impairment resulting from pollution
is often evaluated using indices derived from the sampling data that evaluate
matrices such as community, population and functional parameters.
Examples of indices often derived from the data include the Hilsenhoffs Family
Biotic Index (HBI), Invertebrate Community Index (ICI), Community Similarity
Indices. Community Loss Index, and the Ohio EPA Invertebrate Community
Index.
Laboratory analysis of benthic macroinvertebrate samples is costly and requires
a high degree of taxonomic expertise.
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Fact Sheet No.
Reference
Website
2.3.3-3 (contd.)
Barbouref a/. 1999. Rapid Bioassessment Protocols for Use in Streams and
Wadeable Rivers: Periphyton, Benthic Macroinvertebrates and Fish, Second
Edition, EPA 841-B-99-002. Office of Water. U.S. Environmental Protection
Agency, Washington, D.C.
httpV/www eoa qov/owowwtr1/monitorinq/rbD/ind
ex html
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Method Title
Purpose
Method Summary
Data
Uses/Application
Advantages
Limitations
Reference
2.3.3-4
Laboratory Analysis of Water Column Organisms
To determine composition and abundance from drift net or stream-net samplers.
The organism's collected by drift nets or stream-net samplers are emptied directly
into a white enamel pan or small bucket. The organisms can then be hand-picked
into a sample container and filled three-fourths full of preservative (70-80% ethyl
alcohol), however different mixtures should be used for soft-bodied organisms
(i.e., leeches, aquatic oligochaete, and other soft-bodied organisms). Sample
containers should be large enough so that they are not over one-half full of the
washed sample before the preservative is added.
Samples should be sorted by hand in the laboratory using a low power (2x)
scanning lens or a stereomicroscope). Approximately one or two tablespoonfuls
of the sample will be placed in a white enamel pan filled about one-third full of
water. Ethanol-preserved organisms should float to the top and be removed from
the dish as a sub-sampling procedure. Various staining methods have also been
used for sub-sampling.
Microscope slide mounts are then prepared for all or parts of organisms for
identification purposes. These slides are then identified to a specific taxonomic
level depending on the needs, experience and available resources. For water
quality and pollution analyses, it is important that organisms are identified to the
species level. As organisms are identified, the individuals in each taxonomic
category are counted and the numbers are recorded in laboratory bench sheets.
Macroinvertebrate data such as these are used to measure the status and trends
of environmental pollution on freshwater, estuarine, and marine
macrolnvertebrates, to assess water quality criteria, and monitor surface water
quality. Biological impairment resulting from pollution is often evaluated using
indces derived from the sampling data that evaluate matrices such as
community, population and functional parameters. Examples of indices often
applied include the Hilsenhoff Biotic Index (HBI), Invertebrate Community Index
(ICI), Community Similarity Indices. Community Loss Index, and the Ohio EPA
Invertebrate Community Index .
Macroinvertebrate biomass (weight of organisms per unit area) is a useful
measure of standing crop which is useful in assessing the biological integrity of
surface waters. The results of this analysis feed into the commonly accepted
incdices used to evaluate community health.
Taxonomic analysis requires a team of highly experienced technicians and/or
scientists.
USEPA. 1990b. Macroinvertebrate Field and Laboratory Methods for Evaluating
the Biological Integrity of Surface Waters, EPA/600/4-90/030. Office of Research
and Development, Washington, D.C.
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2.3.3-4 (contd)
htlo //www eoa aov/clanton/clhtml/DubtrtleOR
Dhtml
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Purpose
Method Summary
Data Uses/Application
Advantages
Limitations
Reference
Website
2.3.3-5
SOP-2: Lab Analysis of Lake Trout Stomachs and Data Entry; Appendix B.
Standard Operating Procedure for Lab Analysis of Coho Salmon Stomachs and
Data Entry, LMMB 026 - Appendix 2 & LMMB 027 - Appendix B
To examine and quantify the contents of lake trout and coho salmon stomachs.
Lake trout stomachs: Prey fish in the stomachs are identified, measured (nearest
mm) and weighed (nearest 0.1 kg). The percent digested state is recorded.
Measures of length include: maximum total length, standard length, vertebral
column length, .and length of a multiple of 5 vertebrae. Fish or parts of fish that
cannot be positively identified are recorded as unidentified remains.
Invertebrates are identified, grouped by taxa, and weighed as a taxon group.
The number of individuals in each group is enumerated. Stomach contents are
repackaged and frozen. Using the weight and length of intact prey, conversion
equations are developed to reconstruct total prey length and weight from partial
length measures
Coho salmon stomachs: The stomach is rinsed with rinse water to remove
excess formalin. Prey fish in the stomachs are identified, measured (nearest
mm) and weighed (nearest 0.1 g (large items and 0.02 g for small items) The
percent digested state is recorded. Measures of length include: maximum total
length, standard length, vertebral column length, and length of as many
vertebrae as possible. Invertebrates are identified, grouped by taxa, and
weighed as a taxon group. The number of individuals in each group is
enumerated. The average length and digested state of each taxon group is
recorded. If identification of a prey item is uncertain, the item is examined by a
second identifier and compared to a reference collection of diet items. During
the analysis, examples of each species of prey fish and taxonomic group of
invertebrate is set aside and preserved in 5% formalin. Stomach contents are
repackaged and preserved. Using the weight and length of intact prey,
conversion equations are developed to reconstruct total prey length and weight
from partial length measures.
Standard Method 10600D.2 also discusses diet analysis offish (APHA, 1999).
Stomach content data of upper trophic level fish are important to understand
exposure pathways.
Standardized method enhances uniformity of data.
N/A
USEPA. 1997b. Methods LMMB 026 -Appendix 2 & LMMB 027 -Appendix B.
Lake Michigan Mass Balance Study Methods Compendium, Volume 1: Sample
Collection Techniques, EPA 905-R-97-012c. Great Lakes National Program
Office, U.S. Environmental Protection Agency, Chicago, IL
Last Accessed: 1/31/2003
http //www epa qov/qlnpo/lmmb/methods/qappf
ish pdf
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Method Title
Purpose
Method Summary
Data Uses/Application
Advantages
Limitations
Reference
Website
2.3.3-6
Gonadal Analysis
A method to determine the reproductive stage of oysters, mussels, and zebra
mussels.
A semi-quantitative histological approach is used to rank reproductive stage. For
oysters and mytilid mussels, a dorsal-ventral slice of tissue is taken and fixed in
Davidson's fixative (48 hours for oysters and 1 week for mussels). Zebra
mussels are fixed whole in Davidson's fixative for one week, decalcified with
acetic acid, and embedded whole. Tissue samples are embedded in paraffin,
sectioned at a 5-pm thickness, and stained using a pentachrome staining
protocol. Unstained sections may be used for histopathobgical analysis.
Stained sections are examined under a compound microscope. Sex and state of
gonadal development are determined. The stage of the gametogenic cycle is
assigned a numerical value. For mytilids and zebra mussels, a mean gonadal
index, ranging from 0 to 5, can be calculated by summing the individual stage
numbers. For oysters, the number of individuals with substantial gonadal
development are compared to those having little gonadal volume using an
egg/eggtess ratio.
This method helps to assess the physiological state of bivalve populations.
Analysis of reproductive stage is important in identifying differences in tissue
composition which might affect between site and interannual comparisons of
contaminant data.
The pentachrome staining procedure yields better differentiation of tissue types
and mucins. This analysis provides an assessment of sexual stage in the
gametogenic cycle, and if desired, allows for a concomitant histopathological
analysis, with a single sample preparation protocol.
The procedure cannot be performed on pooled samples, as is commonly done
for chemical parameters, but only on individuals.
NOAA. 1998. Sampling and Analytical Methods of the National Status and
Trends Program, Mussel Watch Project: 1996 Update, NOAA Technical Memo
NOS ORCA 130. National Oceanic and Atmospheric Administration, Silver
Spring, MD 233 pp.
http //ccma nos noaa gov/publications/t Last Accessed: 1/31/2003
m130 odf
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Purpose
Method Summary
Data Uses/Application
Advantages
Limitations
Reference
Website
2.3.3-7
Histopathotogical Evaluatbns of Target and Non Target Fish Species
To determine fish quality in Estuaries
Specimens for histopathotagy analysis are unpacked, logged in, and placed in
70% ethyl alcohol for at least 48 hours prior to examination. A careful visual
inspection is made of the fins and body surfaces. Any abnormalities are noted.
Thorough examinations of the eyes, branchial chambers, buccal cavity, visceral
organs is performed. Representative tissue samples are removed from either
fish or shellfish (USEPA and the Naval Construction Battalion Center, 1992) and
slides are prepared. These slides are then examined using a compound
research microscope to diagnose pathological conditions.
Histopathotogical evaluations provide data that can be used as a composite
index of the incidence of diseases and contaminant body burdens in selected
resident species. Microscopic examination can determine the presence or
absence of pathological changes and evaluate the health of the animal or its
exposure to contaminated material or infectious agents. Changes include
morphological alterations, variations in the normal staining characteristics, or a
change in the rate of occurrence of features (i.e., mitotic figures)
Histopathotogical investigations provide information on the relationship between
incidence of external abnormalities and internal histopathotogical abnormalities.
It is difficult to prove in a legal context that both external and internal
abnormalities are indicators of degraded environmental systems.
USEPA. 1995. Environmental Monitonng and Assessment Program (EMAP),
Laboratory Methods Manual, Estuaries. Volume 1 -Biological and Chemical
Analyses, EPA/620/R-95/008. Office of Research and Development. U.S.
Environmental Protection Agency, Washington, DC.
htto://www eDa.gov/emaD/html/pubs/docs/group Last Accessed: 1/31/2003
docs/estuarv/field/lab man odf
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Fact Sheet No.
Method Title
Purpose
Method Summary
Data Uses/Application
Advantages
Limitations
Reference
Website
2.3.3-8
Hislopathobgy Analysis
A quantitative or semi-quantitative method to determine the prevalence and
density of parasites, pathologies, and diseases afflicting oysters, mussels, and
zebra mussels.
Analyses are conducted on paraffin-embedded tissues sectioned at a 5-um
thickness and stained using a pentachrome staining procedure. Prepared slides
are examined individually under the microscope using a 10X ocular and a 10X
objective. Conditons evaluated are scored for intensity using either a
quantitative or semi-quantitative scale. Conditions scored quantitatively include
parasites, the number of ceroid bodies, incidences of tissue inflammation,
rickettsial bodies, incidences of tissue edema, and suspected neoplasms and
tumors. A running count of incidences of the condition is kept as the slide is
scanned, to avoid re-examining each slide multiple times for each separate
malady. Evaluation of conditions scored semi-quantitatively related to the
intensity of the effector the extensiveness of pathologies affecting large tissue
areas. Semi-quantitative measurement may require re-scanning portions of the
tissue for each malady type to completely assess the degree of tissue
involvement. Infection intensity of parasites, the occurrence and extensiveness
of tissue pathologies, and the intensity of diseases are recorded using semi-
quantitative or quantitative measures.
Histopathology is used to help assess the influence of contaminant exposure on
population health.
Infection intensity quantified by counts or semi-quantitative methods consistently
provides a more robust data set for statistical analysis.
Prevalence rarely provides an adequate description of the population dynamics
of disease and often yields ambiguous results.
NOAA. 1998. Sampling and Analytical Methods of the National Status and
Trends Program, Mussel Watch Project: 1996 Update, NOAA Technical Memo
NOS ORCA 130. National Oceanic and Atmospheric Administration, Silver
Spring, MD. 233 pp.
http //ccma nos noaa gov/puslications/tm Last Accessed- 1/31/2003
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Method Title
Purpose
Method Summary
Data Uses/Application
Advantages
Limitations
Reference
Website
2.3.3-9
Index of Biotic Integrity (IBI)
The IBI is used to identify and assess degraded and undegraded streams.
The steps in developing IBIs are the same for both fish and benthic
macroinvertebrates. Criteria for both reference and degraded sites were
determined based on water chemistry, physical habitat, and land use.
Ecologically-relevant geographic strata were determined using cluster analysis
and nonmetric multidimensional scaling. Candidate metrics were evaluated for
1) their ability to-discriminate (based on classification efficiency) between
reference and degraded sites, and 2) for redundancy. The final suite of metrics
used in the IBIs contained those ecologically significant metrics with the best
classification efficiency. Both IBIs were validated using an independent data set
and overall classification efficiencies were calculated.
An example of the metrices developed for the Fish Index of Biotic Integrity are
provided below:
• Number of native species
• Number of benthic species
• % tolerant individuals
% abundance of dominant species
• % generalists, omnivores and insect vores
• Number of individuals/square meter
• Biomass (grams/square meter) (used for coastal plain streams only)
• % lithophilic spawn ers
• % insectivores (used for non-coastal plain streams only)
IBIs are used to determine biological integrity based on characteristics of the
fish and benthic assemblage at a site. The results of these assessments are
used for watershed management decisions concerning strategies that will
control and minimize point and non-point sources of water pollution.
IBIs use multiple attributes to quantitatively assess stream health. It is a
systematic way in which to interpret data for management decisions.
Different states have developed similar, yet different IBIs. This makes it difficult
to compare the results from one state to another.
USEPA. 1997f. State of the Streams: 1995- 1997 Maryland Biological Stream
Survey Results, Mid-Atlantic Integrated Assessment. Office of Research and
Development, U.S. Environmental Protection Agency, Washington, D C.
http //www dnr state md.us/streams/pubs/ea-99-
6.pdf
Last Accessed: 1/31/2003
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Purpose
Method Summary
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Limitations
Reference
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2.33-10
Fish Bioassessment I and II
These bioassessment strategies use existing and new information in a
systematic manner to determine the health of the local fish community.
Fish Bioassessment I uses a questionnaire to serve as a screening tool to pool
the existing knowledge regarding fishery populations and health from the local
fish community.
The questionnaire polls state fish biologists and university ichthyologists believed
to be knowledgeable about the fish assemblages in stream reaches of concern.
Potential respondents are contacted initially by telephone to identify appropriate
respondents. Then the questionnaire is mailed to all respondents for completion
followed by follow-up mailings and telephone contact.
Questionnaire responses should provide information pertaining to the integrity of
the fish community, the frequency of limiting factors and causes, the frequency
and occurrence of particular fish community condition characterizations, the
geographic patterns of these variables, the temporal trends in the variables, the
effects of water body type and size on the spatial and temporal trends, the
likelihood of improvement and degradation and the major limiting factors. The
data are then analyzed and results are reported as histograms, pie graphs, or
box plots.
Based on the results of the Bioassessment 1 survey, Bioassessment II pursues
standardized field collection, species identification and enumeration, and
community analyses using biological indices or quantification of the biomass and
numbers of key species.
The questionnaire provides a qualitative assessment of a large number of water
bodies quickly an inexpensively Its quality depends on the survey design, the
questbns presented, and the knowledge and cooperation of the respondents.
The fish Bioassessment II survey yields an objective, discrete measure of the
health of the fish community. Data provided in this survey can be used to
develop biological criteria, prioritize sites for further evaluation, provide a
reproducible impact assessment, and monitor trends in fish community status.
Questionnaires can provide information that field surveys cannot such as
historical trends and conditions. Reid surveys can be oriented towards gathering
data in areas where data were missing historically.
Questionnaires are sometimes inaccurate due to hasty responses, they often
report conditions better than they are in reality, and the respondents have
insufficient knowledge to answer the questions.
USEPA. 1993c. Fish Field and Laboratory Methods for Evaluating the Biological
Integrity of Surface Waters. EPA/600/R-92. Office of Research and
Development, U.S. Environmental Protection Agency, Washington, D.C
hltp //www epa gov/biomdicators/html/fish_meth Last Accessed- 1/31/2003
ods hlml
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3.0 REFERENCES
APHA. 1999. Standard Methods for the Examination of Water and Wastewater, 20th Edition,
L.S. Clesceri and A.D. Eaton, Eds., American Public Health Association, Washington D.C.
ASTM. 2001 a. ASTM Book of Standards. Volume 11.01. American Society for Testing and Materials, West
Conshocken, PA.
ASTM. 2001b. ASTM Book of Standards. Volume 11.05. American Society for Testing and Materials, West
Conshocken, PA.
ASTM. 2001 c. ASTM Book of Standards. Volume 11.02. American Society for Testing and Materials, West
Conshocken, PA.
ASTM. 2001d. ASTM Book of Standards. Volume 03.06. American Society for Testing and Materials, West
Conshocken, PA.
ASTM. 2001e. ASTM Book of Standards. Volume 04.08. American Society for Testing and Materials, West
Conshocken, PA.
Barbour, M.T , J Gerritsen, B.D. Snyder, and J.B. Stribling. 1999. Rapid Bioassessment Protocols for Use in
Streams and Wadeable Rivers. Periphyton, Benthic Macroinvertebrates and Fish, Second Edition. EPA 841-
B-99-002. Off ce of Water. U.S. Environmental Protection Agency; Washington, D.C.
Battelle 2001 Natural Recovery of Persistent Organics in Contaminated Sediments at the Sangamo-
Weston/Twelvemile Creek/Lake Hartwell Superfund Site. USEPA National Risk Management Research
Laboratory Cincinnati, OH.
Bligh, E.G. and W.J. Dyer. 1959. A rapid method for total lipid extraction and purification. Canadian Journal of
Biochemistry and Physiology. 37:911.
Brannon, J.M., R.M. Engler, J.R. Rose, P.G. Hunt, and I. Smith. 1976. Selective Analytical Partitioning of
Sediments to Evaluate Potential Mobility of Chemical Constituents During Dredging and Disposal Operations,
WES Technical Report D-76-7. U.S. Army engineer Waterways Experiment Station, Vicksburg MS.
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A Compendium of Chemical, Physical and Biological Methods
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Environment Canada. 1990. Acute Lethality Test Using Rainbow Trout. EPS 1/RM/9 Environmental
Protection Service, Environment Canada, Ottawa, Ontario, Canada.
Environment Canada. 1990. Acute Lethality Test Using Daphnia spp.. EPS 1/RM/11 Environmental
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Environment Canada. 1992. Test of Reproduction and Survival Using the Cladoceran Ceriodaphnia dubia.
EPS 1/RM/21. Environmental Protecton Service, Environment Canada, Ottawa, Ontario, Canada.
Environment Canada. 1992. Test of Larval Growth and Survival Using Fathead Minnows. EPS 1/RM/22
Environmental Protection Service, Environment Canada, Ottawa, Ontario, Canada.
Environment Canada. 1992. Growth inhibition test Using the Freshwater Alga Selenastrum capricornutum.
EPS 1/RM/25. Environmental Protection Service, Environment Canada, Ottawa, Ontario, Canada.
Environment Canada. 1992. Fertilization Assay Using Echinoids. EPS 1/RM/27. Environmental Protection
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Environment Canada. 1997. Test for Survival and Growth in Sediment Using the Larvae of freshwater Midges
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Environment Canada. 1997. Test for Survival and Growth in Sediment Using the Freshwater Am phipod
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New Bedford Harbor Sediments Environmental Toxicology and Chemistry. 16, 551-558.
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Sewage Sludge Disposal at the 106-Mile Site: A Summary and Synthesis of Findings. Journal of Marine
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of Polycylic Aromatic Hydrocaibons Environmental Toxicology and Chemistry. Vol. 15:4. p 574-581.
246
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Lipscomb, S.W. 1995. Quality Assurance Plan for Discharge Measurements Using Broadband Acoustic
Doppler Current Profilers. USGS Open-File Report 95-701.
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Tested in the National Status and Trends Program. NOAA Tech. Memo. NOS OMA 62. National Oceanic and
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Sediment Quality Guidelines for Freshwater Ecosystems. Archives of Environmental Contamination and
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Unconsolidated Sediments. Geol. Surv. Prof. Pap. U.S.. 550-C- 256 - 261.
Murdoch, Alena and Jose M. Azcue. 1995. Manual of Aquatic Sediment Sampling. Lewis Publishers, Boca
Raton, FL 219pp.
NFESC. 2000. Rapid Characterization of Metals in Sediments Using X-Ray Fluorescence (XRF) Technology.
Naval Facilities Engineering Command, Washington DC.
NOAA. 1998. Sampling and Analytical Methods of the National Status and Trends Program, Mussel Watch
Project: 1996 Update, NOAA Technical Memo NOS ORCA 130. National Oceanic and Atmospheric
Administration, Silver Spring, MD. 233 pp.
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Puget Sound, Puget Sound Protocols and Guidelines. Puget Sound Water Quality Action Team, Olympia,
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Sarda, N. and G.A. Burton. 1995. Ammonia Variation in Sediments: Spatial. Temporal, and Method-Related
Effects. Environmental Toxicology and Chemistry. Vol 14: 9.
Sasson-Brickson, G. and G.A. Burton. Jr. 1991. In Situ and Laboratory Sediment Toxicity Testing with
Ceriodaphnia Dubia. Environmental Toxicology and Chemistry. Vol 10. P 201-207.
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Puget Sound Dredged Disposal Analysis (PSDAA) Program U.S Army Corps of Engineers. Seattle District,
U.S Environmental Protection Agency Region 10. Washington State Department of Natural Resources,
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USAGE Engineering and Design.1996. Soil Sampling Engineering Manual. EM 1110-1-1906. Department of
the Army, Washington D.C.
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247
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Settlement at Aquatic Disposal Sites. Environmental Effects of Dredging Technical Notes EEDP-01-5.
Waterways Experiment Station. U.S. Army Corps of Engineers. Vicksburg, MS.
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Monitoring of Aquatic Dredged Material Disposal Sites. EEDP-01-10. Waterways Experiment Station, U.S.
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USEPA. 2001 a. Method 245.7: Mercury in Water by Cold Vapor Atomic Fluorescence Spectrametry, Draft,
EPA 821-R-01-008. Off ice of Water, U.S. Environmental Protecton Agency, Washington, DC.
USEPA. 2001 b. Method 1630: Methyl Mercury in Water by Distillation, Aqueous Ethylation, Purge and Trap,
and CVAFS, EPA 821-R-01-020. Office of Water, U.S. Environmental Protection Agency, Washington. DC.
USEPA. 2001 c. Method 1632, Revision A: Chemical Speciation of Arsenic in Water and Tissue by Hydride
Generation Quartz Furnace Atomic Absorption Spectrometry, EPA-821-R-01-006. Office of Water, U.S.
Environmental Protection Agency. Washington, DC.
USEPA. 2001 d. Appendix to Method 1631: Total Mercury in Tissue. Sludge, Sediment, and Soil by Acid
Digeston and BrCI Oxidation, EPA-821-R-01-013. Office of Water. U.S. Environmental Protection Agency,
Washington, DC.
USEPA 2001 e. Method for Assessing the Chronic Toxicity of Marine and Estuarine Sediment-associated
Contaminants with the Amphipod Leptocheirusplumulosus. EPA 600/R-01/020. Office of Research and
Development, U.S. Environmental Protecton Agency, Washington, DC.
USEPA. 2000a. Bioaccumulation Testing and Interpretation for the Purpose of Sediment Quality Assessment:
Status and Needs, EPA 823-R-00-001. Office of Water and Office of Solid Waste, U.S. Environmental
Protection Agency, Washington, DC.
USEPA. 2000b Coastal 2000 Northeast Component: Field Operations Manual, Environmental Monitoring and
Assessment Program (EMAP). EPA/620/R-00/002. Office of Research and Development, U.S. Environmental
Protection Agency, Washington, DC.
USEPA. 2000c. Method 6200. Field Portable X-Ray Fluorescence Spectrometry for the Determination of
Elemental Concentrations in Soil and Sediment. Office of Solid Waste, U.S. Environmental Protection Agency,
Washington DC.
USEPA 2000d. Methods for Measuring the Toxicity and Bioaccumulation of Sediment-associated
Contaminants with Freshwater Invertebrates, EPA/600/R-99/064. Office of Science and Technology, U.S.
Environmental Protection Agency, Washington, DC.
USEPA 1999a. National Recommended Water Quality Criteria-Correction, EPA-822-Z-99-001. Office of
Water, U S. Environmental Protection Agency. Washington D.C.
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for Assessing and Monitoring the Remediation of Contaminated Sediment Sites February 17,2003
USEPA. 1999b. Method 1631, Revision B: Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor
Atomic Fluorescence Spectrometry, EPA821-R-99-005. Office of Water, U.S. Environmental Protection
Agency, Washington, DC.
USEPA. 1999c. Method 1668, Revision A: Chlorinated Biphenyl Congeners in Water, Soil, Sediment, and
Tissue by HRGC/HRMS, EPA-821-R-00-002. Office of Water, U.S. Environmental Protection Agency,
Washington, DC.
USEPA. 1999d. Innovative Technology Verification Report: Aquatic Research Instruments Russian Peat
Borer, EPA/600/R-01/010. Office of Research and Development, U.S. Environmental Protection Agency,
Washington, DC.
USEPA. 1999e. Sediment Sampling Technology: Art's Manufacturing & Supply, Inc. Split Core Sampler for
Submerged Sediments, Superfund Innovative Technology, Evaluation Program. EPA/600/R-01/009. Office of
Research and Development, U.S. Environmental Protection Agency, Washington, DC.
USEPA. 1998. EMAP: Surface Waters, Field Operations and Methods for Measuring the Ecological Condition
of Wadeable Streams. EPA/6201/R-94/004F. Office of Research and Development. U.S. Environmental
Protection Agency, Washington, DC.
USEPA and USAGE. 1998. Evaluation of Dredged Material Proposed for Discharge in Waters of the U S.-
Testing Manual, Inland Testing Manual, EPA 823-B-98-004. Office of Water. U.S. Environmental Protection
Agency, Washington, DC.
USEPA. 1997a. Ecological Risk Assessment Guidance for Superfund: Process for designing and Conducting
Ecological Risk Assessments, Interim Final. EPA 540-R-97-006. Office of Solid Waste and Emergency
Response, U.S. Environmental Protection Agency, Washington D.C.
USEPA. 1997b. Lake Michigan Mass Balance Study Methods Compendium, Volume 1: Sample Collection
Techniques, EPA 905-R-97-012c Great Lakes National Program Office, U.S. Environmental Protection
Agency, Chicago, IL.
USEPA. 1997c.Lake Michigan Mass Balance Study Methods Compendium, Volume 3: Metals,
Conventional^ Radio chemistry, and Biomonitoring Sample Analysis Techniques. EPA 905-R-97-012C. Great
Lakes National Program Office, U.S. Environmental Protection Agency. Chicago, IL.
USEPA. 1997d. Lake Michigan Mass Balance Study Methods Compendium, Volume 2: Organic and Mercury
Sample Analysis Techniques. EPA 905-R-97-012c. Great Lakes National Program Office, U.S. Environmental
Protection Agency. Chicago. IL.
USEPA. 1997e. Method 1668: Toxic Polychlonnated Biphenyls by Isotope Dilution HRGC/HRMS,
EPA-821-R-97-001. Office of Water, U.S Environmental Protection Agency, Washington, DC.
USEPA. 1997f. State of the Streams: 1995-1997 Maryland Biological Stream Survey Results. Mid-Atlantic
Integrated Assessment. Office of Research and Development. U.S. Environmental Protection Agency,
Washington, D.C.
USEPA. 1996a. Ecological Significance and Selection of Candidate Assessment Endpoints. EPA 540-F-95-
037. ECO Update (January 1996). Office of Solid Waste and Emergency Response, U.S Environmental
Protection Agency, Washington D.C.
USEPA. 1996b. Method 1639: Determination of Trace Elements in AmbientWaters by Stabilized
Temperature Graphite Furnace Atomic Absorption, EPA 821-R-96-006. Office of Water, U.S. Environmental
Protection Agency, Washington, DC
USEPA. 1996c. Method 1637: Determination of Trace Elements in AmbientWaters by Off-Line Chelation Pre-
concentration and Stabilized Temperature Graphite Furnace Atomic Absorption, EPA 821-R-96-004. Office of
Water, U.S. Environmental Protection Agency, Washington. DC.
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USEPA. 1996d. Method 1638: Determination of Trace Elements in Ambient Waters by Inductively Coupled
Plasma-Mass Spectrometry, EPA 821-R-96-005. Office of Water. U.S Environmental Protection Agency,
Washington, DC.
USEPA. 1996e. Method 1640: Determination of Trace Elements in Ambient Waters by On-Line Chelation Pre-
concentration and Inductively Coupled Plasma-Mass Spectrometry, EPA 821-R-96-007. Office of Water, U.S.
Environmental Protection Agency, Washington, DC.
USEPA. 1996f. Method 1632: Inorganic Arsenic in Water by Hydride Generation Quartz Furnace Atomic
Absorption. EPA 821-R-96-013 Office of Water, U.S. Environmental Protection Agency, Washington, DC.
USEPA. 1996g Method 1636: Determination of Hexavalent Chromium by Ion Chromatography EPA821-R-
96-003. Office of Water, U.S. Environmental Protection Agency, Washington, DC.
USEPA. 1996h. Screening of Polychlorinated Biphenyls by Immunoassay, SW846 Method 4020. Office of
Solid Waste, U.S. Environmental Protection Agency, Washington, DC.
USEPA. 1995. Environmental Monitoring and Assessment Program Laboratory Methods Manual, Estuaries,
Volume 1-Biological and Chemical Analyses, EPA/620/R-95/008. Environmental Monitoring and Assessment
Program , U.S. Environmental Protection Agency, Washington DC.
USEPA. 1994a. Field Studies for Ecological Risk Assessment. EPA 540-F-94-014. ECO Update (September
1994). Office of Solid Waste and Emergency Response, U.S. Environmental Protection Agency. Washington
D.C.
USEPA. 1994b. Compendium of Environmental Response Team Standard Operating Procedures. Office of
Solid Waste and Emergency Response, U.S. Environmental Protection Agency, Edison, NJ.
USEPA. 1994c. Method 1613: Tetra-through Octa-Chlonnated Dioxms and Furans by Isotope Dilution
HRGC/HRMS, EPA 821-B-94-005. Office of Water, U.S Environmental Protection Agency, Washington, DC.
USEPA. 1994d Methods for Assessing the Toxicity of Sediment-associated Contaminants with Estuarine and
Marine Amphipods. EPA/600/R-94/025. Office of Research and Development, U.S. Environmental Protection
Agency, Washington, DC.
USEPA. 1993a. Biological and Chemical Assessment of Contaminated Great Lakes Sediment, EPA 905-R93-
006. Great Lakes National Program Office, U.S. Environmental Protection Agency, Chicago, IL.
USEPA. 1993b Assessment and Remediation of Contaminated Sediments (ARCS) Program: Biological and
Chemical Assessment of Contaminated Great Lakes Sediment, EPA 905-R93-006. Great Lakes National
Program Office, U.S. Environmental Protection Agency, Chicago, IL.
USEPA. 1993c. Fish Field and Laboratory Methods for Evaluating the Biological Integnty of Surface Waters,
EPA/600/R-92-111. Office of Research and Development, U.S. Environmental Protection Agency,
Washington, DC.
USEPA. 1992a. Sediment Classification Methods Compendium. EPA/823-R-92-006. Office of Water, U.S.
Environmental Protecton Agency, Washington DC.
USEPA 1992b. Framework for Ecological Risk Assessment. EPA/630/R-92/001. Risk Assessment Forum,
U.S. Environmental Protection Agency, Washington D.C.
USEPA. 1992c. Monitoring Guidance for the National Estuary Program. EPA 842-B-92-004. Office of Water.
Office of Wetlands. Oceans and Watersheds. Washington. D.C.
USEPA. 1991. Draft Analytical Method for Determination of Acid Volatile Sulfide in Sediment, EPA-821-R-91-
100. Office of Water, U.S. Environmental Protection Agency, Washington, DC.
USEPA 1990a Environmental Monitoring and Assessment Program: Near Coastal Component, 1990
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for Assessing and Monitoring the Remediation of Contaminated Sediment Sites February 17,2003
Demonstration Project, Field Operations Manual. DRAFT. Contract #. 68-C8-0066. Office of Research and
Development. Narragansett, Rhode Island.
USEPA. 1990b. Macroinvertebrate Field and Laboratory Methods for Evaluating the Biological Integrity of
Surface Waters. EPA/600/4-90/030. Office of Research and Development, U.S. Environmental Protection
Agency, Washington, D.C.
USEPA. 1989a. Method 1624. Revision B: Volatile Organic Compounds by Isotope Dilution GC/MS,
EPA440-1-89-100. Office of Water, U.S. Environmental Protection Agency, Washington, DC.
USEPA. 1989b. Method 1625, Revision B: Semi-volatile Organic Compounds by Isotope Dilution GC/MS,
EPA440-1-89-100. Office of Water. U.S. Environmental Protection Agency, Washington, DC.
USEPA and the Naval Construction Battalion Center. 1992. Standard Operating Procedures and Field
Methods Used for Conducting Ecological Risk Assessment Case Studies. Technical Document 2296, Naval
Command, Control and Ocean Surveillance Center, RDT&E Division, San Diego, CA.
USEPA and USAGE. 1992. Guidance for Performing Tests on Dredged Material Proposed for Ocean
Disposal. (Draft). U.S. Army Corps of Engineers, New York District and U.S. Environmental Protection
Agency, Region II, New York, New York.
USEPA and USAGE. 1991 Evaluation of Dredged Material Proposed for Ocean Disposal. Testing Manual.
EPA 503-8-91-001. Office of Water. U.S. Environmental Protection Agency. Washington D.C.
USGS. 2001. The Krupaseep. Next Generation Seepage Meter.
http //sofia USQS oov/sfrsf/entdisplavs/krupaseep/. Updated July 23. 2001.
USGS. 1998. Tree Swallow Sample Collection and Processing Procedures, Technical Operating Procedure
WE-410.0. Upper Mississippi Science Center, U.S. Geological Survey. LaCrosse, Wl.
Weber, C.I. 1991. Methods for Measuring Acute Toxicity of Effluents in Receiving Waters for Freshwater and
Marine Organisms. 4*1 edition. EPA/600/4-901027. Environmental Monitonng Systems Laboratory, Office of
Research and Development, U.S Environmental Protection Agency, Cincinnati, OH.
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acid digestion
Fact Sheet # 2.2.2 -1
acid volatile sulfide (AVS)
Fact Sheet #2.2.2 -4
acoustic sampling
Fact Sheet #2.1.1 -18
Fact Sheet #2.2.1 -13
algae
Fact Sheet #2.1.3 -3
Fact Sheet #2.1.3 16
Fact Sheet #2.3.1 -6
Fact Sheet #2.3.1 -7
Fact Sheet #2.3.1 -8
Fact Sheet # 2.3.1 -10
alkalinity
Fact Sheet #2.1.2-30
aluminum
Fact Sheet # 2.2.2 - 2
Fact Sheet # 2.2.2 - 3
Fact Sheet # 2.3.2 - 5
antimony
Fact Sheet #2.1.1 -11
Fact Sheet #2.1.2 -4
Fact Sheet #2.1.2-6
Fact Sheet # 2.2.2 - 3
Fact Sheet # 2.3.2 - 5
arsenic determination
Fact Sheet #2.1.1 -11
Fact Sheet #2.1.2 -8
Index
Total Mercury in Sludge, Settlement, Soil, and Tissue by Acid Digestion
and BrCI Oxidatbn, Appendix to Method 1631
Determination of Acid Volatile Sulfide and Selected Simultaneously
Ex tractable Metals in Sediment
Quality Assurance Plan for Discharge Measurements Using Broadband
Acoustic Doppler Current Profilers
Method No. DRP-2-03: Acoustic Sub-bottom Profiling Systems
Method No. ERT SOP 2027: Chronic Freshwater Algae Test
Method No. NHEERL-AED SOP 1.03.009: Microtox® tests, NHEERL-AED
1.03009
Field-based Penphyton Survey in Wadeable Streams
Laboratory-based Penphyton Survey: Single Habitat Sampling in Wadeable
Streams
Laboratory-based Rapid Periphyton Survey: Multi-habitat Sampling in
Wadeable Streams
Algae and Macroinvertebrate Sampling with Frames
Method No. LMMB 091: Standard Operating Procedure for GLNPO Total
Alkalinity Titration
Trace Element Quantification Techniques
Method Title: Analysis of Marine Sediment and Bivalve
Tissue by X-Ray Fluorescence, Atomic Absorption and Inductively Coupled
Plasma Mass Spectrometry
Analysis of Marine Sediment and Bivalve Tissue by X-Ray Fluorescence,
Atomic Absorption and Inductively Coupled Plasma Mass Spectrometry
Method No. EPA Method 1669- Sampling Ambient Water for Trace Metals
at EPA Water Quality Criteria Levels
EPA Method No. 1639- Determination of Trace Elements in Ambient
Waters by Stabilized Temperature Graphite Furnace Atomic Absorptbn
EPA Method No. 1638: Determination of Trace Elements in Ambient
Waters by Inductively Coupled Plasma — Mass Spectrometry
Method Title: Analysis of Marine Sediment and Bivalve
Tissue by X-Ray Fluorescence, Atomic Absorption and Inductively Coupled
Plasma Mass Spectrometry
Analysis of Marine Sediment and Bivalve Tissue by X-Ray Fluorescence,
Atomic Absorption and Inductively Coupled Plasma Mass Spectrometry
Method No EPA Method 1669: Sampling Ambient Water for Trace Metals
at EPA Water Quality Criteria Levels
EPA Method No. 1632: Inorganic Arsenic in Water by Hydride Generation
Quartz Furnace Atomic Absorption
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Fact Sheet # 2.1.2 - 9 EPA Method No. 1632, Revision A: Chemical Speciation of Arsenic in
Water and Tissue by Hydride Generation Quartz Furnace Atomic
Absorption Spectrometry
Trace Element Quantification Techniques
Method Title: Analysis of Marine Sediment and Bivalve
Tissue by X-Ray Fluorescence, Atomic Absorption and Inductively Coupled
Plasma Mass Spectrometry
Method No. NS&T, Method Title: Trace Element Quantification
Techniques
Chemical Speciation of Arsenic in Water and Tissue by Hydride Generation
Quartz Furnace Atomic Absorption Spectrometry, EPA Method 1632,
Revision A
Fact Sheet # 2.2.2 - 2
Fact Sheet #2.2.2 -3
Fact Sheet # 2.3.2-4
Fact Sheet # 2.3.2 - 6
assimilation efficiency
Fact Sheet #2.1.3 -15
Method No. NHEERL-AED SOP 1.03 013: Growth and Scope for Growth
Measurements with Mytilus edulis
Atterberg limits
Fact Sheet # 2.2.2 - 23 Standard Test Method for Liquid Limit, Plastic Limit, and Plasticity Index of
Soils, ASTM Method D4318
avian samples
Fact Sheet # 2.3.1 - 28 Swallows: Sampling Procedures
Fact Sheet # 2.3.1 - 29 Sample Processing of Swallows
benthic community characterization
Fact Sheet # 2.3.1 -11 Benthic Organism Collection from a Marine Environment, NHEERL-AED
SOP 1.02.001
Fact Sheet # 2.3.1 -12 Benthic Macroinvertebrate Protocols in a Wadeable Stream: Single Habitat
Approach, 1-Meter Kick Net
Fact Sheet # 2.3.1 -13 Benthic Macroinvertebrate Protocols in a Wadeable Stream: Multi-habitat
Approach: D-Frame Dip Net
Fact Sheet # 2.3.1 -14 Photographic Habitat Documentation of the Benthic Community
Fact Sheet # 2.3.1 -15 Sediment Profile Camera
Fact Sheet # 2.3.1 -17 Stream-net Samplers: Surber, Portable Invertebrate Box Sampler, Hess
Sampler, Hess Stream Bottom Sampler, and Stream-bed Fauna Sampler
Fact Sheet #2.3.3 - 3 Laboratory Analysis of Benthic Macroinvertebrates in Wadeable Streams
beryllium -7
Fact Sheet #2.2.2 -26
bioaccumulation
Fact Sheet #2.1.1 -20
Fact Sheet #2.2.3-17
Fact Sheet # 2.3.1 - 28
Method Title: Beryllium-7 as a Tracer of Short Term Sediment Deposition
Caged Bivalve Deployment
Bioaccumulation Test for Marine, Estuarine, and Freshwater Sediments,
EPA Method 100.3
Swallows: Sampling Procedures
Fact Sheet # 2.3.1 - 29 Sample Processing of Swallows
Method No. ERT SOP 2027: Chronic Freshwater Algae Test
bioassay- algae
Fact Sheet #2.1.3-3
bioassay - crustacean
Fact Sheet #2.1.3-1
Method No. ERT SOP 2024. Acute Freshwater Crustacean Bioassay: 48
Hours
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Fact Sheet #2.1.3-4
Fact Sheet #2.1.3 -5
Fact Sheet #2.1.3 -8
Fact Sheet #2.1.3 -10
Fact Sheet #2.1.3 -13
Fact Sheet #2.1.3 -14
bioassay - echinoderm
Fact Sheet #2.1.3 -11
Method No. ERT SOP 2025: Chronic Freshwater Crustacean Bioassay
(7day)
Method No. ERT SOP 2028: Chronic Freshwater Crustaceans Bioassay
(10 days)
Method No. NHEERL-AED SOP 1.03.003: Acute Marine Crustacean
Bioassay
Method No. NHEERL-AED SOP 1.03.005: Chronic Estuarine Survival,
Growth, and Fecundity Test
Toxicity Evaluations of Photomduction of Polycychc Aromatic Hydrocarbons
(PAH): In Situ Analysis
Toxicity Evaluations of Photomduction of Polycyclic Aromatic
Hydrocarbons: Laboratory Analysis of Storm water
Method No. NHEERL-AED SOP 1.03 006: Chronic Echinoderm
Fertilization Test
bioassay - estuarine environments
Fact Sheet # 2.1.3 -10 Method No. NHEERL-AED SOP 1 03.005: Chronic Estuarine Survival,
Growth, and Fecundity Test
Method No. NHEERL-AED SOP 1.03.006: Chronic Echinoderm
Fertilization Test
Chronic Estuarine Amphipod Sediment Bioassay
Fact Sheet #2.1.3 -11
Fact Sheet #2.2.3-12
bioassay - fish
Fact Sheet #2.1.3-2
Fact Sheet #2.1.3 -6
Fact Sheet #2.1 3-9
Fact Sheet #2.1.3-12
Method No. ERT SOP 2022: Acute Freshwater fish Bioassay
Method No. ERT SOP 2026: Chronic Freshwater Fish Bioassay. ERT SOP
2026
Method No NHEERL-AED SOP 1.03.003: Acute Marine Fish Bioassay
Method No. NHEERL-AED SOP 1.03.004: Chronic Marine Fish Bioassay
bioassay - freshwater environments
Fact Sheet # 2.1.3 -1 Method No. ERT SOP 2024: Acute Freshwater Crustacean Bioassay: 48
Hours
Fact Sheet # 2.1.3 - 2 Method No. ERT SOP 2022: Acute Freshwater fish Bioassay
Method No. ERT SOP 2027- Chronic Freshwater Algae Test
Method No. ERT SOP 2025: Chronic Freshwater Crustacean Bioassay
(7day)
Method No. ERT SOP 2028: Chronic Freshwater Crustaceans Bioassay (10
days)
Method No. ERT SOP 2026: Chronic Freshwater Fish Bioassay, ERT SOP
2026
Acute Freshwater Crustacean Sediment Bioassay: Flow-through
Acute Freshwater Crustacean Sediment Bioassay. In Situ Exposures
Acute Freshwater Crustacean Sediment Bioassay. Static Laboratory
Exposures
Acute Freshwater Amphipod and Freshwater Insect Larvae Sediment
Bioassay, EPA Method 100.1
Chronic Freshwater Amphipod Sediment Bioassay. EPA Method 100.4
Life-Cycle Freshwater Midge Sediment Bioassay. EPA Method 100.5
Fact Sheet #2.1.3-3
Fact Sheet #2.1.3-4
Fact Sheet #2.1.3-5
Fact Sheet #2.1.3-6
Fact Sheet # 2.2.3 -1
Fact Sheet # 2.2.3 - 2
Fact Sheet #2.2.3-3
Fact Sheet # 2.2.3 - 4
Fact Sheet #2.2.3-5
Fact Sheet # 2.2.3 - 6
bioassay - marine environments
Fact Sheet #2.1.3 - 7 Method No. NHEERL-AED SOP 1.03.001: Chronic Marine Macroalgae,
Champia parvula, Sexual Reproduction test
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Fact Sheet #2.1.3 -8
Fact Sheet #2.1.3 -9
Fact Sheet #2.1.3-12
Fact Sheet # 2.2.3 - 7
Fact Sheet #2.2.3 -8
Fact Sheet #2.2.3-9
Fact Sheet #2.2.3-10
Fact Sheet #2.2.3-11
Fact Sheet #2.2.3-12
Fact Sheet #2.2.3-13
Method No. NHEERL-AED SOP 1.03.003: Acute Marine Crustacean
Bioassay
Method No. NHEERL-AED SOP 1.03.003: Acute Marine Fish Bioassay
Method No. NHEERL-AED SOP 1.03.004: Chronic Marine Fish Bioassay
Acute Larval Bivalve Sediment Bioassay
Acute Echinoderm Sediment Bioassay
Acute Marine Crustacean Sediment Bioassay
Acute Marine Amphipod Crustacean Sediment Bioassay, EPA Method
100.4
Acute Marine Polychaete Sediment Bioassay, ASTM Method E1611-00
Chronic Estuarine Amphipod Sediment Bioassay
Chronic Marine Polychaete Sediment Bioassay, ASTM Method E1611-00
bioassay - marine/estuarine environments
Fact Sheet #2.1.3-11 Method No. NHEERL-AED SOP 1.03.006: Chronic Echinoderm Fertilization
Test
bioassay- sediment
Fact Sheet #2.2.1-8
Fact Sheet # 2.2.3 -1
Fact Sheet # 2.2.3 - 2
Fact Sheet # 2.2.3 - 3
Fact Sheet # 2.2.3 - 4
Fact Sheet # 2.2.3 - 5
Fact Sheet # 2.2.3 - 6
Fact Sheet # 2.2.3 - 7
Fact Sheet #2.2.3-8
Fact Sheet #2.2.3-9
Fact Sheet #2.2.3-10
Fact Sheet #2.2.3-11
Fact Sheet #2.2.3-12
Fact Sheet #2.2.3-13
bfomass
Fact Sheet #2.3.1 -6
Fact Sheet #2.3.1 -7
Fact Sheet #2.3.1 -8
Fact Sheet # 2.3.3 -1
Fact Sheet # 2.3.3 - 2
brail sampling
Fact Sheet #2.3.1 -18
butyl ins
Fact Sheet #2.2.2-13
Sediment Processing for Chemistry and Toxicity Testing
Acute Freshwater Crustacean Sediment Bioassay: Flow-through
Acute Freshwater Crustacean Sediment Bioassay: In Situ Exposures
Acute Freshwater Crustacean Sediment Bioassay: Static Laboratory
Exposures
Acute Freshwater Amphipod and Freshwater Insect Larvae Sediment
Bioassay. EPA Method 100.1
Chronic Freshwater Amphipod Sediment Bioassay, EPA Method 100.4
Life-Cycle Freshwater Midge Sediment Bioassay, EPA Method 100.5
Acute Larval Bivalve Sediment Bioassay
Acute Echinoderm Sediment Bioassay
Acute Marine Crustacean Sediment Bioassay
Acute Marine Amphipod Crustacean Sediment Bioassay, EPA Method
100.4
Acute Marine Polychaete Sediment Bioassay, ASTM Method E1611-00
Chronic Estuarine Amphipod Sediment Bioassay
Chronic Marine Polychaete Sediment Bioassay, ASTM Method E1611-00
Field-based Penphyton Survey in Wadeable Streams
Laboratory-based Periphyton Survey: Single Habitat Sampling in Wadeable
Streams
Laboratory-based Rapid Periphyton Survey: Multi-habitat Sampling in
Wadeable Streams
Laboratory Identification, Enumeration and Biomass Measurements of
Periphyton in Wadeable Streams
Laboratory Periphyton Biomass Determination
Mussel Collection Using Brails
Butyltin in Sediments
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cadmium
Fact Sheet #2.1.1 -11
Fact Sheet #2.1.2 -4
Fact Sheet #2.1.2 -6
Fact Sheet #2.1.2 -5
Fact Sheet #2.1.2-7
Fact Sheet #2.2.2-2
Fact Sheet # 2.2.2 - 3
Fact Sheet #2.3.2 -4
Fact Sheet #2.3.2 -5
calcium
Fact Sheet #2.1.2-34
carbon-14
Fact Sheet #2.3.1 -4
cesium-137
Fact Sheet # 2.2.2 - 25
chemical fishing techniques
Fact Sheet #2.3.1 -20
chloride
Fact Sheet #2.1.2-27
Fact Sheet #2.1.2-28
chlorophyll-a
Fact Sheet #2.3.1 -2
Fact Sheet #2.3.1 -3
Fact Sheet # 2.3.3 - 2
Method No. EPA Method 1669: Sampling Ambient Water for Trace Metals
at EPA Water Quality Criteria Levels
EPA Method No. 1639: Determination of Trace Elements in Ambient Waters
by Stabilized Temperature Graphite Furnace Atomic Absorption
EPA Method No. 1638: Determination of Trace Elements in Ambient Waters
by Inductively Coupled Plasma — Mass Spectrometry
EPA Method No. 1637: Determination of Trace Elements in Ambient Waters
by Off-line Chelation Pre-concentration and Stabilized Temperature
Graphite Furnace Atomic Absorption
EPA Method No. 1640: Determination of Trace Elements in Ambient Waters
by On-Line Chelation Pre-concentration and Inductively Coupled Plasma-
Mass Spectrometry
Trace Element Quantification Techniques
Method Title: Analysis of Marine Sediment and Bivalve
Tissue by X-Ray Fluorescence. Atomic Absorption and Inductively Coupled
Plasma Mass Spectrometry
Method No. NS&T, Method Title: Trace Element Quantification
Techniques
Analysis of Marine Sediment and Bivalve Tissue by X-Ray Fluorescence.
Atomic Absorption and Inductively Coupled Plasma Mass Spectrometry
Method No. LMMB 095: Total Hardness Titration
Primary Productivity Using 14C: Field Procedure in the Great Lakes, LMMB
016
Method Title: Sediment Age Dating Using Cesium-137
Chemical Fishing
Method No. ESS Method 140.4- Chloride - Automated Flow Injection
Analysis
Method No. ESS Method 200.5: Determination of Inorganic Anions in Water
by Ion Chromatography
Chlorophyll-a Sampling Method and Preservation: Field Procedure in the
Great Lakes, LMMB 015
Chlorophyll-a and Phaeophytin Field Filtering Protocols
Laboratory Periphyton Biomass Determination
chromium
Fact Sheet #2.1.1 -11
Fact Sheet #2.1.2-4
Fact Sheet #2.1.2-10
Fact Sheet # 2.2.2 - 2
Method No EPA Method 1669: Sampling Ambient Water for Trace Metals
at EPA Water Quality Criteria Levels
EPA Method No. 1639: Determination of Trace Elements in Ambient Waters
by Stabilized Temperature Graphite Furnace Atomic Absorption
EPA Method No. 1636, Method Title. Determination of Hexavalent
Chromium by Ion Chromatography
Trace Element Quantification Techniques
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Fact Sheet #2.2.2 -3
Fact Sheet #2.3.2 -4
Fact Sheet #2.3.2-5
clearance rate
Fact Sheet #2.1.3-15
combustion analysis
Fact Sheet # 2.2.2 -14
conductivity
Fact Sheet #2.1.2 -31
Method Title: Analysis of Marine Sediment and Bivalve
Tissue by X-Ray Fluorescence. Atomic Absorption and Inductively Coupled
Plasma Mass Spectrometry
Method No. NS&T, Method Title: Trace Element Quantification
Techniques
Analysis of Marine Sediment and Bivalve Tissue by X-Ray Fluorescence.
Atomic Absorption and Inductively Coupled Plasma Mass Spectrometry
Method No. NHEERL-AED SOP 1.03.013: Growth and Scope for Growth
Measurements with MytBus edulis
Procedures for Sediment Total Organic Carbon (TOC) Determination
Method No. LMMB 094: Standard Operating Procedure for GLNPO Specific
Conductance: Conductivity Bridge
conductivity, temperature, density (CTD) measurements
Fact Sheet # 2.1.1-1 In Situ sampling with the Hydrolab Datasonde3® Unit
consolidation (see sediment consolidation)
copper
Fact Sheet #2.1.1 -11
Fact Sheet #2.1.2 -6
Fact Sheet #2.1.2-7
Fact Sheet #2.2.2-2
Fact Sheet #2.3.2-4
Fact Sheet #2.3.2-5
dioxin analysis
Fact Sheet #2.1.2-17
Fact Sheet #2.2.2-3
Fact Sheet #2.2.2-10
Fact Sheet #2.3.2-11
Method No. EPA Method 1669. Sampling Ambient Water for Trace Metals
at EPA Water Quality Criteria Levels
EPA Method No. 1638: Determination of Trace Elements in Ambient Waters
by Inductively Coupled Plasma — Mass Spectrometry
EPA Method No. 1640: Determination of Trace Elements in Ambient Waters
by On-Line Chelation Pre-concentratbn and Inductively Coupled Plasma-
Mass Spectrometry
Trace Element Quantification Techniques
Method No. NS&T, Method Title: Trace Element Quantification
Techniques
Analysis of Marine Sediment and Bivalve Tissue by X-Ray Fluorescence.
Atomic Absorption and Inductively Coupled Plasma Mass Spectrometry
EPA Method No. 1613: Tetra-through Octa-Chlorinated Dioxins and Furans
by Isotope Dilution HRGC/HRMS
Method Title: Analysis of Marine Sediment and Bivalve
Tissue by X-Ray Fluorescence, Atomic Absorption and Inductively Coupled
Plasma Mass Spectrometry
Tetra- through Octa-Chlorinated Dioxins and Furans by Isotope Dilution
HRGC/HRMS. EPA Method 1613
Tetra- through Octa-Chlorinated Dioxins and Furans by Isotope Dilution
HRGC/HRMS, EPA Method 1613
dissolved organic carbon (DOC)
Fact Sheet #2.1.2-24 Standard Method No 5310: Total Organic Carbon
Fact Sheet # 2.1.2 - 25 Method No. LMMB 096: Standard Operating Procedure for the Analysis of
Dissotved-Phase Organic Carbon in Great Lakes Waters
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dissolved oxygen
Fact Sheet #2.1.1 -1
Fact Sheet #2.1.1 -2
Fact Sheet #2.1.1 -9
dry weight determination
Fact Sheet #2.3.2 -14
'Fact Sheet #2.2.2-17
electrofishing
Fact Sheet #2.3.1 -19
entrapment devices
Fact Sheet #2.3.1 -23
Method Title: In Situ sampling with the Hydrolab Datasonde3®Unit
In Situ Dissolved Oxygen sampling with a YSI Model 58 Dissolved Oxygen
Meter and probe DO meter
Sample and Preservation of Water Specific Parameters
Determination of Percent Dry Weight for Tissues
Procedures for Water Content Determination
Electrofishing
Entrapment Devices
field sampling - in situ measurements
Fact Sheet #2.1.1-1
Fact Sheet #2.1.1-2
Fact Sheet #2.1.1-3
Fact Sheet #2.1.1-4
Fact Sheet #2.2.2-24
Fact Sheet # 2.3.1 - 6
In Situ sampling with the Hydrolab Datasonde3® Unit
In Situ Dissolved Oxygen sampling with a YSI Model 58 Dissolved Oxygen
Meter and probe DO meter
In Situ sampling of Irradiance
In Situ Transparency Sampling
Field Portable X-Ray Fluorescence Spectrometry for the Determination of
Elemental Concentrations in Soil and Sediment
Field-based Periphyton Survey in Wadeable Streams
field sampling - discrete sample collection
Fact Sheet #2.1.1-5
Fact Sheet #2.1.1-6
Fact Sheet #2.1.1 -7
Fact Sheet #2.1.1 -8
Fact Sheet #2.1.1 -9
Fact Sheet #2.1.1 -10
Fact Sheet #2.1.1 -17
Fact Sheet #2.1.1 -19
Fact Sheet #2.3.1 -1
Fact Sheet # 2.3.1 - 2
Fact Sheet #2.3.1 -3
fish collection
Fact Sheet # 2 3.1 -19
Fact Sheet #2.3.1 -20
Fact Sheet # 2.3.1 -21
Fact Sheet # 2.3.1 - 22
Fact Sheet # 2.3.1 - 23
Fact Sheet #2.3.1 -24
Fact Sheet # 2.3.1 - 25
fish community assessment
Fact Sheet #2.3.3-10
Sample Collection Procedures for Marine water
Method No LMMB 013- Field Sampling Using a Rosette Sampler
Method No. ERT SOP #2013: Water Sample Collection with the Kemmerer
Bottle and the Bacon Bomb Sampler
Method No. ERT SOP # 2013: Dip Sampler
Sample and Preservation of Water Specific Parameters
Method No. LMMB 014: Sampling of Particulate-Phase and Dissotved-
Phase Organic Carbon in Great Lakes Waters
LMMB 017: USGS Field Operation Plan: Tributary Monitonng
Seepage Meters
Phytoplankton Sample Collection and Preservation in the Great Lakes.
LMMB 023t
Chlorophyll-a Sampling Method and Preservation: Field Procedure in the
Great Lakes. LMMB 015
Chlorophyll-a and Phaeophytin Field Filtering Protocols
Electrofishing
Chemical Fishing
Fish Collection Using Seine Nets
Entanglement Nets
Entrapment Devices
Pop Nets
Trawls
Fish Bioassessment I and I
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fish age dating
Fact Sheet #2.3.1 -26
fish processing
Fact Sheet #2.3.1-26
Fact Sheet #2.3.1 -27
Fact Sheet #2.3.3-5
fish tissue analysis
Fact Sheet # 2.3.2 -1
Fact Sheet # 2.3.2 - 7
furans (see dioxins)
gas chromatography
Fact Sheet #2.1.2-13
Fact Sheet #2.1.2-14
Fact Sheet #2.1.2-15
Fact Sheet #2.1.2 -16
Fact Sheet #2.1.2-17
Fact Sheet #2.1.2-18
Fact Sheet #2.1.2-19
Fact Sheet #2.2.2-5
Fact Sheet #2.2.2-7
Fact Sheet #2.2.2-8
Fact Sheet #2.2.2-10
Fact Sheet #2.2.2-11
Fact Sheet #2.2.2-12
Fact Sheet #2.2.2-13
Fish Processing Method in the Great Lakes, LMMB 025
Fish Processing Method in the Great Lakes, LMMB 025
Fish Processing
SOP-2: Lab Analysis of Lake Trout Stomachs and Data Entry; Appendix B.
Standard Operating Procedure for Lab Analysis of Coho Salmon Stomachs
and Data Entry, LMMB 026 - Appendix 2 & LMMB 027 - Appendix B
Sample Preparation for Metal Contaminants in Tissue
Extraction and Lipid Separatbn of Fish Samples for Contaminant Analysis
and Lipid Determination, LMMB 043
EPA Method No. 1625: Semi-volatile Organic Compounds by Isotope
Dilution GC/MS
Quantitative Determination of Polvnuclear Aromatic Hydrocarbons by Gas
Chromatography/Mass Spec tram etry (GC/MS) - Selected Ion Monitoring
(SIM) Mode
Method No. LMMB 041: Analysis of Polychlorinated Biphenyls and
Chlorinated Pesticides by Gas Chromatography with Electron Capture
Detection
Method No. LMMB: PCBs and Pesticides in Surface Water by XAD-2 Resin
Extraction
EPA Method No. 1613: Tetra- through Octa-Chlorinated Dioxins and Furans
by Isotope Dilution HRGC/HRMS
EPA Method No. 1668: Toxic Polychlonnated Biphenyls by Isotope Dilution
High Resolution Gas Chromatography/High Resolution Mass Spectrometry
EPA Method No. 1668, Revision A: Chlorinated Biphenyl Congeners in
Water, Soil. Sediment, and Tissue by HRGC/HRMS
Photovac GC Analysis for Soil, Water, and Air/Soil Gas, OSWER SOP#
2109
Quantitative Determination of Polynuclear Aromatic Hydrocarbons by Gas
Chromatography/Mass Spectrometry (GC/MS)--Selected Ion Monitoring
(SIM) Mode
Analysis of Polychlorinated Biphenyls and Chlorinated Pesticides by Gas
Chromatography with Electron Capture Detectbn, LMMB 041
Tetra- through Octa-Chlorinated Dioxins and Furans by Isotope Dilution
HRGC/HRMS, EPA Method 1613
Toxic Polychlorinated Biphenyls by Isotope Dilution High Resolution Gas
Chromatography/High Resolution Mass Spectrometry, EPA Method 1668
Chlorinated Biphenyl Congeners in Water, Soil, Sediment, and Tissue by
HRGC/HRMS, EPA Method 1668 Revision A
Butyltin in Sediments
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Fact Sheet #2.3.2-9
Fact Sheet #2.3.2 -10
Fact Sheet #2.3.2 -11
Fact Sheet #2.3.2-12
Fact Sheet #2.3.2 -13
gonadal analysis
Fact Sheet # 2.3.3 - 6
grain size analysis
Fact Sheet #2 2.2-16
habitat assessment
Fact Sheet #2.1.1 -15
Fact Sheet #2.1.1 -16
Quantitatve Determination of Polynuclear Aromatic Hydrocarbons by Gas
Chromatography/Mass Spectrometry (GC/MS)-Selected Ion Monitoring
(SIM) Mode
Analysis of Pol/chlorinated Biphenyls and Chlorinated Pesticides by Gas
Chromatography with Electron Capture Detection, LMMB 041
Tetra- through Octa-Chlorinated Dioxins and Furans by Isotope Dilution
HRGC/HRMS, EPA Method 1613
Toxic Polychlonnated Biphenyls by Isotope Dilution High Resolution Gas
Chromatography/High Resolution Mass Spectrometry, EPA Method 1-668
Chlorinated Biphenyl Congeners in Water. Soil, Sediment, and Tissue by
HRGC/HRMS, EPA Method 1668 Revision A
Gonadal Analysis
Sediment Grain Size Analysis, NHEERL-AED SOP 1.01.005
Physical Characterization of a stream
Visual based habitat assessment
hardness
Fact Sheet #2.1.2-34
Method No. LMMB 095: Total Hardness Titration
high resolution gas Chromatography
Fact Sheet # 2.3.2 -11 Tetra- through Octa-Chlorinated Dioxins and Furans by Isotope Dilution
HRGC/HRMS, EPA Method 1613
Fact Sheet # 2.3.2 -12 Toxic Pol/chlorinated Biphenyls by Isotope Dilution High Resolution Gas
Chromatography/High Resolution Mass Spectrometry, EPA Method 1668
Fact Sheet # 2.3.2 -13 Chlorinated Biphenyl Congeners in Water, Soil, Sediment, and Tissue by
HRGC/HRMS, EPA Method 1668 Revision A
histopathology
Fact Sheet # 2.3.3 - 7
Fact Sheet # 2.3.3 - 8
hydrographic profiles
Fact Sheet #2.1.1-1
Fact Sheet #2.1.1-2
Fact Sheet #2.1.1-3
Fact Sheet #2.1.1 -4
immunoassay screening
Fact Sheet #2.22-9
Index of Biotic Integrity (IBI)
Fact Sheet # 2.3.3 - 9
Histopathological Evaluations of Target and Non Target Fish Species
Histopathology Analysis
In Situ sampling with the Hydrolab DatasondeS® Unit
In Situ Dissolved Oxygen sampling with a YSI Model 58 Dissolved Oxygen
Meter and probe DO meter
In Situ sampling of Irradiance
In Situ Transparency Sampling
Screening for Polychlonnated Biphenyls by Immunoassay, SW846 Method
4020
Index of Biotic Integrity (IBI)
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Inductively Coupled Plasma Mass Spectrometry (ICPMS)
iron
Fact Sheet #2.2.2-3
Fact Sheet #2.3.2-5
Fact Sheet # 2.2.2 - 2
Fact Sheet # 2.2.2 - 3
Fact Sheet # 2.3.2 - 4
Fact Sheet #2.3.2-5
Analysis of Marine Sediment and Bivalve Tissue by X-Ray Fluorescence,
Atomic Absorption and Inductively Coupled Plasma Mass Spectrometry
Analysis of Marine Sediment and Bivalve Tissue by X-Ray Fluorescence,
Atomic Absorption and Inductively Coupled Plasma Mass Spectrometry
Trace Element Quantification Techniques
Method Title: Analysis of Marine Sediment and Bivalve
Tissue by X-Ray Fluorescence, Atomic Absorption and Inductively Coupled
Plasma Mass Spectrometry
Method No. NS&T, Method Title: Trace Element Quantification
Techniques
Analysis of Marine Sediment and Bivalve Tissue by X-Ray Fluorescence,
Atomic Absorptbn and Inductively Coupled Plasma Mass Spectrometry
lead
Fact Sheet #2.1.1 -11
Fact Sheet #2.1.2 -6
Fact Sheet #2.1.2-5
Fact Sheet #2.1.2-7
Fact Sheet #2.2.2-2
Fact Sheet #2.2.2-3
Fact Sheet #2.3.2-4
Fact Sheet #2.3.2-5
Method No. EPA Method 1669: Sampling Ambient Water for Trace Metals
at EPA Water Quality Criteria Levels
EPA Method No. 1638: Determination of Trace Elements in Ambient Waters
by Inductively Coupled Plasma — Mass Spectrometry
EPA Method No. 1637: Determination of Trace Elements in Ambient Waters
by Off-Line Chelation Pre-concentration and Stabilized Temperature
Graphite Furnace Atomic Absorption
EPA Method No. 1640: Determination of Trace Elements in Ambient Waters
by On-Line Chelation Pre-concentration and Inductively Coupled Plasma-
Mass Spectrometry
Trace Element Quantification Techniques
Method Title: Analysis of Marine Sediment and Bivalve
Tissue by X-Ray Fluorescence, Atomic Absorption and Inductively Coupled
Plasma Mass Spectrometry
Method No. NS&T. Method Title: Trace Element Quantification
Techniques
Analysis of Marine Sediment and Bivalve Tissue by X-Ray Fluorescence,
Atomic Absorption and Inductively Coupled Plasma Mass Spectrometry
lead-210
Fact Sheet #2.2.2-15
Method No. LMMB 084, Method Title: Determination of the Activity of Lead-
210 in Sediments and Soils
light measurements
Fact Sheet #2.1.1-3
macrolnvertebrate - analysis
Fact Sheet #2.3.3-3
Fact Sheet #2.3.3-4
In Situ sampling of Irradiance
Laboratory Analysis of Benthic Macro!nvertebrates in Wadeable Streams
Laboratory Analysis of Water Column Organisms
macroinvertebrate - sample collection
Fact Sheet #2.2.1 -1
Fact Sheet #2.2.1 -2
Fact Sheet #2.2.1 -3
Fact Sheet #2.2.1 -4
Fact Sheet #2.3.1 -9
Fact Sheet #2.3.1 -10
Fact Sheet #2.3.1 -11
Grab Sampling
Core Samplers
Hand Collection
Hand collection at depth with SCUBA
Artificial Substrate Samplers of Macromvertebrates in Wadeable Streams
Algae and Macroinvertebrate Sampling with Frames
Benthic Organism Collection from a Marine Environment, NHEERL-AED
SOP 1.02.001
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Fact Sheet # 2.3.1 -12
Fact Sheet # 2.3.1 -13
Fact Sheet # 2.3.1 -16
Fact Sheet # 2.3.1 -17
magnesium
Fact Sheet #2.1.2 -34
Fact Sheet # 2.2.2 - 2
Fact Sheet # 2.2.2 - 3
Fact Sheet # 2.3.2 - 5
mercury
Fact Sheet #2.1.1 -11
Fact Sheet #2.1.2-1
Fact Sheet #2.1.2 -2
Fact Sheet #2.1.2-3
Fact Sheet #2.2.2-1
Fact Sheet # 2.2.2 - 2
Fact Sheet #2.2.2-3
Fact Sheet #2.3.2-2
Fact Sheet # 2.3.2 - 3
Fact Sheet # 2.3.2 - 4
Fact Sheet # 2.3.2 - 5
metals analysis methods
Fact Sheet #2.1.1 -9
Fact Sheet #2.1.1 -11
Fact Sheet #2 1.2-1
Fact Sheet #2.1.2-6
Fact Sheet #2.1.2-7
Fact Sheet #2.1.2-8
Benthic Macroinvertebrate Protocols in a Wadeable Stream: Single Habitat
Approach, 1-Meter Kick Net
Benthic Macroinvertebrate Protocols in a Wadeable Stream: Multi-habitat
Approach: D-Frame Dip Net
Macroinvertebrate Drift Nets in a Wadeable Stream
Stream-net Samplers: Surber, Portable Invertebrate Box Sampler, Hess
Sampler. Hess Stream Bottom Sampler, and Stream-bed Fauna Sampler
Method No. LMMB 095: Total Hardness Titratbn
Trace Element Quantification Techniques
Method Title: Analysis of Marine Sediment and Bivalve
Tissue by X-Ray Fluorescence, Atomic Absorptbn and Inductively Coupled
Plasma Mass Spectrometry
Analysis of Marine Sediment and Bivalve Tissue by X-Ray Fluorescence,
Atomic Absorption and Inductively Coupled Plasma Mass Spectrometry
Method No. EPA Method 1669. Sampling Am blent Water for Trace Metals
at EPA Water Quality Criteria Levels
EPA Method No. 245.7: Mercury in Water by Cold Vapor Atomic
Fluorescence Spectrometry
EPA Method No. 1631, Revision B: Mercury in Water by Oxidation, Purge
and Trap, and Cold Vapor Atomic Fluorescence Spectrometry
EPA Method No. 1630: Methyl mercury in water by distillation. Aqueous
Ethylation, Purge and Trap, and CVAFS
Total Mercury in Sludge, Settlement, Soil, and Tissue by Acid Digestion and
BrCI Oxidation. Appendix to Method 1631
Trace Element Quantification Techniques
Method Title: Analysis of Marine Sediment and Bivalve
Tissue by X-Ray Fluorescence, Atomic Absorption and Inductively Coupled
Plasma Mass Spectrometry
Total Mercury in Tissue. Sludge. Sediment, and Soil by Acid Digestion and
BrCI Oxidation, Appendix to Method 1631
Versatile Combustion-Amalgamation Technique for the Photometric
Determination of Mercury in Fish and Environmental Samples, LMMB 052
Method No. NS&T, Method Title: Trace Element Quantification
Techniques
Analysis of Marine Sediment and Bivalve Tissue by X-Ray Fluorescence,
Atomic Absorption and Inductively Coupled Plasma Mass Spectrometry
Sample and Preservation of Water Specific Parameters
Method No. EPA Method 1669: Sampling Ambient Water for Trace Metals
at EPA Water Quality Criteria Levels
EPA Method No. 245 7: Mercury in Water by Cold Vapor Atomic
Fluorescence Spectrometry
EPA Method No. 1638: Determination of Trace Elements in Ambient Waters
by Inductively Coupled Plasma — Mass Spectrometry
EPA Method No. 1640. Determination of Trace Elements in Ambient Waters
by On-Line Chelation Pre-concentratton and Inductively Coupled Plasma-
Mass Spectrometry
EPA Method No. 1632. Inorganic Arsenic in Water by Hydride Generation
Quartz Furnace Atomic Absorption
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Fact Sheet #2.1.2 -9
Fact Sheet #2.1.2-10
Fact Sheet #2.2.2- 2
Fact Sheet #2.3.2-1
Fact Sheet #2.3.2 -4
Fact Sheet #2.3.2-5
Fact Sheet #2.3.2-6
EPA Method No. 1632, Revision A: Chemical Speciation of Arsenic in Water
and Tissue by Hydride Generation Quartz Furnace Atomic Absorption
Spectrometry
EPA Method No. 1636: Determination of Hexavalent Chromium by Ion
Chromatography
Trace Element Quantification Techniques
Sample Preparation for Metal Contaminants in Tissue
Trace Element Quantification Techniques
Analysis of Marine Sediment and Bivalve Tissue by X-Ray Fluorescence,
Atomic Absorption and Inductively Coupled Plasma Mass Spectrometry
Chemical Speciation of Arsenic in Water and Tissue by Hydride Generation
Quartz Furnace Atomic Absorption Spectrometry, EPA Method 1632,
Revisbn A
metals toxicity
Fact Sheet #2.1.2-4
microbiological testing
Fact Sheet #2.1.2-5
microwave extraction
Fact Sheet # 2.3.2 -16
EPA Method No. 1639: Determination of Trace Elements in Ambient Waters
by Stabilized Temperature Graphite Furnace Atomic Absorption
EPA Method No. 1637. Determination of Trace Elements in Ambient Waters
by Off-Line Chelation Pre-concentration and Stabilized Temperature
Graphite Furnace Atomic Absorption
Microwave Extraction of Marine Tissue for Semivolatile Organic Analytes,
AED LOP 2.03.030,
Revision 0
mussels
Fact Sheet #2.1.1 -20
Fact Sheet #2.3.1 -18
mutagenlcity testing
Fact Sheet #2.2.3-14
Fact Sheet # 2.2.3 -15
Fact Sheet #2.2.3-16
net tow surveys
Fact Sheet #2.3.1 -5
Fact Sheet #2.3.1 -13
Fact Sheet #2.3.1 -16
Fact Sheet #2.3.1 -21
Fact Sheet #2.3.1 -22
Fact Sheet #2.3.1 -24
Caged Bivalve,Deployment
Mussel Collection Using Brails
Ames Mutagenicity Assay
Mutatox Genotoxicity Assay
V79 Sister Chromatid Exchange Assay, NHEERL-AED SOP 1.03.012
Zooplankton Sample Collection and Preservation in the Great Lakes, LMMB
024
Be nth ic Macroinvertebrate Protocols in a Wadeable Stream1 Multi-habitat
Approach: D-Frame Dip Net
Macroinvertebrate Drift Nets in a Wadeable Stream
Fish Collection Using Seine Nets
Entanglement Nets
Pop Nets
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nickel
Fact Sheet #2.1.1 -11
Fact Sheet #2.1.2-4
Fact Sheet #2.1.2-6
Fact Sheet #2.1.2-7
Fact Sheet #2.2.2 -2
Fact Sheet #2.2.2-3
Fact Sheet #2.3.2-4
Fact Sheet # 2.3.2 - 5
nitrogen determination
Fact Sheet #2.1.2-20
Fact Sheet #2.1.2-21
Fact Sheet #2.1.2-28
organic analysis methods
Fact Sheet #2.1.1 -9
Fact Sheet #2.1.1 -10
Fact Sheet #2.1.2-11
Fact Sheet #2.1.2-13
Fact Sheet #2.1.2-14
Fact Sheet #2.1.2-15
Fact Sheet #2.1.2-16
Fact Sheet #2.1.2-18
Fact Sheet #2.1.2-19
Fact Sheet # 2.3.2 - 7
organotins
Fact Sheet #2.2.2-13
Method No. EPA Method 1669: Sampling Ambient Water for Trace Metals
at EPA Water Quality Criteria Levels
EPA Method No. 1639: Determination of Trace Elements in AmbientWaters
by Stabilized Temperature Graphite Furnace Atomic Absorption
EPA Method No. 1638: Determination of Trace Elements in Ambient Waters
by Inductively Coupled Plasma — Mass Spectrometry
EPA Method No. 1640: Determination of Trace Elements in AmbientWaters
by On-Lme Chelation Pre-concentratbn and Inductively Coupled Plasma-
Mass Spectrometry
Trace Element Quantification Techniques
Method Title: Analysis of Marine Sediment and Bivalve
Tissue by X-Ray Fluorescence, Atomic Absorption and Inductively Coupled
Plasma Mass Spectrometry
Method No. NS&T, Method Title: Trace Element Quantification
Techniques
Analysis of Marine Sediment and Bivalve Tissue by X-Ray Fluorescence,
Atomic Absorption and Inductively Coupled Plasma Mass Spectrometry
Method No ESS Method 220.3: Ammonia Nitrogen and Nitrate+Nitnte
Nitrogen, Automated Flow Injection Analysis Method
Method No. ESS Method 230.1: Total Phosphorus and Total Kjeldahl
Nitrogen, Semi-Automated Method
Method No. ESS Method 200.5: Determination of Inorganic Anions in Water
by Ion Chromatography
Sample and Preservation of Water Specific Parameters
Method No. LMMB 014: Sampling of Particulate-Phase and Dissolved-
Phase Organic Carbon in Great Lakes Waters
EPA Method No. 1624b: Volatile Organic Compounds by Isotope Dilution
GC/MS
EPA Method No. 1625: Semi-volatile Organic Compounds by Isotope
Dilution GC/MS
Quantitative Determination of Pol/nuclear Aromatic Hydrocarbons by Gas
Chromatography/Mass Spectrometry (GC/MS) - Selected Ion Monitoring
(SIM) Mode
Method No. LMMB 041: Analysis of Polychlorinated Biphenyls and
Chlorinated Pesticides by Gas Chromatography with Electron Capture
Detection
Method No. LMMB: PCBs and Pesticides in Surface Water by XAD-2 Resin
Extraction
EPA Method No. 1668: Toxic Polychlorinated Biphenyls by Isotope Dilution
High Resolution Gas Chromatography/High Resolution Mass Spectrometry
EPA Method No. 1668, Revision A: Chlorinated Biphenyl Congeners in
Water, Soil, Sediment, and Tissue by HRGC/HRMS
Extraction and Lipid Separation of Fish Samples for Contaminant Analysis
and Lipid Determination, LMMB 043
Butyltm in Sediments
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February 17.2003
oxidation
Fact Sheet #2.2.2-1
oysters
Fact Sheet # 2.3.3 - 6
PAH analysis methods
Fact Sheet #2.1.2 -14
Fact Sheet #2.1.3-13
Fact Sheet #2.1.3-14
Fact Sheet #2.2.2-6
Fact Sheet # 2.2.2 - 7
Fact Sheet # 2.3.2 - 7
Fact Sheet #2.3.2-8
Fact Sheet # 2.3.2 - 9
Total Mercury in Sludge, Settlement, Soil, and Tissue by Acid Digestion and
BrCI Oxidation, Appendix to Method 1631
Gonadal Analysis
Quantitative Determination of Polynuclear Aromatic Hydrocarbons by Gas
Chromatography/Mass Spectrometry (GC/MS) - Selected Ion Monitoring
(SIM) Mode
Toxicity Evaluations of Photoinduction of Polycyclic Aromatic Hydrocarbons
(PAH): In Situ Analysis
Toxicity Evaluations of Photoinduction of Polycyclic Aromatic Hydrocarbons:
Laboratory Analysis of Storm water
Extraction and Clean-up of Sediments for Semi-volatile Organics Following
the Internal Standard Method, LMMB 040
Quantitative Determination of Polynuclear Aromatic Hydrocarbons by Gas
Chromatography/Mass Spectometry (GC/MS)-Selected Ion Monitoring
(SIM) Mode
Extraction and Lip id Separatbn of Fish Samples for Contaminant Analysis
and Lipid Determination, LMMB 043
Purification of Biological Tissue Samples by Gel Permeation
Chromatography of Organic Analyses
Quantitative Determination of Polynuclear Aromatic Hydrocarbons by Gas
Chromatography/Mass Spectrometry (GC/MS)-Selected Ion Monitoring
(SIM) Mode
participate organic carbon (POC)
Fact Sheet # 2.1.2 - 24 Standard Method No. 5310: Total Organic Carbon
Fact Sheet # 2.1.2 - 26 Method No. LMMB 097: Standard Operating Procedure for the Analysis of
Particulate-Phase Organic Carbon in Great Lakes Waters
PCB analysis methods
Fact Sheet #2.1.2-15
Fact Sheet #2.1.2-16
Fact Sheet #2.1.2-18
Fact Sheet #2.1.2-19
Fact Sheet #2.2.2-6
Fact Sheet #2.2.2-8
Fact Sheet # 2.2.2 - 9
Fact Sheet #2.2.2-11
Fact Sheet #2.2.2-12
Method No. LMMB 041: Analysis of Polychlorinated Biphenyls and
Chlorinated Pesticides by Gas Chromatography with Electron Capture
Detection
Method No. LMMB: PCBs and Pesticides in Surface Water by XAD-2 Resin
Extraction
EPA Method No. 1668: Toxic Polychlorinated Biphenyls by Isotope Dilution
High Resolution Gas Chromatography/High Resolution Mass Spectrometry
EPA Method No. 1668, Revision A: Chlorinated Biphenyl Congeners in
Water, Soil, Sediment, and Tissue by HRGC/HRMS
Extraction and Clean-up of Sediments for Semi-volatile Organics Following
the Internal Standard Method, LMMB 040
Analysis of Polychlorinated Biphenyls and Chlorinated Pesticides by Gas
Chromatography with Electron Capture Detection, LMMB 041
Screening for Polychlorinated Biphenyls by Immunoassay. SW846 Method
4020
Toxic Polychlorinated Biphenyls by Isotope Dilution High Resolution Gas
Chromatography/High Resolution Mass Spectrometry, EPA Method 1668
Chlorinated Biphenyl Congeners in Water. Soil. Sediment, and Tissue by
HRGC/HRMS, EPA Method 1668 Revision A
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Fact Sheet #2.3.2 -7
Fact Sheet #2.3.2-8
Fact Sheet # 2.3.2 -10
Fact Sheet #2.3.2 -12
Fact Sheet #2.3.2 -13
percent dry weight
Fact Sheet #2.3.2 -14
percent lipid
Fact Sheet #2.3.2 -15
percent moisture
Fact Sheet #2.3.2 -14
periphyton
Fact Sheet #2.3.1 -6
Fact Sheet #2.3.1 -7
Fact Sheet #2.3.1 -8
Fact Sheet #2.3.1 -9
Fact Sheet #2.3.3-1
Fact Sheet #2.3.3-2
permeability
Fact Sheet # 2.2.2 - 20
pesticide analysis methods
Fact Sheet #2.1.2-16
Fact Sheet # 2.2.2 - 8
Fact Sheet # 2.3.2 - 8
Fact Sheet #2.3.2-10
Extraction and Lipid Separation of Fish Samples for Contaminant Analysis
and Lipid Determination, LMMB 043
Purification of Biological Tissue Samples by Gel Permeation
Chromatography of Organic Analyses
Analysis of Polychlorinated Biphenyls and Chlorinated Pesticides by Gas
Chromatography with Electron Capture Detection, LMMB 041
Toxic Polychlorinated Biphenyls by Isotope Dilution High Resolution Gas
Chromatography/High Resolution Mass Spectrometry, EPA Method 1668
Chlorinated Biphenyl Congeners in Water, Soil. Sediment, and Tissue by
HRGC/HRMS, EPA Method 1668 Revision A
Determination of Percent Dry Weight for Tissues
Determination of Percent Lipid in Tissue
Determination of Percent Dry Weight for Tissues
Field-based Periphyton Survey in Wadeable Streams
Laboratory-based Periphyton Survey: Single Habitat Sampling in Wadeable
Streams
Laboratory-based Rapid Periphyton Survey: Multi-habitat Sampling in
Wadeable Streams
Artificial Substrate Samplers of Macromvertebrates in Wadeable Streams
Laboratory Identification, Enumeration and Biomass Measurements of
Periphyton in Wadeable Streams
Laboratory Periphyton Biomass Determination
Standard Test Method for Permeability of Granular Soils (Constant Head),
ASTM Method D2434
Method No. LMMB: PCBs and Pesticides in Surface Water by XAD-2 Resin
Extraction
Analysis of Polychlorinated Biphenyls and Chlorinated Pesticides by Gas
Chromatography with Electron Capture Detection, LMMB 041
Purification of Biological Tissue Samples by Gel Permeation
Chromatography of Organic Analyses
Analysis of Polychlorinated Biphenyls and Chlorinated Pesticides by Gas
Chromatography with Electron Capture Detection, LMMB 041
pH
Fact Sheet # 2.1.2 - 29 Method No. LMMB 092: Standard Operating Procedure for Electrometnc pH
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phosphorus
Fact Sheet # 2.1.2 - 21 Method No. ESS Method 230.1: Total Phosphorus and Total Kjeldahl
Nitrogen, Semi-Automated Method
Fact Sheet # 2.1.2 - 22 Method No. ESS Method 310.2, LMMB 064: Phosphorus, Total, Low Level
(Persulfate Digestion)
Fact Sheet # 2.1.2 - 23 Method No. ESS Method 310.1, LMMB 063: Ortho-Phosphorus, Dissolved
Automated, Ascorbic Acid
photographic surveys
Fact Sheet # 2.3.1 -14 Photographic Habitat Documentation of the Benthic Community
Fact Sheet # 2.3.1 -15 Sediment Profile Camera
phytoplankton sampling
Fact Sheet #2.3.1 -1
Phytoplankton Sample Collection and Preservation in the Great Lakes,
LMMB023t
plasticity index
Fact Sheet # 2.2.2 - 23 Standard Test Method for Liquid Limit, Plastic Limit, and Plasticity Index of
Soils, ASTM Method D4318
polychlorinated biphenyls (see PCB analysis methods)
poly eye lie aromatic hydrocarbons (see PAH analysis methods)
pore water
Fact Sheet #2.1.1-13 In Situ Peepers
Fact Sheet # 2.1.1 -14 Suction samplers
Fact Sheet # 2.2.1 -10 Method No. ASTM E 1391-94: Pore Water Extraction through Centrifugation
Fact Sheet # 2.2.1 -11 Method No. ASTM E 1391-94: Pore Water Extraction from Sediments
through Squeezing
Fact Sheet # 2.2.1 -12 Method No. ASTM E 1391-94: Pore water extraction from sediment from
Vacuum Filtration, Gas Pressurization, or Displacement
primary productivity
Fact Sheet #2.3.1 -4
Primary Productivity Using 14C: Field Procedure in the Great Lakes, LMMB
016
radioisotopes
Fact Sheet # 2.2.2 -15 Determination of the Activity of Lead-210 in Sediments and Soils. LMMB 084
Fact Sheet # 2.2.2 - 25 Sediment Age Dating Using Cesium-137
Fact Sheet # 2.2.2 - 26 Beryllium-7 as a Tracer of Short Term Sediment Deposition
Fact Sheet # 2.3.1 - 4 Primary Productivity Using 14C: Reid Procedure in the Great Lakes, LMMB
016
respiration rate
Fact Sheet # 2.1.3 -15 Method No. NHEERL-AED SOP 1.03.013: Growth and Scope for Growth
Measurements with Mytilus edulis
scope for growth (SFG) index
Fact Sheet# 2.1.3 -15 Method No. NHEERL-AED SOP 1.03.013: Growth and Scope for Growth
Measurements with Mytilus edulis
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SCUBA
Fact Sheet #2.2.1 -4
Fact Sheet # 2.3.1 -14
sea floor mapping
Fact Sheet #2.2.1 -13
Fact Sheet #2.2.1 -14
Hand collection at depth with SCUBA
Photographic Habitat Documentation of the Benthic Community
Method No. DRP-2-03: Acoustic Sub-bottom Profiling Systems
Method No. EEDP-01-10: Side Scan Sonar
sediment consolidation
Fact Sheet #2.2.1 -15
Fact Sheet #2.2.2-21
Method No. DRP-2-3. Settlement Phases
Standard Test Method for One-Dimensional Consolidation Properties of
Soil, ASTM Method D2435
sediment cores
Fact Sheet #2.2.1 -2
Fact Sheet #2.2.1 -6
Fact Sheet #2.2.1 -7
sediment dating
Fact Sheet #2.2.2-15
Fact Sheet # 2.2.2-25
Fact Sheet # 2.2.2-26
sediment grain size
Fact Sheet #2.2.2-16
sediment flux
Fact Sheet #2.1.1 -19
Fact Sheet # 2.2.1 - 4
sediment sampling
Fact Sheet #2.2.1 -1
Fact Sheet #2.2.1 -2
Fact Sheet #2.2.1 -3
Fact Sheet #2.2.1 -4
Fact Sheet #2.2.1 -5
Fact Sheet #2.2.1 -6
Fact Sheet #2.2.1 -7
Fact Sheet #2.3.1 -11
Fact Sheet #2.3.1 -12
Fact Sheet #2.3.1 -13
sediment toxicity
Fact Sheet #2.2.3-1
Fact Sheet # 2.2.3 - 3
Fact Sheet # 2.2.3 - 4
Fact Sheet # 2.2.3 - 5
Fact Sheet # 2.2.3 - 6
Fact Sheet # 2.2.3 - 7
Core Samplers
Russian Peat Borer
Split Core Sam pier for Submerged Sediments
Determination of the Activity of Lead-210 in Sediments and Soils, LMMB 084
Sediment Age Dating Using Cesium-137
Beryllium-7 as a Tracer of Short Term Sediment Deposition
Sediment Grain Size Analysis. NHEERL-AED SOP 1.01.005
Seepage Meters
Hand collection at depth with SCUBA
Grab Sampling
Core Samplers
Hand Collection
Hand collection at depth with SCUBA
Sediment traps
Russian Peat Borer
Split Core Sampler for Submerged Sediments
Benthic Organism Collection from a Marine Environment, NHEERL-AED
SOP 1 02.001
Benthic Macroinvertebrate Protocols in a Wadeable Stream: Single Habitat
Approach, 1-Meter Kick Net
Benthic Macroinvertebrate Protocols in a Wadeable Stream. Multi-habitat
Approach: D-Frame Dip Net
Acute Freshwater Crustacean Sediment Bioassay Flow-through
Acute Freshwater Crustacean Sediment Bioassay: Static Laboratory
Exposures
Acute Freshwater Amphipod and Freshwater Insect Larvae Sediment
Bioassay, EPA Method 100.1
Chronic Freshwater Amphipod Sediment Bioassay, EPA Method 100.4
Life-Cycle Freshwater Midge Sediment Bioassay, EPA Method 100.5
Acute Larval Bivalve Sediment Bioassay
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Fact Sheet # 2.2.3 - B
Fact Sheet # 2.2.3 - 9
Fact Sheet #2.2.3 -10
Fact Sheet # 2.2.3 -11
Fact Sheet #2.2.3-12
Fact Sheet #2.2.3-13
Fact Sheet # 2.2.3 -14
Fact Sheet #2.2.3-15
Fact Sheet #2.2.3-16
Fact Sheet #2.2.3-17
Acute Echinoderm Sediment Bioassay
Acute Marine Crustacean Sediment Bioassay
Acute Marine Amphipod Crustacean Sediment Bioassay, EPA Method
100.4
Acute Marine Polychaete Sediment Bioassay, ASTM Method E1611-00
Chronic Estuarine Amphipod Sediment Bioassay
Chronic Marine Polychaete Sediment Bioassay, ASTM Method E1611-00
Ames Mutagenicity Assay
Mutatox Genotoxicity Assay
V79 Sister Chromatid Exchange Assay, NHEERL-AED SOP 1.03.012
Bioaccumutation Test for Marine, Estuarine, and Freshwater Sediments,
EPA Method 100.3
sediment water content
Fact Sheet #2.2.2-17
selected ion monitoring (SIM)
Fact Sheet # 2.2.2 - 7
Fact Sheet # 2.3.2 - 9
selenium
Fact Sheet #2.1.1-11
Fact Sheet #2.1.2-4
Fact Sheet #2.1.2-6
Fact Sheet #2.2.2-2
Fact Sheet #2.2.2 -3
Fact Sheet #2.3.2-4
Fact Sheet #2.3.2-5
Procedures for Water Content Determination
Quantitative Determination of Polynuclear Aromatic Hydrocarbons by Gas
Chromatography/Mass Spectrometry (GC/MS)-Setected Ion Monitoring
(SIM) Mode
Quantitative Determination of Polynuclear Aromatic Hydrocarbons by Gas
Chromatography/Mass Spectrometry (GC/MS)-Selected Ion Monitoring
(SIM) Mode
Method No. EPA Method 1669: Sampling Ambient Water for Trace Metals
at EPA Water Quality Criteria Levels
EPA Method No. 1639: Determination of Trace Elements in Ambient Waters
by Stabilized Temperature Graphite Furnace Atomic Absorption
EPA Method No. 1638: Determination of Trace Elements in Ambient Waters
by Inductively Coupled Plasma — Mass Spectrometry
Trace Element Quantification Techniques
Method Title: Analysis of Marine Sediment and Bivalve
Tissue by X-Ray Fluorescence, Atomic Absorption and Inductively Coupled
Plasma Mass Spectrometry
Method No. NS&T, Method Title: Trace Element Quantification
Techniques
Analysis of Marine Sediment and Bivalve Tissue by X-Ray Fluorescence,
Atomic Absorption and Inductively Coupled Plasma Mass Spectrometry
semi-volatile organic compounds
Fact Sheet* 2.1.2 -13 EPA Method No. 1625: Semi-volatile Organic Compounds by Isotope
Dilution GC/MS
Fact Sheet # 2.2.2 - 6 Extraction and Clean-up of Sediments for Semi-volatile Organics Following
the Internal Standard Method, LMMB 040
Fact Sheet # 2.3.2 -16 Microwave Extraction of Marine Tissue for Semivolatile Organic Analytes,
AED LOP 2.03.030,
Revision 0
settlement plates
Fact Sheet #2.2.1 -15
settling particulate matter
Fact Sheet #2.2.1 -5
Method No. DRP-2-3: Settlement Phases
Sediment traps
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shear strength
Fact Sheet #2.2.2-18
Standard Test Method for Field Vane Shear Test in Cohesive Soil, ASTM
Method D2573
side scan sonar
Fact Sheet #2.2.1 -14
Method No. EEDP-01-10: Side Scan Sonar
silt
Fact Sheet* 2.2.2 - 16 Sediment Grain Size Analysis, NHEERL-AED SOP 1.01.005
silicon
Fact Sheet #2.2.2 -3
Method Title: Analysis of Marine Sediment and Bivalve
Tissue by X-Ray Fluorescence, Atomic Absorption and Inductively Coupled
Plasma Mass Spectrometry
silver
Fact Sheet #2.1.1 -11
Fact Sheet #2.1.2-6
Fact Sheet # 2.2.2 - 3
Fact Sheet # 2.3.2 - 4
Method No. EPA Method 1669: Sampling Ambient Water for Trace Metals
at EPA Water Quality Criteria Levels
EPA Method No. 1638: Determination of Trace Elements in Ambient Waters
by Inductively Coupled Plasma — Mass Spectrometry
Method Title: Analysis of Marine Sediment and Bivalve
Tissue by X-Ray Fluorescence, Atomic Absorption and Inductively Coupled
Plasma Mass Spectrometry
Method No. NS&T, Method Title: Trace Element Quantification
Techniques
simultaneously extracted metals (SEM)
Fact Sheet # 2.2.2 - 4 Determination of Acid Volatile Sulfide and Selected Simultaneously
Extra eta ble Metals in Sediment
soil classification
Fact Sheet # 2.2.2 -18 Standard Test Method for Field Vane Shear Test in Cohesive Soil. ASTM
Method D2573
Fact Sheet # 2.2.2 - 19 Standard Test Method for Specific Gravity of Soil Solids by Water
Pycnometer, ASTM Method D854
Standard Test Method for Permeability of Granular Soils (Constant Head),
ASTM Method D2434
Standard Test Method for One-Dimensional Consolidation Properties of
Soil. ASTM Method D2435
Standard Test Method for Classification of Soils for Engineenng Purposes
(Unified Soil Classification System), ASTM Method D2487
Fact Sheet # 2.2.2 - 23 Standard Test Method for Liquid Limit, Plastic Limit, and Plasticity Index of
Soils. ASTM Method D4318
Fact Sheet # 2.2.2 - 20
Fact Sheet #2.2.2 -21
Fact Sheet # 2.2.2 - 22
specific gravity
Fact Sheet # 2.2.2 - 19 Standard Test Method for Specific Gravity of Soil Solids by Water
Pycnometer, ASTM Method D854
stream characterization
Fact Sheet #2.1.1 -15
Fact Sheet #2.1.1 -16
Fact Sheet #2.1.1 -17
Physical Characterization of a stream
Visual based habitat assessment
LMMB 017: USGS Field Operation Plan: Tributary Monitonng
sub-bottom profiling
Fact Sheet #2.2.1 -13
Method No. DRP-2-03: Acoustic Sub-bottom Profiling Systems
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sulfate
Fact Sheet #2.1.2-28
thallium
Fact Sheet #2.1.1 -11
tin
Fact Sheet #2.1.2-6
Fact Sheet #2.2.2-2
Fact Sheet # 2.2.2 - 3
Fact Sheet #2.3.2-4
total organic carbon (TOC)
Fact Sheet #2.1.2-24
Fact Sheet #2.2.2-14
total suspended solids (TSS)
Fact Sheet #2.1.2-32
Fact Sheet #2.1.2-33
toxicity testing
Fact Sheet #2.1.3-1
Fact Sheet #2.1.3-2
Fact Sheet #2.1.3-3
Fact Sheet #2.1.3-4
Fact Sheet #2.1.3 -5
Fact Sheet #2.1.3-6
Fact Sheet #2.1.3-7
Fact Sheet #2.1.3-8
Fact Sheet #2.1.3-9
Fact Sheet #2.1.3-10
Fact Sheet #2.1.3-11
Fact Sheet #2.1.3-12
Fact Sheet #2.1.3-13
Fact Sheet #2.1.3-14
Method No. ESS Method 200.5: Determination of Inorganic Anions in Water
by Ion Chromatography
Method No. EPA Method 1669: Sampling Ambient Water for Trace Metals
at EPA Water Quality Criteria Levels
EPA Method No. 1638: Determination of Trace Elements in Ambient Waters
by Inductively Coupled Plasma — Mass Spectrometry
Trace Element Quantification Techniques
Method Title: Analysis of Marine Sediment and Bivalve
Tissue by X-Ray Fluorescence, Atomic Absorption and Inductively Coupled
Plasma Mass Spectrometry
Method No NS&T, Method Title: Trace Element Quantification
Techniques
Standard Method No. 5310: Total Organic Carbon
Procedures for Sediment Total Organic Carbon (TOC) Determination
Method No. LMMB 090: Standard Operating Procedure forGLNPO
Turbidity: Nephelometeric Method
Method No. LMMB 065: ESS Method 340.2: Total Suspended Solids, Mass
Balance (Dried at 103-105EC) Volatile Suspended Solids (Ignited at 550EC)
Method No. ERT SOP 2024: Acute Freshwater Crustacean Bioassay: 48
Hours
Method No. ERT SOP 2022: Acute Freshwater fish Bioassay
Method No. ERT SOP 2027: Chronic Freshwater Algae Test
Method No. ERT SOP 2025: Chronic Freshwater Crustacean Bioassay
(7day)
Method No. ERT SOP 2028. Chronic Freshwater Crustaceans Bioassay (10
days)
Method No. ERT SOP 2026: Chronic Freshwater Fish Bioassay, ERT SOP
2026
Method No. NHEERL-AED SOP 1.03.001: Chronic Marine Macroalgae,
Champia parvula, Sexual Reproduction test
Method No. NHEERL-AED SOP 1.03.003: Acute Marine Crustacean
Bioassay
Method No. NHEERL-AED SOP 1.03.003: Acute Marine Fish Bioassay
Method No. NHEERL-AED SOP 1.03.005: Chronic Estuarine Survival.
Growth, and Fecundity Test
Method No. NHEERL-AED SOP 1.03.006: Chronic Echinoderm Fertilization
Test
Method No NHEERL-AED SOP 1 03.004: Chronic Marine Fish Bioassay
Toxicity Evaluations of Photoinduction of Polycyclic Aromatic Hydrocarbons
(PAH): In Situ Analysis
Toxicity Evaluations of Photoinduction of Polycyclic Aromatic Hydrocarbons:
Laboratory Analysis of Storm water
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Fact Sheet #2.1.3 -16
Fact Sheet #2.2.3-1
Fact Sheet # 2.2.3 - 2
Method No. NHEERL-AED SOP 1.03.009: Microtox® tests. NHEERL-AED
1.03.009
Acute Freshwater Crustacean Sediment Bioassay: Flow-through
Acute Freshwater Crustacean Sediment Bioassay: In Situ Exposures
toxicology testing - sample prep
Fact Sheet #2.2.1 -8
Fact Sheet # 2.2.1 - 9
Fact Sheet #2.2.1 -10
Fact Sheet #2.2.1 -11
Fact Sheet # 2.2.1 -12
trace metals analysis
Fact Sheet #2.1.2-1
Fact Sheet #2.1.2-2
Fact Sheet #2.1.2-3
Fact Sheet #2.1.2-4
Fact Sheet #2.1.2-5
Fact Sheet #2.1.2-6
Fact Sheet #2.1.2-7
Fact Sheet # 2.2.2 - 2
Fact Sheet # 2.2.2 - 3
Fact Sheet # 2.3.2 - 4
Fact Sheet #2.3.2-5
transparency
Fact Sheet #2.1.1-4
trawling
Fact Sheet #2.3.1 -25
Sediment Processing for Chemistry and Toxicity Testing
Sediment Processing for Elutriate Toxicity tests
Method No. ASTM E 1391-94: Pore Water Extraction through Centrifugation
Method No. ASTM E 1391-94: Pore Water Extraction from Sediments
through Squeezing
Method No. ASTM E 1391-94: Pore water extraction from sediment from
Vacuum Filtration, Gas Pressurization, or Displacement
EPA Method No. 245.7: Mercury in Water by Cold Vapor Atomic
Fluorescence Spectrometry
EPA Method No. 1631, Revision B- Mercury in Water by Oxidation, Purge
and Trap, and Cold Vapor Atomic Fluorescence Spectrometry
EPA Method No. 1630. Methyl mercury in water by distillation. Aqueous
Ethylaton, Purge and Trap, and CVAFS
EPA Method No. 1639: Determination of Trace Elements in AmbientWaters
by Stabilized Temperature Graphite Furnace Atomic Absorption
EPA Method No. 1637- Determination of Trace Elements in AmbientWaters
by Off-line Chelation Pre-concentratbn and Stabilized Temperature
Graphite Furnace Atomic Absorptbn
EPA Method No. 1638: Determination of Trace Elements in AmbientWaters
by Inductively Coupled Plasma — Mass Spectrometry
EPA Method No. 1640: Determination of Trace Elements in AmbientWaters
by On-Line Chelation Pre-concentratbn and Inductively Coupled Plasma-
Mass Spectrometry
Trace Element Quantification Techniques
Analysis of Marine Sediment and Bivalve Tissue by X-Ray Fluorescence,
Atomic Absorptbn and Inductively Coupled Plasma Mass Spectrometry
Trace Element Quantification Techniques
Analysis of Marine Sediment and Bivalve Tissue by X-Ray Fluorescence,
Atomic Absorptbn and Inductively Coupled Plasma Mass Spectrometry
In Situ Transparency Sampling
Trawls
turbidity
Fact Sheet # 2.1.2 - 32 Method No. LMMB 090: Standard Operating Procedure for GLNPO
Turbidity: Nephelometeric Method
volatile organic compounds (VOC)
Fact Sheet # 2.1.2 -12 Method No. OERR SOP #2109. Photovac GC Analysis for Soil, Water, and
Air/Soil Gas
Fact Sheet # 2.2.2 - 5 Photovac GC Analysis for Soil, Water, and Air/Soil Gas. OSWER SOP#
2109
water column characterization
272
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A Compendium of Chemical, Physical and Biological Methods
for Assessing and Monitoring the Remediation of Contaminated Sediment Sites
February 17, 2003
Fact Sheet # 2.3.3 - 4 Laboratory Analysis of Water Column Organisms
water pycnometer
Fact Sheet #2.2.2-19
water velocity
Fact Sheet #2.1.1 -18
x-ray fluorescence
Fact Sheet #2.2.2-3
Fact Sheet #2.2.2-24
Standard Test Method for Specific Gravity of Soil Solids by Water
Pycnometer, ASTM Method D854
Quality Assurance Plan for Discharge Measurements Using Broadband
Acoustic Doppler Current Profilers
Analysis of Marine Sediment and Bivalve Tissue by X-Ray Fluorescence.
Atomic Absorption and Inductively Coupled Plasma Mass Spectrometry
Field Portable X-Ray Fluorescence Spectrometry for the Determination of
Elemental Concentrations in Soil and Sediment
zinc
Fact Sheet #2.1.1 -11
Fact Sheet #2.1.2-4
Fact Sheet #2.1.2-6
Fact Sheet # 2.2.2 - 2
Fact Sheet # 2.2.2 - 3
Fact Sheet # 2.3.2 - 4
Fact Sheet # 2.3.2 - 5
zooplankton sampling
Fact Sheet #2.3.1 -5
Method No. EPA Method 1669: Sampling Ambient Water for Trace Metals
at EPA Water Quality Criteria Levels
EPA Method No. 1639: Determination of Trace Elements in AmbientWaters
by Stabilized Temperature Graphite Furnace Atomic Absorption
EPA Method No. 1638: Determination of Trace Elements in AmbientWaters
by Inductively Coupled Plasma — Mass Spectrometry
Trace Element Quantification Techniques
Method Title: Analysis of Marine Sediment and Bivalve
Tissue by X-Ray Fluorescence, Atomic Absorption and Inductively Coupled
Plasma Mass Spectrometry
Method No. NS&T, Method Title: Trace Element Quantification
Techniques
Analysis of Marine Sediment and Bivalve Tissue by X-Ray Fluorescence,
Atomic Absorption and Inductively Coupled Plasma Mass Spectrometry
Zooplankton Sample Collection and Preservation in the Great Lakes, LMMB
024
273
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?/EPA
United States
Environmental Protection
Agency
National Risk Management
Research Laboratory
Cincinnati, OH 45268
Official Business
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Permit No. G-35
EPA/6007R-03/108
April 2004
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