UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT AND COMPLIANCE ASSURANCE
OFFICE OF CRIMINAL ENFORCEMENT, FORENSICS AND TRAINING
ENVIRONMENTAL CRIME
er A. Sijggs, MS
"Yarbrough, BS
Barbara L;
assistance provided by:
, NEIC '-?:\... 1
( Vis-tronix)
14th International
Author to whom
Bldg. 25,
NATIONAL
Diana
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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT AND COMPLIANCE ASSURANCE
OFFICE OF CRIMINAL ENFORCEMENT, FORENSICS AND TRAINING
ENVIRONMENTAL CRIME
Jennifer A. Suggs, MS
Kenna R. Yarbrough, BS
Library assistance provided by:
Dorothy E. Biggs, NEIC
Barbara L. Wagner, Contractor (Vistronix)
Nancy B. Greer, Contractor (Vistronix)
Prepared for:
14th International Forensic Science Symposium
Author to whom correspondence should be addressed:
Jennifer A. Suggs
EPA-NEIC
Bldg. 25, Denver Federal Center
Denver, CO 80225
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Diana A. Love, Director
Denver, Colorado
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CONTENTS
LIST OF ACRONYMS[[[3
INTRODUCTION [[[6
OVERVIEW [[[6
AUTHORS' PERSPECTIVE[[[6
ENVIRONMENTAL CRIME SCENE[[[ 7
VOLUNTARY CONSENSUS STANDARDS AND
METHOD STANDARDIZATION """"""""""""""""""""""""""".........................7
SAMPLING GUIDANCE [[[8
LABORATORY ANALYSIS OF ENVIRONMENTAL SAMPLES........................................... 10
RECENT. BOOKS [[[10
General Environmental Chemistry Books ...... ..... .."......... ............. ........... ................. ........10
General Instrument Techniques Books.......................... .............. ........... ....... ............... .....10
Method and Technique Specific Books............ ......................... ........................ ............. ...11
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LIST OF ACRONYMS
Il-AED - micro-atomic emission detector
Il-ECD - micro-electron capture detector
AA - atomic absorption
AAS - atomic absorption spectrometry
AE - atomic emission
AED - atomic emission detection
AES - atomic emission spectrometry
AF - atomic fluorescence
ANSI - American National Standards Institute
AOCD - 9-(2-acridone)oxyethylcarbonylimidazole
APCI - atmospheric pressure chemical ionization (mode)
APEO - alkylphenol ethoxylate
ASE - accelerated solvent extraction
A TR - attenuated total reflectance
BFRs - brominated flame retardants
BTEX - benzene, toluene, ethylbenzene, and xylene
CAA - Clean Air Act
CAS - Chemical Abstracts Service (as in CAS #)
CDFMS - compact double-focusing mass spectrometer
CE - capillary electrophoresis
CERCLA - Comprehensive Environmental Response, Compensation, and Liability Act
CFR - US Code of Federal Regulations
CIT - cylindrical ion trap .
CLU-IN - USEPA Technology Innovation Program. Hazardous Waste Clean-Up Information
CMC - chromatomembrane cells
CRM - certified reference material
CW A - Clean Water Act
DFG - Deutsche Forschungsgemeinschaft (German Research Foundation)
ECD - electron capture detector
EDCs - endocrine disrupting compounds or endocrine disrupting chemicals
EDSP - Endocrine Disruptor Screening Program
EDXRF - energy dispersive X-ray fluorescence
EPCRA - Emergency Planning and Community Right-To-Know Act
ES - electrospray
ESA - Endangered Species Act
ESI - electro spray ionization (mode)
ET AAS - electrothermal atomic absorption spectrometry
ETV - electrothermal vaporization
FA - flow analysis
F AAS - flame atomic absorption spectrometry
FEM - USEP A Forum on Environmental Measurement
FFDCA -Federal Food, Drug and Cosmetic Act
PI - flow injection
FID - flame ionization detector
FIFRA - Federal Insecticide, Fungicide, and Rodenticide Act
FIMS - fiber introduction mass spectrometry
FLD - fluorescence detection
FM - focused-microwave (irradiation)
FMASE - focused-microwave assisted Soxhlet extraction
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FMOC - 9-fluorenylmethyl chloroformate
FPC - focal plane camera
FPD - flame photometric detection
FSL - fused-silica-lined
Ff - Fourier transform
FfIR - Fourier transform infrared (spectrometry)
GC - gas chromatography
GC x GC - two-dimensional gas chromatography
GD - glow discharge
GPO - US Government Printing Office
HFs - hydraulic fluids
HG - hydride generation
HPLC - high performance liquid chromatography
HS - headspace
IC - ion chromatography
ICP - inductively coupled plasma
ICR - ion cyclotron resonance
IR - infrared
ISO - International Organization for Standardization
LC -liquid chromatography
LIP -laser induced fluorescence
LLLME - liquid-liquid-liquid microextraction
LPME - liquid-phase microextraction
LVI -large-volume injection
MAE - microwave assisted extraction
MC - multi collector
MEC - microwave enhanced chemistry
MIP - molecularly imprinted polymer
MS - mass spectrometry
MTBE - methyl t-butyl ether
MWFs - metalworking fluids
NCI - negative chemical ionization
NEIC - National Enforcement Investigations Center
NEPA - National Environmental Policy Act
NI - negative ion (mode)
NICI - negative ion chemical ionization
NIST - National Institute of Standards and Technology
NMR - nuclear magnetic resonance
NSAIDs - nonsteroidal anti-inflammatory drugs
NTIS - National Technical Information Service
NTT AA - National Technology Transfer and Advancement Act
OCPs - organochlorine pesticides
OERR - USEP A Office of Emergency a~d Remedial Response
OES - optical emission spectrometry
OMB - US Office of Management and Budget
OP A - Oil Pollution Act
ORD - USEP A Office of Research and Development
OSWER - USEP A Office of Solid Waste and Emergency Response
OV As - organic vapor analyzers
P AHs - polycyclic aromatic hydrocarbons or polynuclear aromatic hydrocarbons
PBDEs - polybrominated diphenyl ethers
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PCBs - polychlorinated biphenyls
PCDDs - polychlorinated dibenzodioxins or polychlorinated dibenzo-p-dioxins
PCDFs - polychlorinated dibenzofurans
PFBBR - pentafluorobenzyl bromide
PFE - pressurized fluid extraction
PFP A - pentafluoropropionic acid
PI - positive ion (mode)
PID - photoionization detector
PIP - photochemically induced fluorimetry
PLE - pressurized liquid extraction
PM - particulate matter
PP A - Pollution Prevention Act
PPCPs - pharmaceuticals and personal care products
PXRF - portable X-ray fluorescence
PyGC - flash pyrolysis gas chromatography
RCRA - Resource Conservation and Recovery Act
RP - reversed-phase
SARA - Superfund Amendments and Reauthorization Act
SBSE - stir bar sorptive extraction
SCCPs - short-chain chlorinated paraffins
SDW A - Safe Drinking Water Act
SES - sequential extraction schemes
SF - sector field
SIA - sequential injection analysis
SIM - selected ion monitoring
SPE - solid phase extraction
SPME - solid-phase microextraction
SRMs - standard reference materials
SSPE - sequential solid-phase extraction
SVOCs - semi-volatile organic compounds
SW-846 - Test Methodsfor Evaluating Solid Waste: Physical/Chemical Methods
TBA - t-butyl alcohol
TBT - tributyltin
THMs - trihalomethanes
TIC - total ion chromatogram
TLC - thin-layer chromatography
TMA - trimethylamine
TMSD - trimethylsilyldiazomethane
TMSI - N-trimethylsilylimidazole
TOF - time-of-flight
TSCA - Toxic Substances Control Act
TXRF - total reflection X-ray fluorescence
UE - ultrasonic extraction
US - United States
USEP A - United States Environmental Protection Agency
USGS - United States Geological Survey
VOCs - volatile organic compounds
WRI - USGS Water-Resources Investigations Report
WWTP - wastewater treatment plant
XRF - X-ray fluorescence
XRS - X-ray spectrometry
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INTRODUCTION
OVERVIEW
This environmental crime review is a follow-up to the 2001 review paper prepared for the
13th International Forensic Science Symposium. 1 Some information presented earlier will be
repeated such as resources for sampling methods and the annual or biannual instrumentation
reviews regularly featured in some journals. Other topics within the paper are new or in an
expanded presentation such as consensus standards, environmental measurements, sampling
guidance, and endocrine disrupting compounds.
The paper will proceed in an order roughly resembling that taken during an
environmental crime investigation, as the previous review paper did. Information regarding the
fieldwork or work at the actual crime scene will be presented first then followed by a section on
analytical methods developed and published during the past 3 years. Reference information has
been gathered from books, websites, and journals.
AUTHORS' PERSPECTIVE
The United States Environmental Protection Agency (USEP A) was established to protect
human health and the environment in the United States (US). Several environmental laws
provide the guidance for this mission (a list of major environmental laws is provided in
Appendix A). The National Enforcement Investigations Center (NEIC) is part of the USEP A. 2
The NEIC investigates, develops, and assists in prosecuting environmental crimes.
The Code of Federal Regulations (CPR) contains the guidance, requirements, and
boundaries for environmental crime investigations. 3 The USEP A is bound by these regulations
for the prosecution of environmental crime cases. Many specific sampling and testing methods
are required by law for the prosecution of an environmental crime. Much of the information
presented here (for example, alternate methodologies) is not being used in the prosecution of
environmental crimes in the United States, but it is our hope that it may be useful to other
environmental protection entities.
While the USEP A NEIC is limited to enforcement, other sections of the agency are
involved in the research of new environmental issues, the development of methods for
identification and quantitation of hazardous substances, and the development of improved ways
of sampling and assessing sites, as well as improving the treatment or recovery of these same
sites. The Office of Research and Development (ORD) is the scientific research arm of the
USEP A. ORD has eight priority areas for scientific research: air, drinking water, ecosystem
assessment and restoration, global change, human health protection, water ~uality, pollution
prevention and new technologies, and endocrine disrupting chemicals (EDCs). Internationally,
endocrine disrupting chemicals (or endocrine disrupting compounds) and the affects of these
chemicals on human and environmental health are developing areas of concern. A brief section
on EDCs and analytical techniques for the identification and quantitation of EDCs has been
included after the laboratory methods section.
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ENVIRONMENTAL CRIME SCENE
Decisions made by investigators regarding an environmental investigation must be
supported by facts obtained about the scene. If samples are taken and if laboratory analysis
occurs, all individuals gathering information and evidence need to maintain certain high
standards of care that will enable results to be accurate and reproducible. Several organizations
are involved in developing consistent, quality standards for sampling and field measurements.
The general agreements on what should be included in the quality standards become consensus
standards.
VOLUNTARY CONSENSUS STANDARDS AND METHOD ST ANDARDIZA TION
Voluntary consensus standards are standards developed or adopted by voluntary
consensus standards bodies. These bodies must agree to make the standards available on a non-
discriminatory, royalty-free or reasonable royalty basis to all interested parties. Voluntary
standards are distinguished from mandatory standards, which are published standards that are
part of a code, rule or regulation and there is an obligation by certain parties to conform to the
standard. Some voluntary standards become de-facto mandatory standards when they are
referenced or required by a code, rule, or r~gulation.
In February 1998, the revised circular No. A-119 was published by the Office of
Management and Budget (OMB) concerning federal participation in the development and use of
voluntary consensus standards. 5 The circular directs US federal agencies to use voluntary
consensus standards in lieu of government-unique standards except where inconsistent with law
or otherwise impractical. This circular was developed due to the approval of the 1995 National
Technology Transfer and Advancement Act (NTT AA) which emphasized the use by federal
agencies of standards developed by private, consensus organizations. 6 A recent article in ASTM
Standardization News makes the point that regulators may be forced to change regulations to
incorporate provisions of relevant consensus standards. 7
The American National Standards Institute (ANSI) is a private, non-profit organization
that administers and coordinates the US voluntary standardization system. 8 It is the official US
representative to the world's leading standards bodies, including the International Organization
for Standardization (ISO). ANSI has a membership of approximately 1000 companies,
organizations, government agencies and others. Although ANSI doesn't develop standards, it
provides interested parties a setting to come together, working toward common agreements. A
1996 National Institute of Standards and Technology (NIST) document reports that there are
almost 700 standards producing bodies in the United States, with more than 93,000 standards
produced. 9 The NSSN is a product of ANSI, and serves as a comprehensive data network on
developing and approved nationallinternational standards and regulatory documents on the
World Wide Web. 10 The NSSN routes different users to both commercially available and
regulatory technical documents that they may need. NSSN has many helpful lists concerning
consensus standards and the bodies that develop them, for example, the acronym directory of US
standards developers. II This list is updated regularly.
Environmental measurement related voluntary consensus standards are developed from
many different national and international organizations. The ISO produces the largest number of
international standards. 12 ISO has standards concerning environmental measurements and
sampling, particularly wastewater sampling, and these standards are available for purchase on the
organization's webpage. 13 ASTM International is also one of the largest voluntary consensus
standard development organizations in the world. This organization has many different
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committees and subcommittees on environmental measurements. 14 The ASTM committee on
Waste Sampling is designated as D-34. This committee focuses on the promotion of knowledge,
stimulation of research and development of test methods, practices, etc. relating to the
management of wastes, especially as they relate to sampling of waste streams. Other ASTM
International committees concerning environmental measurements and sampling are D-18, Soil
and Rock; D-19, Water; and D-22, Sampling and Analysis of Atmospheres. Of additional
interest is Committee E-30, Forensic Sciences. The scope of this committee focuses on the
promotion of knowledge and development of standards for methods and standard reference
materials for the collection, preservation, scientific examination, preparation and reports relating
to physical evidence for forensic purposes and the general practice of forensic science.
Additional information concerning these committees and the standards available for purchase is
located on the organization's webpage. 15
The USEP A has created a Forum on Environmental Measurement (FEM). 16 This
committee of senior USEP A managers was formed in order to enhance measurement programs
by agreeing on basic principles to promote consistency and consensus within the agency on
measurement issues. Some Agency-wide measurement issues that are being worked on include:
. Validation of new USEP A measurement methods
. Identifying and correcting problems with existing measurement methods
. Ensuring and demonstrating the competency of USEP A laboratories
. Consolidation USEP A supported measurement science conferences and
. Use of performance approach in USEP A-mandated monitoring programs
The work being performed concerning validation of new USEP A measurement methods
is to help the FEM develop guidelines as to what represents the minimum level of method
validation and peer review before methods are issued by the Agency.
SAMPLING GUIDANCE
The USEPA publication, SW-846, titled Test Methods for Evaluating Solid Waste,
Physical/Chemical Methods is the USEPA's official compendium of analytical and sampling
methods that have been evaluated and approved for use in complying with the USEPA's waste
regulations (Resource Conservation and Recovery Act or RCRA). 17 This guidance publication
has acceptable, through not required, methods for the regulated/regulating communities to use
for RCRA-related sampling and analysis requirements. Chapters 9 and 10 of SW-846 concern
developing sampling plans and sample methodologies. The multi-volume publication changes
over time as new information and data are available. The current version is available on-line or
an official printed copy of SW -846 and most of its updates can be purchased from either the US
Government Printing Office (GPO) or the National Technical Information Service (NTIS). 18, 19
In October 2002, the USEP A made available a new draft guidance document for public comment
entitled "RCRA Waste Sampling Draft Technical Guidance." This new RCRA waste sampling
guidance updates the information provided in Chapter 9 of SW -846, which was last published in
1986, and is also available on-line.
Methods and Guidance for Analysis of Water is the USEPA's primary resource for
sampling and analyses of water. This resource was most recently updated in 1999. 20 The
USEPA Office of Solid Waste and Emergency Response (OSWER) published a groundwater
forum issue paper in 2002 with the most up-to-date groundwater sampling issues and guidelines.
21 Most air emission sampling and measurement methods for the US EP A have been proposed or
promulgated in the Federal Register and codified in the Code of Federal Regulations (CFR). The
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methods are directly cited by specific regulations for determining compliance under the air
regulations in 40 CFR Parts 60, 61, and 63.3
Within the USEP A Office of Emergency and Remedial Response (OERR) Superfund
program for cleaning up abandoned waste sites, there are several representative sampling
guidances for air, water, sediment/soil, biota, and waste. 22-26 These and other sampling and
environmental technologies are available through the USEPA Technology Innovation program's
Hazardous Waste Clean-Up Information (CLU-IN) internet site. 27 The USEPA's Information
Sources webpage lists hundreds of published reports and test methods/sampling procedures and
many are available for direct downloading. 28 Also, the USEPA's most comprehensive list of
sampling, measurement, and analytical test methods was developed by the Region 1 library staff.
29 The list is continually updated, currently contains about 1600 methods, and the majority of
sources listed have live web links to the actual method.
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LABORATORY ANALYSIS OF ENVIRONMENTAL SAMPLES
Environmental analysis continues to be a growing field and while not all current areas of
study can be applied directly to environmental crime investigations, the research can provide
insights into the latent potential of new developments in instrumentation and techniques.
RECENT BOOKS
General Environmental Chemistry Books
A few books published during the past three years provide introductions for the
newcomer into environmental chemistry. The Fundamentals of Environmental Chemistry
textbook has a fast, basic overview of environmental chemistry. The first third of the book
consists of a general chemistry primer with a touch of biochemistry. The rest of the book
provides a quick, clear foundation for learning about the environmental chemistry and pollution
of water, soil and the atmosphere. Topics in this section progress to include industrial ecol08Y'
hazardous wastes, toxicological chemistry, analytical chemistry, and environmental analysis. 3
Environmental Organic Chemistry is a textbook that progresses from the basic makeup of
organic compounds to the interaction of these compounds in environmental systems. Major
sections include the introduction to basic concepts in organic chemistry, the equilibrium between
the gas, liquid and solid phases, transformation processes of organic compounds (chemical,
photochemical and biological), transport phenomena (diffusion and interaction between
boundaries, for example, the air-water interface) and environmental case studies combining the
concepts presented throughout the book. One clear benefit to the user of this book is the
extensive bibliography allowing further follow-up for the subjects covered in the book. 31
Soil and Environmental Analysis is an updated book on analytical techniques for the
analysis of environmental samples-primarily soil, but topics do include some water and gas
analyses. Each chapter provides a general background on techniques and addresses several
technique-specific concerns like sample preparation, sample introduction systems and specific
applications of the technique within environmental analysis. 32
Introduction to Environmental Forensics walks the reader through the early steps of an
environmental forensic investigation (witness statements, historical documents, and photographic
records) into the analytical measurements taken for forensic use. The majority of the book deals
with the measurements and includes topics such as chemical fingerprinting of hydrocarbons, air
dispersion modeling, particulate pattern recognition and statistical methods. Each chapter
provides a list of references or additional reading sources at the end and the appendices contain
detailed chlorinated solvent information (history, chemical names, commercial synonyms, and
chemical properties). 33
General Instrument Technique Books
A history of mass spectrometry (MS) and its developments in sample introduction and
detection is given by de Laeter in the first portion of his book, Applications of Inorganic Mass
Spectrometry. The majority of the book contains an overview of the large number of
applications for the MS technique including a chapter on environmental science. de Laeter's
book also has extensive references at the end of each chapter. 34
U.S
EPA Headquarters Library
Mail code 3404T
1200 Pennsylvania Avenue NW
Washington, DC 20460
202-566-0556
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X-Ray Spectrometry: Recent Technological Advances is an up-to-date review of progress
in X-ray spectrometry (XRS); most of the references within this book are less than eight years
old. It does not revisit the fundamentals of analytical chemistry techniques based on X-rays, but
does include references to handbooks and text books that provide the basic information. Early
chapters include details on advances and improvements in X-ray sources, optics and detector
technology. Other sections are dedicated to special XRS configurations, computerized advances
and developments in specific fields. 35
According to one of the editors, R. Van Grieken, there has been a steady increase in the
amount of work published on the environmental applications of XRS analysis. A section worth
highlighting is the one titled "Portable Equipment for X-ray Fluorescence Analysis." The
authors describe the form and function of energy-dispersive X-ray fluorescence (EDXRF)
equipment and the advances of internal construction-the miniatures and lightweight solutions
for X-ray tubes and detectors. The portable EDXRF systems rival laboratory-sized
spectrometers in analytical capability and have the advantage of providing results "on the scene"
for immediate decision-making.
Budde in Analytical Mass Spectrometry: Strategies for Environmental and Related
Applications presents gas chromatography coupled with mass spectrometry (GC/MS) analyses as
the "killer application" of mass spectrometry and the bulk of the book is dedicated to GC/MS
methods. The author limits his scope to those methods used by the USEP A and the chapters
separate into organic and semi-volatile organic compounds amenable to gas chromatography
(separate chapters), strategies to improve analytical results, and compounds that are not
amenable to GC. A brief mention of ICP/MS is near the end of the book. 36
Method and Technique Specific Books
The "Air Analysis" group of the Deutsche Forschungsgemeinschaft (DFG), the German
Research Foundation, published a tidy, well-organized source of methods for the analysis of
hazardous materials in the air in several volumes. The most recent volume is #8 and among the
analytical methods included are ones for atrazine (herbicide), polychlorinated biphenyls (PCBs),
polycyclic aromatic hydrocarbons (PAHs), and lacquer aerosols. A brief method summary with
a description of the substance (CAS #, structure, physical properties and synonyms) and the data
quality results (accuracy, recovery and limit of quantitation) begins each method. Methods
include extensive details on equipment, chemicals and solutions, sample collection, operating
conditions, sources of error and references. At the back of the book, there is a list of the methods
contained in volumes #1-8. The list is in numerical order by the CAS # of the substance. 37
The US Geological Survey (USGS) National Water Quality Laboratory has published
several methods of analysis for contaminants in water samples or sediment samples in the Water-
Resources Investigations Report (WRI) series. Methods include both organic and inorganic
analyses. A list of the available methods and information on how to obtain these reports is
provided in Appendix B.
Crompton wrote an exceptional reference book on preconcentration techniques for the
analysis of organics, organometallics and inorganics (divided into cations and anions) for water
samples. Each major section ends with one or more summary tables for preconcentration of
specific types of compounds (hydrocarbons, PCBs, insecticides and herbicides, etc.) or within
certain matrices (non-saline water, sea water, surface water, wastewater, etc.). Crompton
provides references for every method and has organized this book to be a master source of
information on preconcentration techniques. 38
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Substance Specific Books
Organometallic Compounds in the Environment provides analytical methods and
environmental details (toxicology, pathways, fate, etc.) for organometallic compounds
containing Hg, Sn, Pb, As, Sb, Si, Se, Tl, Bi, Cd, Te, Mn, Ge or Co. 39
A hefty two-volume set titled Handbook of Residue Analytical Methods for
Agrochemicals contains sections of compound classes and the analytical methods for each class.
Some method information is specific to one compound within the particular class. In addition to
the compound class section, volume two has "best practices in the generation and analyses of
residues in environmental samples" including water, soil, sediment, and air samples. 40,41
If an environmental release of a petroleum product must be investigated, Analytical
Advances for Hydrocarbon Research contains a variety of techniques including gas
chromatography (GC), gas chromatography mass spectrometry (GC-MS), liquid chromatography
mass spectrometry (LC-MS), thin-layer chromatography (TLC), and X-ray spectrometry (XRS)
for the characterization of petroleum and fossil fuel samples. 42 ASTM International has
published tables of test methods for products like aviation fuel, automotive gasoline, fuel
oxygenates, crude oils, and more. A brief quality assurance section and a detailed sampling
section (with diagrams) are included. 43
INSTRUMENT A TION AND TECHNIQUES BY TOPIC
Environmental Analysis
. Biennial review; developments in mass spectrometry as applied to environmental
analysis; primarily includes work published during 2002 and 2003 44
. Annual review of atomic spectrometry as applied to environmental analysis; major
sections are divided by the matrix (air, water, soil and plant material, and geologic
materials) 45 ..
. Biennial review; developments in environmental analytical chemistry from 2001 and
2002; contents include sampling, extraction methods, detection techniques, analytes of
interest and emerging trends 46
. Annual review; analysis of environmental samples by atomic spectroscopy; divided into
analysis categories of air, water, soils, and geologic materials 47
. Review; covers developments in environmental mass spectrometry during 2000 and 2001
with emphasis on new and emerging contaminants and issues 48
Sampling, SJmPle Preservation, Sample Preparation
.I
.
Review; addresses changes that may occur in water samples during storage and
techniques for water sample preservation 49
Reviews factors affecting stability of inorganic mercury and methylmercury during
sample stora~e, mechanisms for loss of mercury, and suggested treatments to decrease
these losses 5
Review; methods of sample preparation for separation techniques; includes examples of
extraction and concentration of analytes from solid, liquid, and gas matrices 51
Sample pretreatment using chromatomembrane cells (CMC) for extraction and
preconcentration of pollutants (polycyclic aromatic hydrocarbons and extractable organic
halogens) from wastewater 52
.
.
.
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.
Addresses sample handling and analysis for resin acids in water samples; provides tables
of analytical techniques (primarily gas chromatography and liquid chromatography, with
various detectors) 53
Extraction
.
Comprehensive review of sequential extraction schemes (SES) for metal fractionation of
environmental samples; massive applications tables of SES based on types of samples
(soils, sediments, sewage sludges, etc.) 54
Comparison of leaching tests on various soils and sediments for the extraction of Cd, Cr,
Cu, Ni, Pb, and Zn 55
Use of an ultrasound accelerated sequential extraction method for rapid metal partitioning
profiles; study compares results from conventional extraction and ultrasound extraction
on compost samples 56
Ultrasonic extraction (UE) as sample preparation technique for elemental analysis;
extracted standard reference materials and analyzed by inductively coupled plasma
atomic emission spectrometry (ICP-AES) 57
Comparison of ultrasound-assisted extraction to other techniques (Soxhlet, microwave-
assisted, and supercritical fluid extraction) 58
Chelating polymeric sorbent for metal ion extraction (Mn, Pb, Ni, Co, Cu, Cd and Zn);
method applied to sea water, well water, and tap water samples 59
Methods of extraction for isolating and preconcentrating organic analytes from
. I. 60
envlronmenta matnces
.
.
.
.
.
.
Air Analysis
.
Study of recoveries and stabilities of volatile organic compounds (VOCs) stored in fused-
silica-lined (FSL) and SUMMA polished canisters; tables of recoveries under various
humidified conditions and over various time intervals at a set relative humidity 61
System for generating gas mixtures of volatile and semi-volatile organic compounds
(VOCs and SVOCs) for use as calibration standards prior to air sampling and analysis 62
Development of a solid-phase microextraction (SPME) technique for the ana~sis of
odorous gases (triethylamine, propionic and butyric acids, and sulfur compounds) 3
Method for the sampling and analysis of airborne particulate matter (PM) from an
inhaler-administered drug, spray insect repellant, and tailpipe diesel exhaust by SPME
fibers and a needle trap device; the designed devices proved useful for simple and
inexpensive screening and were robust enough for field sampling 64
Use of microwave heating for the preparation of gas standards containing mixtures of
VOCs and SVOCs; method uses a domestic microwave oven and 1 liter gas-sampling
bulbs 65
.
.
.
.
Water Analysis
.
Biennial review; developments in water analysis during 2001 and 2002; contents focus on
new, emerging contaminants and environmental issues 66
Methods of analysis of methyl tert-butyl ether (MTBE) and tert-butyl alcohol (TBA) in
ground and surface water samples; summarizes issues with direct aqueous injection,
headspace analysis, purge-and-trap, and solid-phase microextraction 67
Review; analysis for organic contaminants in sea water sam£les; includes table of
analytes, pre-treatment, analysis technique, and limit of detection 8
.
.
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. Brief review of methods for the determination of organochlorine compounds in
wastewater discharge samples 69
. Fast, inexpensive screening method for heavy metal contamination in water samples 70
. Sample screening method for benzene, toluene, ethylbenzene, and xylenes (BTEX) in
water using a headspace sampler with a mass spectrometer 71
Pesticides, Herbicides, Insecticides
. . Method for determining pesticides in environmental ground and surface water using
solid-phase extraction (SPE) with liquid chromatography (LC) electrospray (ESI) tandem
mass spectrometry (MS-MS) 72
. Methods and instrumentation used to detect substituted urea compounds used as
herbicides and insecticides; techniques include gas chromatography, liquid
chromatography (and coupling of both to mass spectrometry detectors) and capillary
electrophoresis (CE) 73
. Solid-phase extraction of sulfonylurea herbicides in water and soil samples using a
molecularly imprinted polymer (MIP) 74
. Study of pyrethroid insecticide tralomethrin and its transformation product, deltamethrin,
in gas chromatographic (GC) pesticide residue analysis; separation and identification of
compounds were possible using LC-MS 75
. Determination of organophosphorus pesticides in aqueous samples by SPME and GC
with flame photometric detection (FPD) 76
. Comparison of different SPME fiber coatings for the extraction and analysis of
organochlorine pesticides in groundwater; optimized methods for each fiber type were
applied to the analysis of polluted groundwater samples 77
. Determination of residues of eight selected herbicides (trifluralin, butachlor, pretilachlor,
metolachlor, atrazine, acetochlor, alachlor, and fluroxypyr-meptyl) in groundwater
samples by SPME 78
. Comparison of six organic solvents for the GC ana~sis of pesticides; study emphasized
the stability of selected pesticides in a given solvent 9
Polychlorinated & Polybrominated Compounds
. Review of analytical methods for the determination of brominated flame retardants
(BFRs) with an emphasis on polybrominated diphenyl ethers (PBDEs); sample pre-
treatment, extraction, cleanup, chromatogra~hic separation, detection methods, and
quality control are among the topics discussed 0
. Application of SPME to the analysis of BFRs in water. samples; method uses GC tandem
MS for quantification 81
. Use of two-dimensional gas chromatography (GC x GC) to separate and identify the 209
PCBs 82
. Study of the effects from solvent and temperature to the various extraction methods for
removing PCBs and polychlorinated dibenzodioxins (PCDDs) from fly ash 83
. Method for the determination of polychlorinated dibenzo-p-dioxins (PCDDs),
dibenzofurans (PCDFs), and biphenyls (PCBs) using GC-MS; the use of different reagent
gases is studied 84
14
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Spec~ation
. Application of liquid chromatography (LC) coupled with inductively coupled plasma-
mass spectrometry (ICP-MS) in field of elemental speciation; a few key elements for
speciation (As, Se, Cd) are highlighted 85
. Review of applications and instrumentation for speciation analysis; focus is on ICP-MS
and electrospray ionization mass spectrometry (ESI-MS) 86
. As speciation using classical ion-exchange column chromatography; presents strategies
for separation and pre-concentration of arsenic species 87
. Sb speciation problems and progress; table of Sb speciation from water, soil, and extracts
using high performance liquid chromatography (HPLC) separation 88
. Review; trace metal speciation in environmental studies using sector field inductively
coupled plasma mass spectrometry (ICP-SFMS) and multi collector inductively coupled
plasma mass spectrometry (MC-ICP-MS) 89
. Review of As speciation analysis using HPLC coupled to ICP-MS 90
. Review of developments in GC-plasma interfaces for use in elemental speciation;
advantages and disadvantages of GC-plasma interfaces, t('Pes of plasmas and mass
spectrometers, and variants of plasma sources are discussed 9
. Review of modem sample preparation techniques used in speciation analysis that reduce
waste generation and minimize environmental hazards 92
. Comparison of extraction methods for arsenic speciation analysis; river sediment, sewage
sludge, and agricultural soil reference materials were used in the study; analyses were
completed by high-performance liquid chromatography-hydride generation-atomic
fluorescence spectroscopy 93
Field-Portable Techniques & Instrumentation
. Portable capillary electrophoresis instrument prototype; basic instrument design and three
electrochemical detection methods are discussed 94
. Use of portable X-ray fluorescence (PXRF) instrumentation in analysis of environmental
samples; includes tables comparing PXRF analysis of certified reference materials and
comparing performance of PXRF and laboratory ICP-AES results 95
. Use of SPME for sampling environmental contaminants in air, water, and soil for
analysis by GC-MS in the field 96
. Design test for the next generation of field-portable and low-cost GC-MS; the design
combined a small gas chromatograph with a compact double-focusing mass spectrometer
(CDFMS) as the detector 97
. Comparison of organic vapor analyzers (OV As) with either a flame ionization detector
(FID) or a photoionization detector (PID) to the analysis of soils contaminated with diesel
fuel 98
. Development of a portable laser-induced plasma spectrometer; field results on steel-scrap
samples were compared to laboratory X-ray fluorescence (XRF) results 99
. Report on prototype portable GC for use in the determination of complex vapor mixtures;
analysis was performed on a 30-vapor mixture and performance compared to indoor air
quality monitoring applications 100
. Enhancement of selectivity in field-portable high-speed GC analysis for organic vapors
using a thicker film in the nonpolar column 101
. Development of a battery-operated, miniature, cylindrical ion trap (CIT) mass
spectrometer that maintains laboratory-scale instrument functionality and performance 102
15
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.
Use of a portable in-situ spectrophotometric analysis system for the measurement of
. I 103
copper In coasta waters
Overview of field-portable OC-MS analytical systems and applications to environmental
. 104
and forensic analyses
Development of a fast gas chromato~raph coupled to a time-of-flight mass spectrometer
(OC-TOFMS) for portable field use I 5 °
.
.
Atomic Spectrometry
.
Annual review; atomic spectrometry update on chemical analysis of environmental
samples; extensive table summarizes applications by analyte, matrices (soils, plants,
sediments, etc.), and technique 106
Annual review; new developments in atomic emission (AE), atomic absorption (AA),
atomic fluorescence (AF), and related techniques 107 .
Annual review of novel developments and trends in atomic emission, atomic absorption,
and atomic fluorescence spectrometry 108
Annual review of trends and developments in atomic emission, absorption, and
109
fluorescence spectrometry
Review of advances in atomic emission, absorption, and fluorescence spectrometry and
related techniques 110
Biennial review of atomic spectroscopy developments published from January 2002 to
December 2003; includes AA, AF, AE, ICP-MS, and glow discharge (OD) III
Biennial review of new developments in atomic absorption, atomic fluorescence, atomic
emission, glow discharge atomic spectrometry and inductively coupled plasma-mass
spectrometry from October 1999 to October 2001; primarily new applications and
methodology 112
Review of recent advances in the hydride-generation technique for analysis by atomic
emission spectrometry (AES) 113
.
.
.
.
.
.
.
Atomic Absorption Spectrometry (AAS)
.
Comparison of analytical performance of atom trapping systems and atomization
techniques for flame atomic absorption spectrometry (FAAS) 114
Review; developments and trends in sample pretreatment for electrothermal atomic
absorption spectrometry (ET AAS); coupling of flow injection (FI) for analyte separation
. 115 .
and preconcentrat~on
Procedure for determininf Cu, Ca, and Cr in interferents using pulsed peristaltic pumps
and Fourier transforms II
.
.
Capillary Electrophoresis (CE)
.
Review of applications of capillary electrophoresis for detection and determination of
pesticides in formulations, environmental samples, and for chiral separations; includes
comparison table of detection limits for different detectors 117
Review for determining pesticide residues in environmental matrices; provides overview
of current developments and emerging techniques (CE-MS); includes analyte and sample
preparation methods table and provides comparison of CE to gas chromatography (OC)
and liquid chromatography (LC) pesticide-residue analysis techniques 118
Review; use of CE in the speciation of metal ions; includes table of metal ions and
I. do . 119
ana YSIS con ltIons
.
.
16
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. Developments in sample preparation for capillary electrophoresis including clean-up and
concentration methods 120
. Reviews sensitivity enhancements for CE and ~ives several examples of water sample
analysis for both inorganic and organic analytes 21
Gas Chromatography (GC)
. Biennial review of developments in gas chromatography including published work from
2002 and 2003, primarily; sections are divided into reviews and general interest, column
principles and technology, high-speed and portable GC, and detectors 122
. Biennial review of developments in gas chromatography (articles from 2000 and 2001);
contents include high-speed and portable GC, detectors, column technology, and general
. bl" 123
mtere.st pu IcatlOns
. Review of the use of GC in identification and quantification of environmental pollutants;
pollutant groups covered include volatile organic compounds (VOCs), polycyclic
aromatic hydrocarbons (PAHs), pesticides, and halogenated compounds 124
. Two-dimensional gas chromatography (GC x GC) for separation and identification of
organic compounds in environmental samples 125
. Two-dimensional gas chromatography (GC x GC) and recommended column
combinations for separating polychlorinated biphenyls (PCBs) 82
. Use of two-dimensional GC coupled to time-of-flight mass spectrometry for the
improved analysis of polychlorinated biphenyl (PCB) congeners 126
. Overview of the two-dimensional gas chromatographic technique 127
. Data interpretation for two-dimensional gas chromatographic separations 128
. Use of pressurized liquid extraction (PLE) and two-dimensional gas chromatography as a
broad screening method for P AHs in soil 129
. Overview of fast GC with table of "speeding up" options and the practical aspects related
to the reduction in analysis time 130
. Review; developments in coupled-column GC for the analysis of environmental toxins
such as dioxin, PCBs, and P AHs 131
Gas Chromatography-Atomic Emission Detection (GC-AED)
. Brief overview of GC-AED technique including applications, performance issues, and
extended hyphenation options 132
. Simultaneous determination of polychlorinated organic compounds using GC with micro-
electron capture detector (JL-ECD) and micro-atomic emission detector (JL-AED);
mixtures of organochlorine pesticides and PCBs were analyzed 133
. Analysis of river sediments and sewage sludges by flash pyrolysis coupled with gas
chromatography and atomic emission detection (PyGC-AED); results from comparison
analyses made using flash pyrolysis coupled with gas chromatography and mass
spectrometry (PyGC-MS) are provided; river sediments were collected from rivers
known to be polluted by agricultural and industrial activities and sewage sludges were
taken from industrial and urban wastewater treatment plants and a lagoonal purification
system 134
. Use of GC-AED with a microwave-induced helium plasma for speciation of Hg, Sn, and
Pb compounds; includes large summary of GC-AES methods for determining inorganic
mercury and organomercury species in a variety of sample matrices 135
17
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Gas Chromatography-Inductively Coupled Plasma-Mass Spectrometry (GC-ICP-MS)
. Review article; advances in gas chromatography (GC) coupled with inductively coupled
plasma mass spectrometry (ICP-MS) 136
. Application note about the use of GC-ICP-MS for metal speciation in environmental
samples 137
Gas Chromatography-Mass Spectrometry (GC-MS)
. Simultaneous determination of semi-volatile organic compounds (SVOCs) in air samples
by GC-MS; two combined disk-type filters used as adsorbents for air sampling 138
. Analysis for P AHs and heavy me~als in storm water and sediments using GC-MS 139
. Study combining large-volume injection (LVI) to fast GC-MS in the analysis of 15
organochlorine pesticides (OCPs) in aqueous solutions; all analytes separated in less than
8 minutes 140
. Review of analyses for metalworking fluids (MWFs) and hydraulic fluids (HFs) in oily
wastewater using GC/MS with "soft" ionization and two-dimensional GC techniques 141
High Performance Liquid Chromatography (HPLC), Liquid Chromatography (LC)
. Review of developments in liquid chromatography equipment and instrumentation from
January 2000 through December 2001; topics include instrumentation, columns, detectors
(elemental, o~tical, luminescent, electrochemical, mass spectrometry, and others), and
computation 42
. Glossary of terms used in HPLC 143
. Determination of trimethylamine (TMA) in water samples by LC; the analyte was
derivatized in a precolumn using 9-fluorenylmethyl chloroformate (FMOC) 144
. Analysis for phenols (from river and coke plant water) and herbicides (from soil samples)
by solid-phase extraction (SPE) and HPLC 145
. Review of analysis for non-metals (carbon, sulfur, phosphorus, and halogens) using high
performance liquid chromatography coupled with inductively coupled plasma (HPLC-
ICP) 146
. Precolumn derivatization method for the determination of free amines in real water
samples (wastewater from different sampling sites) by HPLC with fluorescence
detection; the amide intermediate, 9-(2-acridone)oxyethylcarbonylimidazole (AOCD),
formed from the reaction of 9-(2-hydroxyethyl)acridone and N,N' -carbonyldiimidazole,
reacts with free amines in the presence of a base catalyst, 4-(dimethylamino)pyridine 147
. Review of the use of HPLC in metal speciation (As, Se, Pb, Hg, Sn, and Cr); includes
sections on sample handling and different chromatographic modes 148
Ion Chromatography (IC)
. Overview of use of ion chromatography (IC) for the determination of inorganic ions in
drinking water; includes table of regulatory methods and analytes 149
. Basic principles, methods, and applications of ion chromatography 150
. Comparison of IC detection techniques; includes table rating characteristics of each
technique 151
. Approaches to sample pretreatment to overcome analysis problems from difficult
matrices 152
18
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.
Coupling ion chromatography with ICP-AES and ICP-MS; highlights advantages and
applications in sample preconcentration, elimination of interferences, and speciation
analysis 153
Inductively Coupled Plasma-Atomic Emission Spectrometry (lCP-AES), Inductively
Coupled Plasma-Optical Emission Spectrometry (ICP-OES)
. Review on matrix effects during ICP-AES sample analysis; addresses the effects from
easily ionized elements to the plasma and the analytical signal; includes a section on
. h d 154
correctIon met 0 s
. Preconcentration and determination of Cd, Hg, Ag, Ni, Co, Cu and Zn in water and
sediment samples using a chelating resin and ICP-AES 155
. . Determination of total metals with discrimination of chemical forms present in a sea
water matrix; use of solid-~hase extraction for separation and preconcentration prior to
ICP-AES sample analysis I 6
. Method for studying long-term stability in ICP-AES 157
Inductively Coupled Plasma-Mass Spectrometry (ICP-MS)
. Biennial review; developments in ICP-MS from October 2001 to October 2003; topics
include sample introduction, spectroscopic interferences, and isotope ratios 158
. Biennial review; developments in ICP-MS from October 1999 to September 2001;
several tables with selected methods such as chemical vaporization, electrothermal
vaporization (ETV), and speciation are provided 159
. Use of a modified Burgener parallel path nebulizer for vapor ~eneration of noble and
transition metal species through reaction with tetrahydroborate 16
. Comparison of on-line preconcentration columns in sequential injection analysis (SIA)
for the determination of metals in sea water (AI, As, Co, Cu, Mn, Mo, Ni, Pb and V) by
ICP-MS 161
. Trace metal determination (Cr, Mn, Fe, Co, Ni and Cu) in saline water using a flow
injection on-line precipitation system coupled to ICP-MS 162
. Overview of "practical aspects" of environmental analysis (measurement parameters and
analytical parameters) by ICP-MS 163
. Determination of hexavalent chromium in ambient air with analysis using ICP-MS 164
. Analysis for Sn in soil samples using potassium hydroxide fusion followed by continuous
hydride generation coupled to ICP-MS 165
. Overview of the electrothermal vaporization (ETV) technique for ICP-MS 166
Infrared (IR) Spectrometry
. Analytical technique for the simultaneous determination of Sb, As, and Sn in aqueous
samples; coupled flow analysis (FA) hydride generation (HG) and Fourier transform
infrared (FTIR) spectrometry system 167
. Quantitative determination of various alkaline and alkaline earth metals in aqueous
solutions using Mid-FTIR spectroscopy 168
. Quantitative method for the determination of ion concentrations of aqueous polyatomic
anions using attenuated total reflectance (ATR) FTIR spectroscopy 169
19
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Liquid Chromatography-Mass Spectrometry (LC-MS)
. Review of applications of liquid chromatography coupled with mass spectrometry (LC-
MS) using atmospheric pressure ionization in water analysis 170
. Summary of problems using LC-MS for qualitative and quantitative analysis of organic
compounds in water 171
. Determination of trace amounts of specific antibiotics in natural waters and wastewater
using SPE combined with hi9h performance liquid chromatography-ion trap tandem mass
spectrometry (LC-MS-MS) I 2 .
. Method for the determination of halogenated and non-halogenated nonylphenols and
nonylphenol carboxylates using liquid chromatography tandem mass spectrometry in
water and sludge samples from a drinking water treatment plant 173
. Summarizes sources of error in HPLC-MS analyses and suggests solutions 174
. Analysis for emerging environmental contaminants using LC/TOF/MS I75
. Analysis for fluorinated surfactants in spiked sludge samples using LC-MS-MS after
extraction and separation 176 .
Liquid-Phase Microextraction (LPME)
. Developments in liquid-phase microextraction (LPME) based on disposable hollow
fibers; the technique principles, set-up, applications, and trends for the future are
discussed 177
. Use of LPME coupled to GC-MS to analyze for pesticides in soil samples 178
. Developments in liquid-phase microextraction; includes details on some environmental
applications (polycyclic aromatic hydrocarbons, herbicides, pesticides, etc.) 179
. Determination of trihalomethanes (THMs) such as chloroform, dichlorobromomethane,
chlorodibromomethane, and bromoform in drinking water samples (tap water and well
water) using headspace liquid-phase microextraction (HS-LPME) with gas
chromatography-electron capture detection (GC-ECD) 180
Microwave-Assisted Extraction (MAE) & Microwave-Enhanced Chemistry (MEC)
. Overview of microwave-based devices used in solid sample pretreatment; includes both
closed and open, multi-mode and focused-microwave systems 181
. Extraction and determination of selected endocrine disrupting chemicals (EDCs) in river
sediments by microwave-assisted extraction followed by gas chromatography mass
spectrometry (GC-MS) 182
. Study of a microwave digestion technique for the analysis of metals (Ca, Mg, Fe, Mn, Zn,
Cr, Cd, Cu, Pb, and V) in sediments and soils; samples analyzed included standard
reference materials (SRMs) of sewage sludge, marine sediment, urban particulate matter,
and coal carbonization site soil 183
. Review of sample extraction and digestion procedures using focused-microwave
radiation; includes tables of focused-microwave-assisted extractions of organic,
inorganic, and organometallic comfounds and of focused-microwave-assisted digestions
of organic and inorganic samples 18
. Use of focused-microwave (PM) irradiation to improve upon conventional Soxhlet
extraction; includes section on the use of FM-assisted Soxhlet extraction (PMASE) in the
analysis of environmental pollutants (polycyclic aromatic hydrocarbons, alkanes,
herbicides, metals, etc.) 185
20
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.
Review of extraction. and digestion procedures assisted by focused-microwave radiation;
applications presented include inorganic, organic, and organometallic analyses in a
. f 1 184
vanety 0 samp e types
Comparison of microwave-assisted total digestion to aqua regia and nitric acid digestions
for the determination of heavy metal content in environmental samples (sediments, soils,
sludges, and plant materials) 186
Study of three microwave digestions for the determination of metals in sludge, soil, and
sediment samples; metals analysis performed by ICP-AES 187
Determination of 17 chlorophenolic compounds in ash samples obtained from different
incineration plants; a microwave system with closed extraction vessels was used in the
1 . 188
samp e preparatIon
Digestion of organic samples using microwave-assisted sample combustion; cadmium
and copper were determined in the samples using electrothermal atomic absorption
189
spectrometry
Study of the thermal degradation of five carbamates (propoxur, thiuran, propham,
methiocarb, and chlorpropham) in microwave-assisted extraction followed by HPLC
analysis 190
.
.
.
.
.
Mass Spectrometry (MS)
. Annual review of atomic mass spectrometry; review focuses on significant developments
in instrumentation and methodology and an improved understanding of the fundamental
phenomena of MS 191
. Annual review of atomic mass spectrometr~; developments in instrumentation and
methodology or fundamental principles of MS 92
. Annual review of developments in atomic mass spectrometry 193
. Structural and chemical characterization of compounds in complex environmental
mixtures using electrospray ionization Fourier transform ion cyclotron resonance mass
spectrometry (ESI Ff-ICR MS) 194
. Brief comparison of GC-MS and LC-MS 195
. Development of a mass spectrometer with simultaneous detection using a Faraday cup-
based detector called the focal plane camera (FPC) 196
. Direct coupling of SPME with mass spectrometry to make a new analytical technique,
fiber introduction mass spectrometry (FIMS); analysis of VOCs, SVOCs, and two
herbicides using the new technique is discussed 197
Nuclear Magnetic Resonance Spectroscopy (NMR)
.
Use of high performance liquid chromatography coupled with nuclear magnetic
resonance spectroscopy (HPLC-NMR) in environmental analysis as a method of
identifying components of complex mixtures; references work using HPLC-NMR for the
I . f. 1 . 198
ana YSIS 0 enVlfonmenta contammants .
Study of two techniques used for the analysis of perfluorinated surfactants in water
samples-19F NMR and LC-MS-MS; techniques complimented each other for sample
analysis and the methodology is applicable to other sample matrices 199
Use of NMR in hyphenated techniques with HPLC and MS with potential of separating
complex mixtures of pharmaceuticals or drug metabolites 200
.
.
21
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Pressurized Fluid Extraction (PFE), Pressurized Liquid Extraction (PLE), Accelerated
Solvent Extraction (ASE)
. Overview' of the accelerated solvent extraction (ASE) technique for the extraction of
environmental pollutants from solid samples; presents basics of technique and
comparison to other extraction techniques 201
. One-step cleanup and extraction method for the analysis of polycyclic aromatic
hydrocarbons (PAHs) using pressurized liquid extraction (PLE) 202
. Study of efficiency of a pressurized liquid extraction (PLE) system for the isolation of
organic pesticides and polychlorinated biphenyls (PCBs) under varying pressure and
do ° 203
temperature con lhons
. Pressurized liquid extraction of veterinary antibacterial agents from soil samples followed
by SPE and LC-MS analysis 204 .
Solid-Phase Extraction (SPE)
. Reviews use of solid-phase extraction for separation and sensitive determination of metal
ions (primarily in water samples); includes tables of on-line and off-line SPE ~plications
with details on matrix, trace elements, experimental conditions and methods 20
. Innovative development of molecularly imprinted polymers (MIPs) for use in solid-phase
extraction (SPE) to selectively extract analytes from complicated matrices; addresses
analytes of environmental interest 206
. Comparison of extraction techniques-solid-phase extraction (SPE) and solid-phase
microextraction (SPME)-in the analysis for short-chain chlorinated paraffins (SCCPs) in
tap and river water samples using GC coupled to negative chemical ionization mass
spectrometry (GC-NCI-MS) 207
. Sample clean-up and separation by sequential solid-phase extraction (SSPE) for analysis
of polar pollutants in water samples; analyses of samples from wastewater treatment
plants (WWTPs), rivers, and streams were performed using LC-ESI-MS 208
. Comparison of SPE materials for the removal of polar compounds from spiked water
samples; phenolic compounds and organochlorine pesticides were studied 209
Solid-Phase Microextraction (SPME)
. General overview of SPME technique 210
. Comparison of the extraction efficiencies of five different SPME fiber coatings in the
analysis of 52 pesticides and PCBs 211
. Derivatization and SPME of organotin and organolead compounds in aqueous samples
with analysis by gas chromatography atomic emission detection (GC-AED);
derivatization is carried out in situ using sodium tetrapropylborate 212
. Rapid procedure for determining butyltin species in sediments by SPME; analysis was
performed on a certified reference material (CRM-462) and coastal sediment samples 213
. Direct headspace SPME method for the determination of polynuclear aromatic
hydrocarbons (PAHs) in atmospheric particulate matter; results showed potential for
using method as a screening tool 214
. Simple and fast procedure for the analysis of aldehydes in water using SPME technique
with on-fiber derivatization; quality of results were evaluated using spiked bidistilled
water, chlorinated tap water, and well water 215
. Determination of tributyltin (TBT) in water and sediment by automated in-tube SPME
and HPLC coupled to a quadropole mass spectrometer with electrospray ionization 216
22
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.
Use of SPME and GC-MS to characterize odorant emISSIOns from a landfill;
demonstrated use as an on-site analysis tool 217
Comparison of SPME with stir bar sorptive extraction (SBSE) in the extraction of semi-
volatile compounds (polycyclic aromatic hydrocarbons, organochlorines) in water; post-
extraction analysis was performed using GC-MS 218
Analysis for BTEX in water samples using headspace solid-phase microextraction (HS-
SPME) with GC-FID 219
.
.
X-ray Spectrometry (XRS)
.
Review of developments and improvements in X-ray spectrometry published during 2002
and 2003 220
Annual review of X-ray fluorescence (XRF); developments during 2002 and 2003 in
instrumentation and detectors, trends in analysis, and a range of applications including
environmental 221
Annual review of developments in instrumentation and applications of X-ray
fluorescence including environmental applications 222
Annual review; developments during 2000 and 2001 in X-ray fluorescence; contents
include instrumentation and detectors, optics, portable and mobile XRF, and applications
of XRF 223 .
Biennial review of developments in XRS and related fields (from late 1999 to the end of
2001); topics include those of detection, instrumentation and optics, and several
applications 224
On-line preconcentration flow system for the simultaneous determination of Co, Cu, Mn,
Ni, Pb and Zn by total reflection X-ray fluorescence (TXRF) sr:ectrometry;
improvements in detection limits; system was applied to river water samples 25
.
.
.
.
.
23
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SPECIAL TOPIC - ENDOCRINE DISRUPTING COMPOUNDS (EDCS)
Although not a consideration for the environmental crime field at this time, concern over
endocrine disrupting compounds (EDCs-also known as "endocrine disrupting chemicals") in the
environment has been increasing. Endocrine disrupters have been defined as "exogenous agents
that interfere with the production, release, transport, metabolism, binding, action, or elimination
of the natural hormones in the body responsible for the maintenance of homeostasis and the
regulation of developmental processes." 2 6 Research to identify compounds that may interfere
with hormonally-controlled body systems has been increasing for both governmental and private
research entities.
Currently, the USEPA is developing methods for the screening and testing of thousands
of contaminants with the potential to disrupt the endocrine system.227 USEPA, as tasked by the
Federal Food, Drug and Cosmetic Act (FFDCA), developed the Endocrine Disrupter Screening
Program (EDSP) to "screen pesticide chemicals and environmental contaminants for their
T}Q
potential to affect the endocrine systems of humans and wildlife." When complete, the EDSP
will provide validated methods for screening drinking water sources for EDCs.
Several other countries have taken steps to define the EDC problem and pursue solutions.
The United Kingdom Environment Agency has presented a position on phamaceuticals in
watercourses (prioritizing some of these Pharmaceuticals for monitoring) and a strategy paper on
EDCs in the environment. 229> 23° Environment Canada also has a national strategy regarding
endocrine disrupters in the environment. 231
The Australian Government Department of the Environment and Heritage has made
available an EDC information paper wherein parties "agreed on the need to investigate, in depth,
the human, environmental and ecotoxicological aspects of endocrine disrupting substances." 232
Deustche Forschungsgemeinschaft (DFG) has established research training group 546 for the
"elimination of endocrine-disrupting substances from waste water." 233
The Japan Environment Agency has summarized on-line the plans for investigations,
research, testing, and method development for SPEED '98-Strategic Programs on Environmental
Endocrine Disrupters '98. 234 The Danish Environmental Protection Agency has provided on-
line an "Evaluation of Analytical Chemical Methods for the Detection of Estrogens in the
Environment." This document provides environmental and chemical properties of estrogens,
analytical methods and applications to estrogens, and recommendations. The document also
contains active links to tables and numerous references. 235
METHODS FOR THE IDENTIFICATION OF ENDOCRINE DISRUPTORS
Pharmaceutically Active Compounds
(antibiotics, anti-inflammatories, antibacterial agents, etc.)
• Investigates the presence of sulfadimidine (sulfamethazine), an antibiotic used for
animals, in liquid manure and soil samples; surface water samples from river banks were
extracted and analyzed by LC-MS/MS for more than 20 antibiotics used in both animal
and human therapy236
• Review of pharmaceutical antibiotic compounds in soils with an extensive section on fate
studies237
24
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. Analysis for the nonsteroidal anti-inflammatory drugs (NSAIDs) ibuprofen and 2-(4-
chlorophenoxy)-2-methylpropionic acid in wastewater; method used reversed-phase high
performance liquid chromatography (RP-HPLC) combined with a simple, fast, and
inexpensive two-step liquid-liquid-liquid microextraction (LLLME) 238
. Analysis for NSAIDs in water samples using solid phase microextraction (SPME), on-
fiber silylation (derivatization), and GC/MS determination; the SPME method was
compared to the use of solid phase extraction (SPE) for analysis of ibuprofen and
naproxen in the influent and effluent from a sewage water treatment plant 239
. Method for the determination of the fluoroquinolines ciprofloxacin and norfloxacin
(antibacterial agents) in sewage sludge and sludge-treated soil samples; samples were
extracted using accelerated solvent extraction (ASE); extracts were cleaned using SPE
and analyzed by liquid chromatography fluorescence detection (LC-FLD) 240 .
. Extracts from sewage treatment plant wastewater and from surface water were analyzed
for carbamazepine (a drug used in the treatment of epilepsy, schizophrenia, bipolar
disorders and more) and five metabolites of carbamazepine using electro spray LC-
MS/MS with selected reaction monitoring 241
. Determination of clofibric acid using acid and base/neutral liquid-liquid extraction,
derivatization with trimethylsilyldiazomethane (TMSD) and analysis by GC/MS 242
. Analysis for polar pharmaceuticals by LC-MS without derivatization; samples of river
sediment were spiked with standards and prepared by ultrasonicated solvent extraction
and solid phase extraction (SPE) prior to analysis 243
. Simultaneous determination of acidic and neutral pharmaceuticals in wastewater using
high-performance liquid chromatography photochemically induced fluorimetry (HPLC-
PIF) providing a clean, fast and inexpensive on-line post-column photoderivatization
procedure; SPE clean-up was used on the sewage water sample 244
. Analysis for nine neutral pharmaceuticals in river water and wastewater samples (influent
and effluent from municipal sewage treatment plants) by liquid chromato~raphy
electrospray tandem mass spectrometry (LC-ES-MS-MS) with SPE enrichment 24
. Details six different analytical methods that (when totaled) allow for the analysis of
nearly 80 pharmaceutical compounds and phenolic antiseptics 246
. Brief report on proficiency test results for pharmaceuticals in river water and wastewater;
both GC/MS and LC-MS/MS methods were used by participants for the analyses 247
Pharmaceutical and Personal Care Products (PPCPs)
. Study of the removal of selected pharmaceutical and personal care products (PPCPs)
through wastewater treatment processes; includes results from analyses of sewage
treatment works influent and effluent samples and the methodology used in analyzing for
five different groups of PPCPs 248 .
. Method for detection of PPCPs that have a structure conducive to fluorescence using
capillary zone electrophoresis - laser induced fluorescence (CE-LIF); the determination
of salicylic acid in sewage effluent is presented 249
. Review of investigations of musk residues in sewage, sewage sludge, surface water,
aquatic sediment, and biota 250
Steroid Hormones
. Analysis for steroid hormones (gestagens, androgens, and estrogens) in drinking water
and groundwater; samples were extracted (SPE) and derivatized prior to GC/MS analysis
in selected ion monitoring (SIM) mode 251
25
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. Quantitation of estrogens in groundwater samples and swine lagoon samples; extracts
were derivatized with pentafluorobenzyl bromide (PFBBR) and N-trimethyl-
silylimidazole (TMSI) then analyzed using negative ion chemical ionization (NICI) gas
chromatography tandem mass spectrometry (GC-MS-MS) 252
. Analysis for estrogens in surface water and wastewater treatment plant samples; samples
were extracted using SPE, derivatized using PFPA (pentafluoropropionic acid
anhydride), and analyzed by GC/MS 253 .
. SPE-GC-MS method for the analysis of steroids and phenolic compounds in water
samples; changes in the method parameters were made to test the effects on the recovery
of the endocrine disrupting compounds (EDCs); parameters included different types of
SPE cartridges, elution solvent, salt concentration, pH, and humic acid concentration 254
. Analysis of sewage treatment plant influent, effluent and river water for selected
estrogens, phytoestrogens, mycoestrogens and alkylphenols by LC-MS-MS; optimization
of instrument conditions for the EDC groups is detailed including results from
electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI)
'modes, negative ion (NI) and positive ion (PI) modes, and, mobile phase compositions 255
. Determination of chlorinated and brominated derivatives of alkyl phenol ethoxylate
(APEO) surfactants (industrial cleaning agents that mimic endogenous hormones) in
sludges, waters and sediments; extracts from samples were analyzed using reversed phase
LC/MS with a comparison of APCI and ESI interfaces 256
. Analysis for steroid hormones in wastewater treatment plant (WWTP) effluent using
liquid chromatography tandem mass spectrometry (LC-MS-MS); samples were extracted
by SPE and cleaned with a liquid-liquid separation followed by a Florisil cartridge 257
. Presents several methodologies for separation and analysis of steroid estrogens in sludge,
sediment, sewage effluent and surface water; details on the methods are summarized in a
flowchart and table; biological methods for determining the endocrine-disrupting activity
, of a chemical are also discussed 258
General EDC Analytical Methods
. Analysis of samples from 139 streams for pharmaceuticals, hormones, and other organic
wastewater contaminants using targeted methods and selected ion monitoring (SIM) for
improved sensitivity 259
. Use of a liquid chromatography tandem mass spectrometry (LC-MS/MS) method for
analysis of pharmaceuticals, steroids, and personal care products; method used one solid-
phase extraction (SPE) procedure and ESI (in positive and negative modes) and APCI (in
positive mode) 260
. Comparison of separatory funnel liquid-liquid extraction to on-line continuous liquid-
liquid extraction in the analysis of several EDCs in water samples; data was collected in
both total ion chromatogram (TIC) mode and selective ion monitoring (SIM) mode of
GC/MS 261
. Evaluation of matrix effects on 35 endocrine disrupting chemicals for the analysis of
environmental water samples by LC-ESI-MS/MS; efficient sample clean-up and the use
of internal standards showed reduced matrix effects regardless of the type of
environmental water sample (surface water, rain water, groundwater, channel water,
wastewater treatment plant effluents and industrial effluents) 262
26
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Appendix A
MAJOR ENVIRONMENTAL LA WS OF THE UNITED STA TES
ENVIRONMENTAL PROTECTION AGENCY (USEPA)
Environmental Law Summary
Federal Food, Drug, and Cosmetic Set safety and quality requirements for food, cosmetics, drugs and
Act (FFDCA) therapeutic devices. Allows EP A to establish safe tolerance levels for
pesticide chemical residues present in raw or processed foods. 263
Federal Insecticide, Fungicide, and Provided federal control of pesticide distribution, sale, and use. EP A was
Rodenticide Act (FIFRA) given authority to study the results of £esticide use and to require users to
register when purchasing pesticides. 2 4,265
Federal Water Pollution Control Act Established the basic structure for regulating discharges of pollutants into
a.k.a. Clean Water Act (CW A) the waters of the United States and set water quality standards for all
contaminants in surface waters. Gave EPA the authority to implement
pollution control programs. 266,267
Clean Air Act (CAA) The comprehensive federal law that regulates air emissions from area,
stationary, and mobile sources. EPA was authorized to establish National
Ambient Air Quality Standards to protect public health and the
environment. 268.269
National Environmental Policy Act Early environmental law that established a broad national framework for
(NEP A) protecting our environment by requiring that all branches of government
consider the environmental impact prior to undertaking any major federal
action that might significantly affect the environment. Environmental
Assessments and Environmental Impact Statements are required when
airports, buildings, military complexes, highways, park land purchases, and
other federal activities are proposed. 270,271
Safe Drinking Water Act (SDW A) Established to protect the quality of drinking water and focused on all
waters actually or potentially designed for drinking use (above ground or
underground sources). 272
Toxic Substances Control Act Gave EP A the ability to track the 75,000 industrial chemicals currently
(TSCA) produced or imported into the United States. EPA repeatedly screens these
chemicals, can require reporting or testing of potentially hazardous
chemicals and can ban the manufacture and import of chemicals that pose
an umeasonable risk. Mechanisms also exist to track newly developed
h . I . h k d h" 273-275
C emlca s Wit un nown or angerous c aractenstlcs.
Resource Conservation and RCRA (pronounced "RICK-rah") gave EPA the authority to control
Recovery Act (RCRA) hazardous waste from the "cradle-to-grave" and included the generation,
transportation, treatment, storage, and disposal of hazardous waste. The
tracking of hazardous waste through this act only involves active and future
facilities. A framework for the management of non-hazardous wastes was
also established with this act. 276,277
Comprehensive Environmental CERCLA (pronounced "SIR-cia") created a tax on chemical and petroleum
Response, Compensation, and industries and provided broad Federal authority to respond directly to
Liability Act (CERCLA or releases or threatened releases of hazardous substances to the environment.
Superfund) The tax went to a trust fund, the "Superfund," for paying the costs of
cleaning up abandoned or uncontrolled hazardous waste sites as well as
accidents, spills and emergency releases of pollutants. Through CERCLA,
EP A was authorized to identify parties responsible for any type of release
and enjoin their participation in the cleanup or recover costs involved in the
cleanup. 278-280
27
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Environmental Law Summary
Superfund Amendments and Amended CERCLA to increase State involvement, increase the size of the
Reauthorization Act (SARA) trust fund, increase focus on human health problems and revise the Hazard
Ranking System to accurately assess the relative degree of risk to human
health and the environment from uncontrolled hazardous waste sites. 280-282
Emergency Planning and As part of SARA, EPCRA was enacted to help local communities protect
Community Right-To-Know Act public health, safety, and the environment from chemical hazards. Each
(EPCRA) state was required to appoint a State Emergency Response Commission,
divide the states into Emergency Planning Districts and name a Local
Emergency Planning Committee for each district. 283,284
Pollution Prevention Act (PPA) Focused industry, government, and public attention on reducing pollution
through cost-effective changes in production, operation, and raw materials
use. Efforts to reduce pollution prior to the need for treatment or disposal
are referred to as "source reduction." Pollution prevention also includes
conservation and practices that increase efficiency in the use of energy,
water, or other natural resources. 285,286
Oil Pollution Act (OP A) Required oil storage facilities and vessels to submit plans detailing how
they will respond to large discharges, established a tax on oil to finance a
trust fund for spill cleanup costs, and required the development of
contingency plans for oil spill response. EP A published regulations dealing
with above ground oil storage facilities. 287,288
Endangered Species Act (ESA) Provided a program for the conservation of threatened and endangered
plants and animals and their habitats. EP A approval to register a pesticide
is based in part on the risk of adverse effects on endangered species and
habitats. Under FIFRA, EP A can issue emergency suspensions of certain
pesticides (cancel or restrict the use) if an endangered species will be
adversely affected. 289,290
28
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Appendix B
USGS NATIONAL WATER QUALITY LABORATORY METHODS OF ANALYSIS
Water-Resources Investigations (WRI)
Report Number
2003-4293
2003-4174
2003-4139
2003-4079
2002-4222
2002-4144
2002-4071
2001-4186
2001-4134
2001-4132
2001-4098
Title
Determination of Organochlorine Pesticides and Polychlorinated
Biphenyls in Bottom and Suspended Sediment by Gas
Chromatography with Electron-Capture Detection 291
Evaluation of Alkaline Persulfate Digestion as an Alternative to
Kjeldahl Digestion for Determination of Total and Dissolved Nitrogen
and Phosphorus in Water 292
Determination of Organophosphate Pesticides in Whole Water by
Continuous Liquid-Liquid Extraction and Capillary-Column Gas
Chromatography with Flame Photometric Detection 293
Determination of Gasoline Oxygenates, Selected Degradates, and
BTEX in Water by Heated Purge and Trap/Gas Chromatography/Mass
Spectrometry 294
Determination of Organophosphate Pesticides in Bottom Sediment by
Gas Chromatography with Flame Photometric Detection 295
Arsenic Speciation in Natural-Water Samples Using Laboratory and
Field Methods 2%
Determination of Organophosphate Pesticides in Filtered Water by Gas
Chromatography with Flame Photometric Detection 297
Determination of Wastewater Compounds by Polystyrene-
Divinylbenzene Solid-Phase Extraction and Capillary-Column Gas
1QQ
Chromatography/Mass Spectrometry
Determination of Pesticides in Water by Graphitized Carbon-Based
Solid-Phase Extraction and High-Performance Liquid
Chromatography/Mass Spectrometry 2"
Determination of Organic Plus Inorganic Mercury in Filtered and
Unfiltered Natural Water with Cold Vapor-Atomic Fluorescence
Spectrometry 30°
Determination of Moderate-Use Pesticides and Selected Degradates in
Water by C-18 Solid-Phase Extraction and Gas Chromatography/Mass
Spectrometry 301
Methods can be purchased from the USGS through the "Publications Warehouse" on the USGS website.
302
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3.
4.
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6.
7.
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Prevention. Available at: http://www4.law.comell.edu/uscode/42/ch133.html. Accessed
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47
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LOCAL RESTORATION EFFORTS
By 1990, when the United States Army Corps of Engineers re-
leased its findings on the degradation of the Anacostia River
(summarized in the text on the cover), the process of restoring
the watershed was already under way. The Anacostia Water-
shed Restoration Committee was formed in 1987 under the au-
thority of the Anacostia Watershed Restoration Agreement
signed by the District of Columbia, Montgomery County,
Princes George's County, the State of Maryland, and the U.S.
Army Corps of Engineers. In 1991, the Committee adopted a
plan entitled A Commitment to Restore Our Home River: A Six
Point Action Plan to Restore the Anacostia River. That restoration
initiative established six scientifically based goals for restoring
and protecting the Anacostia River watershed. It emphasized
the need for interagency and intercommunity cooperation in
achieving the goals.
Since 1991, the Anacostia River watershed has experienced
certain improvements in water quality and its ability to sustain
critical habitat and aquatic life. More importantly, there has been
a groundswell of environmental, public and civic group activism
to clean-up the River and protect the watershed from further
degradation. The Anacostia is no longer the "forgotten River./I It
is clearly undergoing a rebirth with local groups leading the way.
FEDERAL INVOLVEMENT
Small waterways like the Anacostia River do not often com-
mand the direct or targeted attention of Federal environmental
protection programs. Their welfare is left to local initiatives, ex-
emplified by the work of the Anacostia Watershed Restoration
Committee and the public-interest groups, private citizens, and
local officials that have supported it. These special problem
areas often escape Federal attention when the impacted com-
munities do not muster sufficient political clout. The combined
influence of those two factors is demonstrated by the disparate
attention paid at the Federal level to pollution of Washington's
two main waterways prior to 1990. The millions of dollars spent
on restoring and protecting the large, high-profile Potomac
River and the successes achieved there stand in sharp contrast
to the modest Federal resources applied to cleaning up the
Anacostia River.
Eventually, the extent of the Anacostia's plight and the con-
sequences of neglect. to the capital city's image, to the water
quality of the Potomac River and the Chesapeake Bay, and to
the quality of life in the communities that line the river's
banks-were spotlighted in a Report to Congress prepared by
the U.S. Environmental Protection Agency in 1992. Based on
the recommendations in that document, the Anacostia water-
shed was designated by the President of the United States as
one of seven ecosystems in the nation requiring priority restora-
tive attention. Recommendations from this White House
Ecosystem Management Task Force included a stronger and
more coordinated Federal role in the restoration. EPA began to
work in earnest with the Army Corps of Engineers and others to
bring the full benefit of Federal involvement to the Anacostia
watershed restoration.
In July 1994, the Agreement of Federal Agencies on Eco-
system Management in the Chesapeake Bay (developed by the
Chesapeake Bay Program of the U.S. Environmental Protection
Agency, Region III) was signed by 23 Federal agencies and de-
partments. A line item in that document pledged the signers'
full support of a Federal workplan to clean up the Anacostia in
cooperation with the Anacostia Watershed Restoration
Committee. That item reflected the fact that the Anacostia River
is linked to the Chesapeake Bay via its outflow into the Potomac
River, which in turn flows into the Bay.
Three months later, in September 1994, the Environ-
mental Protection Agency, Region III, introduced its
Anacostia Ecosystem Initiative. This was the culmination
of some three years of work from the time the Agency
first espoused the restoration of the Anacostia River wa-
tershed in the early 1990s. The Initiative would allow the
Agency to sign on as a full partner in ~he local restoration
effort.
ANACOSTIA ECo..~l
u.s. Environmental Protectior
JI~ eginning with the Special Report to Congress
in 1992, prepared by the Chesapeake Bay
o ~~~~:~t~~ :~a~:g;~~~ ;~~~~~~se%;:~~~;
to the effort to strengthen the Federal presence in
restoration activities. Federal participation allows for the
establishment of an Urban Watershed Model that can be
used in other urban areas throughout the country.
In September 1994, the EPA Region III announced the
Anacostia Ecosystem Initiative. The four main features of
the Initiative are: watershed restoration; multi-media risk
reduction; environmental justice; and public education
and involvement.
Activities under the Initiative can be broken down as
follows:
. To identify and target compliance and enforcement
activities at Federal facilities in the watershed.
. To assist in coordinating restoration activities at
Federal facilities in the watershed.
. To seek greater controls over combined sewer and
storm water discharges.
. To ensure equal protection from environmental haz-
ards of the watershed community regardless of race,
ethnicity, or economic status.
. To provide a full-time liaison to the Anacostia com-
munity to seek out and report local concerns and
interests.
GOALS OF THE INITIATIVE
Watershed restoration
Multi-media risk reduction
Environmental justice
Public education/involvement
-------
INITIATIVE
~M
~gency, Region III
. PROGRESS TO DATE
. .
COMMUNITY LIAISON APPOINTED
In May 1995, EP A Region III hired a community liaison for the
Anacostia River restoration project. The liaison has established a base at
the Kramer Middle School in Anacostia, and divides time between that
location and home base at EPA Region Ill's Chesapeake Bay Program of-
Ifice in Annapolis. The liaison has regular contact with citizens, community
leaders, and interest groups to maintain a two-way flow of information and
ideas associated with the day-to-day and long-term aspects of the restoration
project. The liaison also assists in delivering environmental science educa-
tion to the District of Columbia's school children.
EPA REGION III BECOMES A FORMAL PARTNER
In May 1996, the relationship between EPA Region III and the local groups
working on the Anacostia River's restoration was formalized in a
Memorandum of Understanding signed by the Region III Administrator of the
~nvironmental Protection Agency and the Chairman of the Anacostia
"shed Restoration Committee. The two parties to the Agreement
pledged to cooperate in continuing the restoration of the Anacostia River
and in providing diligent outreach and environmental services to the river's
bordering communities. As a result of the agreement, EP A Region III
became a non-voting member of the Anacostia Watershed Restoration
Committee.
KEY STRATEGIES FORMALIZED
Two achievements in 1996 stemmed directly from the 1994 Agreement of
Federal Agencies all Ecosystem Management in the Chesapeake Bay.
Key strategies were developed with considerable Federal leadership and
participation:
. Special Tributary Strategy for Federal Lands in the District of Columbia.
. Biennial Federal Workplan for the Anacostia River Watershed
In addition, a third strategy was completed in October 1996 with extensive
public participation:
. Regional Action Plan for Toxics
'~~'~~i~...........-..- ....
. f '~,..-~~~,
.
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"'.
Special Tributary Strategy for Federal Lands: On March 25, 1996, the
Special Tributal}' Strategy for Federal Lands in the District of Columbia was
signed by 18 high-level Federal officials at the U.S. National Arboretum on
the banks of the Anacostia River. The voluntary agreement calls for im-
proved control of stormwater runoff on all Federal lands in the District of
Columbia. It also supplements the District's strategy to meet the 40% nutri-
ent reduction goal of the Chesapeake Bay Program.
Biennial Federal Workplan: On November 22, 1996, a draft Biennial
Federal Workplan for the Anacostia River Watershed was introduced by EPA
Region Ill's Chesapeake Bay Program and the U.S. Army Corps of
Engineers (Baltimore District) in cooperation with the Anacostia
Watershed Restoration Committee.
The workplan translates the goals of the Anacostia Watershed Res-
toration Committee's Six-Point Action Plan into specific actions to be under-
taken by Federal agencies and facilities that impact water quality in the
Anacostia and watershed. The workplan emphasizes that the Federal agen-
cies cannot singlehandedly restore and protect the Anacostia River water-
shed. Success will depend on the continuation of efforts by state and local
agencies, private landholders,
and citizens organizations.
The primary purpose of the
workplan is to provide guidance
necessary to ensure that Federal
actions are:
. Coordinated and collabo-
rative in their approach;
. Compatible with and sup-
portive of actions of other
Federal and non-Federal
participating groups;
. Designed to address ef-
fectively the restoration
priorities defined in the
Six-Point Action Plan and others that may subsequently arise;
. Able to be routinely tracked and documented in terms of cost and
progress.
Success will depend on
the continuation of efforts
by state and local agencies,
private landholders, and
citizens' groups.
Regional Action Plan for Toxics: In October 1996. the District of
Columbia completed a Regional Action Plan for Toxics. The plan defines a se-
ries of steps that organizations may take to minimize toxic loading into the
Anacostia River and to rectify past damage to the river. The plan incorpo-
rates inputs from local citizens and interest groups that were obtained during
interviews and public forums. The work was supported by grants from the
Chesapeake Bay Program.
INSPECTIONS CONDUCTED AT FEDERAL FACILITIES
~
In 1995, EP A Region III conducted multi-media inspections to determine
compliance under various environmental statutes at the Washington Navy
Yard. the Southeast Federal Center, and the Bureau of Engraving and
Printing. Subsequently. there were high-level meetings with Navy personnel
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to address the outstanding compliance issues at the facility. Section 7003
of the Resource Conservation and Recovery Act was used as the basis
for an Order addressing hazardous-waste contamination of soil, ground
water, and surface water. In June 1996, the Navy agreed to contract for
immediate clean up of contaminated sediments in three outfall locations
and to perform additional clean up in 1997.
Follow up of compliance issues involving the Southeast Federal
Center continues. A special Federal appropriation of $15 million was
directed to environmental remediation at this location.
Two other Notices of Violation under the Resource Conservation
and Recovery Act were issued to the Navy in June 1996 and are pending
resolution. They concern violations at the Washington Navy Yard and
the Anacostia Naval Station.
Assessments conducted at the Washington Navy Yard site indicate
that the contamination there in the presence of a subsistence fishery and
other sensitive environments would qualify the site for inclusion on the
Superfund National Priorities List. In July 1996, EPA Region III
requested District of Columbia concurrence with the listing and
subsequently received it in October 1996. Meanwhile, progress toward
clean up continues under the Resource Conservation and Recovery Act
action.
The Bureau of Engraving and Printing is presently in compliance.
CONTROL Of
COMBiNED SEWER OVERFLOW IMPROVED
A new operating permit for the Blue Plains sewage-treatment plant is
now strengthening the monitoring, public notification, and control of
combined sewer overflows in the District of Columbia. The new permit
was issued by the Environmental Protection Agency in January 1997, fol-
lowing certification by the District of Columbia. It incorporates controls
on combined sewer overflow and nutrients in the Anacostia that are in
line with national policy. The permit also defines Biological Nitrogen
Removal pilot plant requirements that will further reduce nutrient pol-
lution in the Potomac River basin and, consequently, in the Anacostia
River, since the basin is a tidal system.
FINANCIAL SUPPORT TO COMMUNITY PROJECTS
Since the start of its Anacostia Ecosystem lnitiativein 1994, EP A Region III
has channeled over $1 million to
projects designed to generate
community involvement and
awareness in the issues associ-
ated with the Anacostia's pollu-
tion and restoration. Examples
include support for the Toxics
Action Plan and Biennial Federal
Workplan described previously.
Further examples include fish
advisory signs along the river,
educational canoe trips for
school children, science fairs and
festivals, comparative risk stud-
ies on overall health risks, and
environmental justice projects.
In addition to those individ-
ual, relatively small grants, EP A
Region III, through its
Chesapeake Bay Program and Non-Point Source Program, has chan-
neled more than $2.5 million to the District of Columbia and Maryland
for environmental protection work.
DISTRICT OF COLUMBIA
FISHING NOTICE
REGULACIONES PARA LA PESCA
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How to find out more about the
ANACOSTIA ECOSYSTEM INITIATIVE
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The staff of the U.S. Environmental Protection
Agency, Region III, will be happy to respond to
questions and comments about the Anacostia
Ecosystem Initiative-the restoration project itself
and related community involvement. Below is a list
of contacts and their areas of expertise.
REGION III CONTACTS
Jon M. Capacasa, Anacostia Ecosystem Initiative Manager
(215) 566-5422
Eric Ashton, Federal Facilities Coordinator
(215) 566-2713
Bill Arguto, Remedial Project Manager/Superfund
(215) 566-3367
Jim McCreary, Hazardous Waste Sites Study
(215) 566-3243
Claudette Reed, Enforcement Coordination/Compliance Snapshot
(215) 566-2997
Elaine Harbold, Blue Plains Permit/CSOs
(215) 566-5744
Reginald Harris, Environmental Justice
(215) 566-2988
Written correspondence to these individuals should be addressed to:
U.S. Environmental Protection Agency, Region III
841 Chestnut Building
Philadelphia, PA 19107
LOCAL AREA CONTACT
Bev Baker, Community Liaison
U.S. Environmental Protection Agency
Chesapeake Bay Program
410 Severn Avenue, Suite 109
Annapolis, MD 21403
1800 YOUR BAY, ext. 772
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1 :.,:O..t.ji)"'n'(l'" 'I .' '
1 ",. t:' . . 1<';'/ i8 ,L\.venue NW
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Visit the Initiative's web site at
http://www. epa. gov/ch esa peake/ anacostia/
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I'. n November 1996, EPA Region III issued an updated workplan
. ,.. for the Anacostia Ecosystem Initiative. The overall goal to restore
; the Anacostia River and its watershed remains the same, with
planning for the following objectives:
o To target U.S. Environmental Protection Agency programs to
the benefit of the project.
o To minimize pollution from combined-sewer-overflows.
o To provide public outreach and education.
o To assist and coordinate restoration activities at Federal instal-
lations in the watershed.
o To pursue reduction of environmental risk to the public from
air, soil, and water contamination.
lfARGH~NG IENVIRONMENTAl
PROUCnON AGENCY PROGRAMS
The Anacostia Working Group within EPA Region IH will continue
to coordinate activities across all programs and divisions. The Group
will identify issues that EP A Region HI can help to resolve and op-
portunities for channeling resources for the benefit of the Anacostia
watershed restoration.
The comprehensive assessment of historical hazardous waste sites,
begun in July 1996, will continue aggressively, resulting in targeted in-
vestigations of dozens of sites that have attracted the concern of the
citizens of the Anacostia community and the Environmental
Protection Agency. Periodic status reports will be delivered to the
community by meetings and facts sheets. Brownfields will be assessed
for their redevelopment potential and clean-up or stabilization needs.
In March 1997, EPA Region III will launch the "Compliance
Snapshot" report for the Anacostia. This public report will tally the
facility-by-facility status of compliance with various environmental
laws. By making this readily accessible to the public, EP A is providing
an additional Right to Know database.
In cooperation with leaders and river restoration personnel in the
Anacostia community, EP A Region IU will continue its development
of environmental indicators and measures of progress that was initi-
ated under this Anacostia Ecosystem Initiative.
The feasibility of addressing sediment remediation in the
Anacostia River as part of the process of nominating deserving sites
for inclusion in the Superfund National Priorities List will be investi-
gated. Prior compliance/enforcement proceedings will be followed up
and targets for new pollution inspections will be sought as resources
allow.
Enforcement lawyers and managers will be provided ready access
to a current Supplemental Environmental Projects lists of Anacostia
River projects for use in their settlement negotiations. .
The automotive service and repair facilities will be assisted and
pollution-prevention workshops will be conducted in the District of
Columbia to reduce toxics and oil pollution in the Anacostia River.
Specifically, the sources of oil/grease pollution to Hickey Run will be
investigated by sewer tracing in conjunction with the Metropolitan
Washington Council of Governments and the District of Columbia.
Compliance/enforcement procedures will be initiated as warranted.
COMBINED-SEWER-OVERFLOW CONTROL
EP A will closely monitor newly issued discharge permits for the
watershed. Monitoring of combined-sewer-overflow loads into the
Anacostia River will be enhanced and information on the discharges
will be disseminated to foster scientific study in the area. Technical-
exchange meetings among the several interested agencies and groups
will be convened to review long-term control strategies. Funding,
monitoring, and other issues pertinent to long-term resolution of the
problem will be explored with all the interested parties.
COMMUNITY OUTREACH AND !EDUCATION
EPA Region HI will continue to fund and support the liaison for the
communities that border the Anacostia River. The community liaison
will continue to establish regular contact with citizens, community
leaders, and interest groups to maintain a two-way flow of informa-
tion and ideas associated with the day-to-day and long-term aspects
of the Anacostia River restoration project. Special emphasis will be
placed on bringing the story and the science of the Anacostia River
restoration project to the school children of the area.
At least two major public meetings/forums per year will be con-
ducted in the Anacostia community, and program and project man-
agers will be encouraged to conduct similar outreach sessions. The
meetings will be oriented toward enhancing feedback to EP A Region
III concerning its programs and to building consensus on the assign-
ment of priorities to the community's perceived needs.
Fact sheets, newsletters, news releases, etc, will be issued and the
Internet site will be used to deliver current news and information to
the public about the Anacostia River restoration project and the cur-
rent condition of the river.
Staff members will dedicate time to supporting the Science in
Education program in the District of Columbia's schools and launch~
ing an environmental science curriculum at Kramer Middle School i~
Anacostia.
COOPERATiON fROM fEDERAL INSTALLATiONS
EPA Region HI will assist in the finalization of the Biennial Federal
Workplan for the Anacostia River Watershed in April 1997, to ensure
that it will serve effectively as a needs and assessment master plan for
environmental restoration work at Federal installations in the
Anacostia watershed.
RISK REDUCTION FOR THE COMMUNITY
The District of Columbia Environmental Characterization RepOlt will
be distributed to interested parties and the public by April 1997,
following completion of peer review and local-community review.
The report will be used as a benchmark for future risk assessment in
the District of Columbia.
A working session attended by representatives of EP A Region III,
the U.S. Army Corps of Engineers, and the Metropolitan Washington
Council of Governments is scheduled for early 1997 to discuss imple-
mentation of the Regional Action Plan for Toxics, which was com-
pleted in October 1996. EPA Region HI will press for the document
to be expanded by a "Phase Two" effort that would provide a parallel
plan for the Maryland portion of the watershed. Inclusion of that in-
formation would make the document a truly comprehensive action
plan for the entire Anacostia watershed.
EPA will continue to explore, along with the various partners
under this Initiative, various means to officially designate the
Anacostia as a National Urban Watershed Restoration Model in leg-
islation and policy directives. This will promote the exchange of suc-
cessful techniques and lessons learned with other urban river
restoration efforts across the United States.
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