NETI-WEST
BASIC INSPECTOR
TRAINING COURSE
STUDENT MANUAL
May 2001
U.S. Environmental Protection Agency
Office of Enforcement and Compliance Assurance
Office of Criminal Enforcement, Forensics, and Training
National Enforcement Training Institute
Lakewood, Colorado
1 ifNETI
NATIONAL ENFORCEMENT TRAINING INSTITUTE-West
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COURSE EVALUATION
Basic Inspector Training Course
National Enforcement Training Institute
ORGANIZATION: NAME (Optional):
Years of Experience as an Inspector:
Job Title:
Course Date(s):
Please take a few minutes to assist us in evaluating this training program. Please comment and make
recommendations for improvements in future courses.
1. I FEEL THE OVERALL PROGRAM WAS:
VERY WORTHWHILE WORTHWHILE OF SOME VALUE OF LITTLE
VALUE
COMMENTS:
2. ORGANIZATION OF PROGRAM AND MATERIAL WAS:
EXCELLENT SATISFACTORY INADEQUATE
COMMENTS:
3. PRESENTATION AND MATERIAL:
WERE APPROPRIATE EXCEEDED NEEDS OF THE CLASS WERE INSUFFICIENT FOR CLASS
NEEDS
COMMENTS:
MARCH 2000
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4.
HOW WELL DID THIS COURSE MEET YOUR PURPOSE:
EXCELLENT TOO BASIC TOO TECHNICAL
COMMENTS:
SATISFACTORY
5. WHICH PRESENTATION^) DID YOU THINK WERE MOST BENEFICIAL AND WHY?
6. WHICH PRESENTATION^), IF ANY, DO YOU THINK SHOULD BE REMOVED FROM THE
COURSE AND WHY?
7. WHAT CHANGES, IF ANY, DO YOU THINK WOULD IMPROVE THIS TRAINING COURSE?
8. ADDITIONAL COMMENTS ON COURSE, SPEAKERS, FACILITY, OR OTHER ASPECTS OF THE
COURSE
MARCH 2000
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Introduction/Purpose of Course
Introduction to Environmental Compliance
3
Summary of Environmental Statutes
4
Inspector Issues
5
Inspection Planning
6
Administrative Procedures
7
Sources of Information
8
Entry, Opening Conference and Site Inspection
9
Evidence
10
Interviewing
11
Records Review
12
Sampling Issues
13
Closing Conference
14
Inspection Report
15
Enforcement Process Responsibilities
16
Mock Trial
17
Agency/Regional Initiative
mnm
Introduction to Criminal Investigations
Wrap-Up and Evaluation
19
20
APPENDIX: Manual - Conducting Environmental
21
Compliance Inspections (K.I.S.S.)
22
23
24
25
26
27
28
29
30
31
>AVERY"
READY INDEX5 INDEXING SYSTEM
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1
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SESSION 1
TOPIC: INTRODUCTION AND PURPOSE OF COURSE
Time: IS minutes
Purpose
Key Points
• Provide course overview and logistics.
• Explain why course was developed.
• Conduct introductions and get-acquainted discussion.
• Identify inspection-related problems inspectors have encountered and
relate them to course content
• Inspectors play a crucial role in ensuring that the nation's environmental
laws are implemented.
• The inspector's job is complex, requiring legal, technical, and
communication skills.
List of Visuals
List of Handouts
1-1
Welcome (Title Slide)
1-2
Administrative
1-3
Introduction
1-4
Introduction/Purpose of die Course
1-5
Why this Course?
1-6
Basic Inspector Training Course
1-7
Basic Inspector Training Course
1-8
Basic Inspector Training Course
1-9-1-12
Summary of Course Schedule
1-13
Introductions
1-14
Inspector Profile
None
MARCH 2000
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Welcome
The National Enforcement Training Institute
Presents
The Basic Inspector Training Course
Administrative
¦ Facilities
¦ Schedule/breaks
• Telephones
¦ Messages
• 1 imf|i
Introduction
¦ Materials
o Student mutual
• Reference manual
o Evaluation fonn
o K]SS manual
« CD-ROM/law*
¦ Questions
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Introduction/Purpose
of the Course
Why This Course?
• Inspectors play a crucial role in ensuring
that the nation's environmental laws are
implemented
• Inspector's work is very complex, involving:
¦ Legal aipem
a Technical apecis
¦ fViniiimi'
• Course to provide foundation
Basic Inspector Training Course
¦ Course required for EPA by EPA order
¦ Strongly recommended for non-EPA
• Developed by EPA in 1988
• Revised by EPA senior inspectors and state
senior inspectors in 1996
• Principals and policies applicable u> all
• Targeted for new inspectors
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Basic Inspector Training Course
* Fulfills requirements for Basic Training in
» Legal
b Technical
° Admmistruive
¦ Must also take Health and Safety
V9
Basic Inspector Training Course
• Instructors, senior inspectors and experts from
Headquarters and Nfc l I
"¦ Maybe some redundancy -all phases are --
interrelated
• Does not focus on any one program or set of
regs - provides fundamentals for all programs
Summary of Course Schedule
¦ Day 1
c Registration
" Introduction/Purpose of the Course
• Introduce oc to Envinmmentil Compliance
o Summary of Environmental Statutes
o lnrp***irf Ifntrff
o pimnmg
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Summary of Course Schedule
Day 2
• Admmiflnnve issues
° Sources of Information
' Entry, Opening Conferenoe & Site Tour, end
Inspection Techniques
¦ Evidence
s Interviewing
° On-S ile Records Review
Summary of Course Schedule
• Day 3
° Sampling Issues
a Closing Conference
' Inspection Report
o Enforcement Process Responsibilities
0 Mode triil
¦ Agency/Regional Issues
Summary of Course Schedule
¦ Day 4
e Inrryvfrimni tn Primmd
° Wrap-Up and Evaluation
4
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Introductions
• Ask questions
¦ Participate
¦ Provide instructors with benefit of your
experience
H)
Inspector Profile
Mt
5
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2
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SESSION 2
TOPIC: INTRODUCTION TO ENVIRONMENTAL COMPLIANCE
Time: 90 minutes
Purpose
•
Provide the context for the work of inspectors.
•
Explain the role of inspectors in each aspect of an enforcement case.
•
Provide an overview of civil litigation
•
Provide an overview of Federal, State, and Tribal relations.
•
Provide an introduction to pollution prevention and waste minimization
•
Introduce inspectors to criminal enforcement and explain how to
recognize potential criminal violations.
Key Points
•
Knowledge of program compliance and enforcement strategies aids
inspectors in making appropriate field decisions.
•
Inspectors are involved in every aspect of an enforcement case.
•
Inspectors should recognize potential criminal violations and refer them
for investigation.
Federal, State, and Tribal relations are important factors in
environmental compliance.
•
Pollution prevention and waste minimization programs and efforts
impact environmental compliance
2-1
Introduction to Environmental Compliance (Title Slide)
List of Visuals
2-2
Overview of Enforcement
2-3
Compliance and Enforcement Program
2-4
Laws and Regulations
2-5
Compliance and Enforcement Strategies
2-6
Compliance Monitoring
2-7
Enforcement Response
2-8
Fol low-Up to Enforcement Actions
2-9
Steps in an Enforcement Action
2-10
What Can We Get From an Enforcement Action?
2-11
Types of Legal Cases
2-12
Principal Elements of Civil Litigation
2-13
Stages of Civil Litigation
2-14
Complaint
2-15
Complaint
2-16
Complaint
2-17
Complaint
2-18
Discovery Motion
2-19
Motion in Limine
2-20
Principal Differences Between Civil and Criminal Enforcement
i MARCH 2000
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2-21 "Red Flags" That Indicate Possible Criminal Activity
2-22 Relationships Between Federal, State, and Tribal Authorities
2-23 Enforcement Agreements Between EPA and the State
(Performance Partnership Agreement)
2-24 Tribal Issues
2-25 Overview of Pollution Prevention and Waste Minimization
2-26 Pollution Prevention/Waste Minimization definition
2-27 The Environmental Management Hierarchy
2-28 Basic Waste Minimization Requirements of HSWA
2-29 Minimum Requirments for Inspectors for Waste Minimization
Sample Enforcement Response Policy
ii
MARCH 2000
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Introduction to
Environmental Compliance
Overview of Enforcement
.raj
If
• Components of a
compliance program
¦ Civil litigation
• Role of inspector in
enforcement actions
¦ Criminal enforcement in
EPA (Will be addressed in
Session 18)
Compliance and
Enforcement Program
¦ Laws and regulations
• Compliance and
enforcement strategies
¦ Compliance monitoring
¦ Enforcement response
• Follow-up to
enforcement actions
1
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Laws and Regulations
¦ Should be written
clearly to indicate
° Who is subject 10 them
° What is and is not a
violation
M
Compliance and
Enforcement Strategies
¦ Compliance monitoring plans
¦ Enforcement response policies
• Other policy and guidance documents
Compliance Monitoring
• Source self-monitonng and reports
* Inspections
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Enforcement Response
• Based on inspector's findings and self-monitoring
• Agency policy enforcement
¦ Graduates with seventy of violation
° Informal administrative response
° Formal administrative response
D Civil judicial response
c Criminal judicial response
Follow-Up to
Enforcement Actions
• Reports and certifications of compliance by
source
¦ Follow-up inspections
¦ More severe enforcement response if facility
remains in violation
Steps in an
Enforcement Action
¦ Violation found and documented
¦ Decision made on level and type of
enforcement response
' Enforcement documents drafted and filed
¦ Settlement negotiations entered
• Hearing or trial conducted
3
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What Can We Get From an
Enforcement Action?
Depending on law, violation, and circumstances'
Civil
¦ Comphancc with
requirement
• Monetary penalty
• Cleanup of
contamination
Criminal
• Monetary fine
¦ Prison sentence
Principal Elements of
Civil Litigation
¦ Theory of the case
• Burden of proof
• Standards of proof
»U
4
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Stages of Civil Litigation
¦ Conception and
preparation
¦ Pleadings
¦ Discovery
• Motion practice
• Trial
¦ Post-trial and appeal
COMPLAINT
COMPLAINT
This Court has Jurisdiction of ttw stfe)oct utur of
tlila icuon pursuant to Section 11X61 of th« CM. (i O i C
f 1411 (bl . taction 10»lb) or Lha cvjl. doic * 1J19 (t>» -
•action 1009 la) ct RCIU 42 0 • C f «92t(al. ItcUon )2*(b
• M (C) of IKM, 42 0 S C t 1104Mb) and (C). and pursuan
to »• 0 s C || last 1)4), and US)
Vanua i• propar in thin Diauict pursuant to taction
113(b) of tfts CM, 4? 0 t C t "Ulltbl taction 30»(») of
tna CWA, )) U l C • UDlDl, lacuen lOOItaMll of ACftA. «
OtC t *«>4411ls) III and lb) 11). ttw Director
prowiaod a copy of tna voueii of violation to the stataa 0
Kaavteky tod Ohio
*
5
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COMPLAINT
Aahlaad ia • corporation laaorporatad HMt th« lav* e
tha CflHBBMtlUt or Kantucky. wiu iti principal placa of
buiiBtit in HumiU, Mntuei)
Aahland own* and eptnui potroloua rafinariaa in,
«*ong othar plocaa Catlattaourg. Kantucky St faul Fart.
NimMU, and Canton. Glut Tn«a* ttcillUti ptoAie* •
varioty of patrolata preoieu Tha allagatiooa aot forth
balow apply Co tboaa throa faeilitiaa only
Aahlaad la a "paroon" within tot aoaaing or •action
302(a) of UN CJUk, «} O.S.C f 7*02 (a), Saction 50215) of
tha au, 3) 0 S C f 1)«2I3). and faction 1004(19) of *CJU.
42 D S.C f «»0)I1S), and taction 12»P) of EKJU, 42 0 1 C
f 11049(7)
B CUM |LX» ACT - ia!WUIU AMD aaCIATOI MaifJK)
Tha Claan Air Act aatabliahod a ragulatoxy a chap*
oaaignad to protact and anfianca th« quality of tn« nation's
air ao aa to prsaou tha public Milth and mKin ios tha
preductiva capacity of Ita papulation 42 0 S C f
>40lib)<1)
•action UOiai of to* CAA. 42 o » c 5 "Miou).
taquiraa oacft Stata to adept and lulalt te tna Adainlttrato
for approval, a plan for tha iaplaaaatatlon »alntonanea.
and anforeaaont of priaary aMnant ait quality ataourai aa
> H
COW PLAINT
=-¦=— '"a
DISCOVERY
U. ===¦——
MOTION
iti
——¦
6
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Motion in
Limine
Principal Differences Between Civil
and Criminal Enforcement
• Warrants based on "probable cause"
¦ Other constitutional guarantees
¦ Burden of proof, "beyond a reasonable doubt"
¦ More severe penalties imprisonment or fine
"Red Flags" That Indicate Possible
Criminal Activity
• Conflicting data
¦ Conflicting stones
¦ Unsubstantiated data
¦ Deliberate actions
¦ Claims of ignorance
about requirements
7
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Relationships Between Federal,
State, and Tribal Authorities
Federal Laws
¦ Treaties
Enforcement Agreements Between
EPA and the State
(Performance Partnership Agreement)
¦ Establish criteria and standards for EPA
oversight
• Establish criteria for direct EPA enforcement
¦ Specify data states will report to EPA
Tribal Issues
¦ 564—Federally
recognized tribes
. 227—Village
groups in Alaska
8
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Overview of Pollution Prevention
and Waste Minimization
» Pollution prevention
and waste minimization
• Hazardous and Solid
Waste Amendments of
1984
• Pollution Prevention
Act of 1990
Pollution Prevention - works for
"source reduction," and other practices
that reduce or eliminate the creation of
pollutants.
Waste Minimization - focuses on
reducing the generation and subsequent
release to the environment of the most
persistent, bioaccumulative, and toxic
chemicals in hazardous wastes
The Environmental
Management Hierarchy
• The environmental management hierarchy
consists of
0 Prevention
° Recycling
° Treatment
<¦ Disposal
ir
9
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Basic Waste Minimization
Requirements of HSWA
¦ Hazardous waste generators submit waste
minimization information as part of the
biennial reports
¦ Generators certify on manifest that waste
reduction program is in effect
• As a permit requirement, all TSDFs must
certify annually that waste reduction system is
in place
Minimum Requirements for
Inspectors for Waste Minimization
¦ Checking the manifest
¦ Checking the biennial report and operating
record
¦ Other waste minimization language
• Outreach
lo
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HAZARDOUS WASTE
CIVIL ENFORCEMENT RESPONSE POLICY
March 15, 1996
The policies and procedures set forth in this document are intended
solely for the guidance of employees of the Environmental
Protection Agency and State Enforcement Agencies. They are not
intended to, nor do they, constitute rulemaking by EPA. They may
not be relied upon to create a right or a benefit, substantive or
procedural, enforceable at law or in equity, by any person.
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2
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TABLE OF CONTENTS
Page
I. INTRODUCTION 1
12. RELATIONSHIP TO OTHER AGENCY
POLICY AND GUIDANCE 2
III. DEFINITIONS 4
A. Classification of non-compliance .........4
1. Significant Non-Complier (SNC) 4
2. Secondary Violators (SV) S
B. Enforceable 5
C. Evaluation Date 5
D. Formal Enforcement 5
E. implementing Agency 5
F. informal Enforcement —. — - 5
G. Return to Compliance 5
H. Sanctions €
IV. APPROPRIATE ENFORCEMENT RESPONSE 6
A. Formal Enforcement Response 6
B. Informal Enforcement Response 7
V. RESPONSE TIME GUIDELINES 8
A. Evaluation Date 8
B. Formal Enforcement Response Time 8
C. Exceedance of Formal Enforcement
Response Time 9
D. Informal Enforcement Response Time 11
VI. EPA ACTION IN AUTHORIZED STATES 12
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ATTACHMENT:
Enforcement Response Timeline
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I. INTRODUCTION
The goal of the Resource Conservation and Recovery Act
(RCRA) compliance monitoring and enforcement program is to attain
and maintain a high rate of compliance within the regulated
community. This goal is accomplished by establishing a
comprehensive monitoring and inspection program, and addressing
the most serious violators with timely, visible, and effective
enforcement actions. A timely and appropriate enforcement action
will return the facility to compliance as expeditiously as
possible, as well as deter future or potential non-compliance.
In December of 1984, the U.S. Environmental Protection
Agency's (EPA's) Office of Solid Waste and Emergency Response
issued the first RCRA Enforcement Response Policy (ERP). The ERP
sets forth response guidance for violations occurring pursuant to
RCRA where the State or EPA intends to pursue civil action,
including administrative or judicial action.
The 1984 ERP strengthened the RCRA enforcement program by
establishing guidance on timely and appropriate enforcement
response, and delineating conditions for EPA enforcement actions
in authorized States. The policy promoted the concept of prompt
escalation of an action when compliance was not achieved. In
addition, the policy -directed -enforcement-efforts -to-the~roost.
serious violators. The 1984 ERP was modified in December 1987.
The 1967 Revised ERP addressed changes in the program
resulting from the 1984 Hazardous and Solid Waste Amendments
(HSWA) to RCRA. The HSWA Amendments necessitated modifications
to the 1984 ERP in order to incorporate the broadening
programmatic responsibilities, including among other things
corrective action requirements, land disposal restrictions and an
emphasis on hazardous waste generators, treatment and storage
facilities, as well as land disposal facilities.
Since the development of the 1987 ERP, the RCRA enforcement
program has evolved. The RCRA regulated universe has expanded
due to the promulgation of new regulations. With the expansion
of previous enforcement authorities related to federal facilities
(i.e., 1992 Federal Facilities Compliance Act), the 1996 ERP will
now address all violating facilities including federal
facilities, in accordance with the criteria set forth in this
document. In addition, EPA continues to develop a tnulti-media
approach to facility compliance and encourages the use of
national. Regional and State enforcement initiatives to address
areas of non-compliance. Finally, EPA and State agencies are
working together to authorize States for significant portions of
the RCRA program. State primacy in implementing RCRA
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necessitates that the ERP accommodate the individual enforcement
processes utilized by State agencies in achieving compliance with
RCRA. The previous ERPs primarily reflected EPA's federal
enforcement process. The 1996 ERP will address the need for
increased flexibility, as well as incorporate program
developments from recent years.
The policies and procedures set forth herein are intended
solely for the guidance of employees of the EPA and State
enforcement agencies. They are not intended to, nor do they,
constitute rulemaking by EPA. They may not be relied upon to
create a right or a benefit, substantive or procedural,
enforceable at law or in equity, by any person.
The revised Hazardous Haste Enforcement Response Policy will
be effective on April 15, 1996.
II. RELATIONSHIP TO OTHER AGENCY POLICY AND GUIDANCE
The ERP is one of several documents that, together, define
the-national-RCRA-Enforcement -Program,--The--ERP -provides -a
general framework for identifying violations and violators of
concern and describing timely and appropriate enforcement
responses to non-compliance. The ERP should be read in
conjunction with the Office of Enforcement and Compliance
Assurance (OECA) Memorandum of Agreement (MQA) . The MOA
establishes annual priorities for compliance monitoring and
enforcement actions as identified by EPA Headquarters media
programs, Regions and States. The MQA encourages use of the full
range of tools to achieve compliance while emphasizing vigorous,
timely, and high quality enforcement against violators of
environmental statutes.
Other basic guidance utilized in the RCRA Enforcement
Program include the Policy Framework for State/Federal
Enforcement Agreements (revised August 1986, May 1992, February
1993, and July 1993) and the National Criteria for a Quality
Hazardous Waste Management Program Under RCRA (July 1986}. The
Policy Framework document is an Agency-wide guidance that calls
for enforcement agreements between EPA and States. It describes
what the State/EPA enforcement agreements should address,
including oversight criteria and measures, information needs,
procedures for notification and consultation, and criteria for
direct federal enforcement. The requirements of the MOA, RCRA
Implementation Plan, and other RCRA guidance are made applicable
to the States through the enforcement agreements.
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The National Quality Criteria document establishes basic
goals, objectives, and general performance expectations to assure
that EPA and the States have a common understanding of what must
be accomplished to effectively implement the RCRA program.
The National Quality Criteria document also outlines how
performance is to be measured and describes how EPA and the
States should respond when criteria are not met. The enforcement
program criteria modifications contained in the 1996 ERP
supersede and replace all timely and appropriate criteria
outlined in the Performance Expectations section of the National
Quality Criteria document.1 To the extent that a violator is
deemed eligible for consideration under the Compliance Incentives
for Small Businesses Policy, Small Communities Policy, the
Voluntary Environmental Self-Policing and Self-Disclosure Policy,
or the Audit Policy, the ERP will function as a supplement to
these policies. The Audit Policy states that it "supersedes any
inconsistent provisions in media-specific penalty or enforcement
policies... To the extent that existing EPA enforcement policies
are not inconsistent, they will continue to apply in conjunction
with this policy," provided that a regulated entity may not
receive additional penalty mitigation for satisfying similar
conditions under other policies for the same violations.
¦Incentives-for Self-_Policing: ,Jliscoyery,._Diaclosure^ Correction,
and Prevention of Violations," €0 Fed. Reg. €6706 (Dec. 22,
1995).
The ERP does not address the use of an order pursuant to
Section 3008(h) Of RCRA, 42 U.S.C. § 6926(h), to compel
corrective action; the use of an order pursuant to Section 3013
of RCRA, 42 U.S.C. 5 6934, to compel monitoring, testing and
analysis; or the use of an order pursuant to Section 7003 of
RCRA, 42 U.S.C. § 6973, to address situations that may present an
imminent and substantial endangerment to human health or the
environment. In addition, the ERP does not address violations
determined to be potentially criminal in nature and investigated
and prosecuted pursuant to Federal or State criminal authorities.
Guidance on the use of these authorities is set forth in other
policy documents except, and to the extent that, the ERP applies
when RCRA orders, decrees, or judgments are violated.
III. DEFINITIONS
1 The 1986 National Criteria For A Quality RCRA Program
permits adjustments to Regional/State Performance Expectations.
The 1996 ERP modifies previous enforcement response criteria to
encompass program developments, unique State authorities and
individual State enforcement processes.
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A. Classifications of non-compliance: Violators are
classified based on an analysis of the facility's overall
compliance with RCRA which includes prior recalcitrant behavior
or a history of non-compliance. This ERP establishes two
categories of violators: Significant Non-Compilers (SNC) and
other Secondary Violators (SV) .
1. Sicmif 1""^ pya-Compilers (SNCs) are those
facilities which have caused actual exposure or a substantial
likelihood of exposure to hazardous waste or hazardous waste
constituents; are chronic or recalcitrant violators; or deviate
substantially from the terms of a permit, order, agreement or
from RCRA statutory or regulatory requirements. The actual or
substantial likelihood of exposure should be evaluated using
facility specific environmental and exposure information whenever
possible. This may include evaluating potential exposure
pathways and the mobility and toxicity of the hazardous waste
being managed. However, it should be noted that environmental
impact alone is sufficient to cause a facility to be a SNC,
particularly when the environmental media affected require
special protection (e.g., wetlands or sources of underground
drinking water). Facilities should be evaluated on a multi-media
basis;^however,--a-facility may be-found-to-be -a-chronic—or
recalcitrant violator based solely on prior RCRA violations and
behavior.
2. Secondary Violators are violators which do not
meet the criteria listed above for SNCs. Secondary Violators
(SV) are typically first time violators and/or violators which
pose no actual threat or a low potential threat of exposure to
hazardous waste or constituents. A facility classified as a SV
should not have a history of recalcitrant or non-compliant
conduct. Violations associated with a SV should be of a nature
to permit prompt return to compliance with all applicable rules
and ^regulations.
B. Enforceable means the instrument creates an
independent, affirmative obligation to comply and imposes
sanctions for the prior failure to comply.
C. Evaluation Date is the first day of the inspection or
record review during which a violation is identified, regardless
of the duration of the inspection or the stage in the inspection
at which the violation is identified.
D. Formal Enforcement is an action which mandates
compliance and initiates a civil, criminal, or administrative
process which results in an enforceable agreement or order.
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E. frUPlfmptinq Agency is the agency with responsibility
for undertaking the required enforcement response.
F. Informal are those actions other than
formal enforcement that notify the facility of its non-compliance
and establish a date by which that non-compliance is to be
corrected.
G. Facilities will be deemed to have Returned to
ConmllMflrnt when they are in full physical compliance with
regulatory and/or statutory requirements or when they are in full
compliance with a compliance schedule established in a formal
enforcement action (either an order or an agreement).
H. Sanctions include penalties as well as other tangible
obligations, beyond returning to compliance, that are imposed
upon the owner/operator.
IV. APPROPRIATE ENFORCEMENT RESPONSE
The selection of an appropriate enforcement response is an
integral component of the RCRA enforcement and compliance
assurance progranw --An appropriate- response .w±ll ~achievfi .a .timely
return to compliance and serve as a deterrent to future non-
compliance by eliminating any economic advantage received by the
violator. This section establishes the criteria for determining
when formal and informal enforcement responses are appropriate.
A. FORMAL ENFORCEMENT RESPONSE
The designation of Significant Non-Complier (SNC) is
intended to identify non-compliant facilities for which formal
enforcement is appropriate. Specifically, SNCs are those
facilities which have caused actual exposure or a substantial
likelihood of exposure to hazardous waste or hazardous waste
constituents; are chronic or recalcitrant violators; or deviate
substantially from the terms of a permit, order, agreement or
from RCRA statutory or regulatory requirements.
The actual or substantial likelihood of exposure should be
evaluated using facility specific environmental and exposure
information whenever possible. This may include evaluating
potential exposure pathways and the mobility and toxicity of the
hazardous waste being managed. However, it should be noted that
environmental impact alone is sufficient to categorize a facility
as a SNC, particularly when the environmental media affected
require special protection (e.g., wetlands or sources of
underground drinking water).
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6
Facilities should be evaluated on a multi-media basis to
determine whether they are chronic violators or recalcitrant.
However, facilities may also be found to be chronic or
recalcitrant violators based solely on prior RCRA violations and
behavior.
Due to the nature of their violations, a SNC should be
addressed through a formal enforcement response. This response
must mandate compliance and initiate a civil, criminal, or
administrative process which results in an enforceable agreement
or order. The formal enforcement response should also seek
injunctive relief that ensures the non-conpliant facility
expeditiously returns to full physical compliance.
An enforcement response against a SNC by the implementing
agency will be considered appropriate when economic sanctions in
the form of penalties, or alternative punitive mechanisms, are
incorporated in the formal enforcement response. Penalties
incorporated in the formal enforcement response, or alternative
punitive mechanisms that recover the economic benefit of non-
compliance plus some appreciable amount reflecting the gravity of
the violation will be considered appropriate. The portion of the
penalty-which does-not account -for -the economic -benefit, .of-non--
compliance may be addressed through the use of Supplemental
Environmental Projects (SEPs) or Pollution Prevention Projects as
deemed appropriate by the implementing agency.2 The Agency
recognizes, however, that recoupment of the full amount of
economic benefit of non-compliance plus some appreciable portion
of gravity may not be possible in every case. A lesser penalty
amount may be appropriate where, for example, the violator
demonstrates an inability to pay the full penalty. In addition,
there may be circumstances where the nature of the violation(s)
and the manner of correction advance important policy objectives
such that substantial mitigation is warranted (e.g., where the
violation was discovered by the violator during an audit or self-
evaluation, and thereafter promptly and voluntarily disclosed to
the government and corrected, or where the violation by a small
business was disclosed and corrected pursuant to a government-
approved compliance assistance program).
In addition to the injunctive relief discussed above, the
implementing agency is encouraged to impose other measures
3 Federal enforcement actions that include a SEP or
Pollution Prevention project should comply with the criteria set
forth in the 1995 Interim Revised Supplemental Environmental
Projects Policy.
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against the non-compliant facility. Examples of non-penalty
measures include, but are not limited to, SEPs, permit decisions,
suspension and debarment proceedings, receivership or special
masters.
B. INFORMAL ENFORCEMENT RESPONSE
If a facility is found to be in violation but is not
designated a SNC it is designated a SV. An informal enforcement
response is the minimally appropriate enforcement response for
all SVs. An informal enforcement response consists of a
recitation of the violations and a schedule for returning the
facility to full compliance with all substantive and procedural
requirements of applicable regulations, permits and statutes.3
Facilities which fail to return to compliance following an
informal enforcement response should be re-classified as a SNC in
accordance with Section V. A. set forth below. The appropriate
enforcement response for a re-classified facility i6 the
immediate escalation to formal enforcement.
V. RESPONSE TIME GUIDELINES
This .section establishes-response time guidelines, for-formal
and informal enforcement actions. The guidelines are
designed to expeditiously return non-compliant facilities to
compliance with all applicable requirements of the Federal RCRA
program or the authorized State equivalent. ~ Response times are
divided into two categories, formal enforcement actions and those
for informal enforcement actions. A timeline depicting these
guidelines is attached. The timeline establishes response times
for three types of formal enforcement. The timeline also
establishes a 90 day deadline for the implementing agency to
determine whether the appropriate enforcement response is a
formal or informal enforcement action. Finally, -the timeline
establishes timeframes for the escalation from an informal
response to a formal enforcement response due to the violator's
failure to return to compliance.
A. EVALUATION DATE
The evaluation date will be defined as the first day.of any
inspection or record review during which a violation is
identified, regardless of the duration of the inspection or the
1 As noted in Bection II, above, "Relationship to other
Agency Policy and Guidance," compliance assistance efforts, such
as those set forth in the Compliance Incentives for Small
Business policy, may be applied in conjunction with this policy.
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8
stage in the inspection at which the violation is identified.
The first day of the inspection is the evaluation date,
regardless of the duration of the inspection or the stage in the
inspection which the violation is discovered. For violations
detected through some method other than record reviews or
inspection, the evaluation date will be the date upon which the
information (e.g., self-reporting violators) becomes available to
the implementing agency. In the case of a State referral to EPA
pursuant to Section VI. below, the evaluation date will be
considered the date of the referral to EPA. In the case of SV
facilities which are reclassified for failure to return to full
compliance (See Section IV. B. above), the evaluation date will
be considered the first day of discovery of non-compliance with
the compliance schedule established through the informal
enforcement response.
B. FORMAL ENFORCEMENT RESPONSE TIME
The attached timeline depicts the target response times for
enforcement pursuant to RCRA. The timeline establishes target
response times for three types of formal enforcement: (1) final
or consent orders; (2) unilateral orders; and (3) referrals to
-the Department of-Justice or the-Attorney ^General's Office. The
timeline delineates separate response times .for formal
enforcement and the escalation to formal enforcement from
informal enforcement.
(1) Final or consent orders are those documents for which
no appeal remains before the trier of fact. These orders
represent the agreement of the parties involved or the
decision of a trier of fact.
(2) Unilateral or initial orders are issued by the
implementing agency and assert the agency's position that
violations have occurred. However, the respondent/defendant
is afforded the opportunity to appeal the agency's
determination of violations to a trier of fact.
(3) For purposes of the ERP, a referral to the Department
of Justice or the State Attorney General's Office occurs
when the matter is officially transmitted to those offices
for action. A federal referral is considered to be
initiated upon the signature of the referral package by the
Regional Administrator or his/her designee, or the Assistant
Administrator for OECA, as appropriate. Kith regard to the
State's referral to the Attorney General's Office, each
State agency should establish a formal process for
requesting that the Attorney General's Office initiate
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9
enforcement proceedings on behalf of the State.4 Completion
of that process would then constitute referral to the
Attorney General's Office as set forth in the timeline,
C. EXCEEDANCE OF FORMAL EST OHCEMENT RESPONSE TIME
Response times articulated in the ERP should he adhered to
by the Regions and States to the greatest extent possible.
However, there are recognized circumstances (see discussion
below) which may dictate an exceedance of the standard response
times. In this revision to the ERP, a ceiling of 20% per year is
being established for consideration of cases involving unique
factors which may preclude the implementing agency from meeting
the standard response times. The 20% exceedance figure should be
calculated based on the total number of civil caBes existing in
the Region or State at any given time.
In cases where response times will be exceeded due to case
specific circumstances, the implementing agency must prepare a
brief justification for the delay and develop an alternative
schedule for case resolution. In the event that the Region does
not find adequate basis within the ERP guidelines for the State's
delay in enforcement, EPA reserves the -right to initiate-federal
-action. EPA will conduct periodic evaluations of Regional and
State enforcement response times for the purpose of determining
appropriate ceiling levels. Authorized State programs will have
response time reviews performed during evaluations conducted by
the Region pursuant to 40 CFR Section 35.150.
The Regions and States should strive to comply with the
standard response times contained in the ERP. However, when the
following considerations exist, up to 20% of the Regional/State
enforcement cases may exceed the standard response times:
o Cases involving violations of two or more media;
(e.g., environmental protection statutes)
o Cases involving more than one facility;
o Potential criminal conduct which iB under
investigation;
o National enforcement initiatives;
4 All references to the State Attorney General's Office in
this document should be interpreted as including any State
enforcement body that possesses the authority to initiate actions
in State Court.
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10
o Cases involving nationally significant issues;5
o Novel legal issues or defenses;
o Site abandonment;
o Additional sampling or information requests are
required to confirm the violation(s); and
o Need for outside technical experts.
- The Agency recognizes that circumstances may arise where the
enforcement response times specified may be insufficient to
prepare and initiate the appropriate enforcement response as set
forth in this policy. It is also recognized that instances may
occur where immediate action is appropriate. The Agency expects
that the Region or State will take priority enforcement action in
the following situations:
o Where a release or other violation poses an
immediate threat to human health or the
environment.
o Where activities of the owner/operator must be
stopped or redirected, such as cases in which the
Agency or the State seek to immediately halt
improper construction or installation of a
regulated unit.
o Where the threat of a dissipation of assets would
undermine closure, post-closure, or corrective
action activities.
o Where there is an imminent statute of limitations
deadline or bankruptcy deadline.
D. INFORMAL ENFORCEMENT RESPONSE TIME
Once a determination is made to utilize an informal
enforcement mechanism, a violator is given notice of its non-
compliance and the implementing agency will establish a date by
which all violations must be corrected. The objectives of an
informal enforcement response are to compel the violator to cease
9 Requests for exceedance of the formal enforcement
response times due to existence of nationally significant issues
are generally reserved for EPA enforcement responses.
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11
its non-compliant activities and ensure that full physical
compliance is achieved in the shortest possible time frame.
At the time a violator is formally notified of the violation
determination it is given a compliance date which establishes a
deadline for the violatior to correct all known violations. A
correction period during which a violator should correct all
known violations should not exceed 90 days. For a violator to be
considered a candidate for informal enforcement, violations must
be of a nature that will permit such a prompt return to
compliance with all applicable rules and regulations. Violators
addressed through an informal enforcement response should not
have a history of recalcitrant or non-compliant conduct.
Violators that will require an extended compliance schedule
in order to achieve full physical compliance should be addressed
through a formal enforcement response. The compliance date
should reflect the minimum period of time necessary for the
violator to return to full physical compliance. A violator that
has corrected its violations on or before the assigned compliance
date is officially deemed to have returned to compliance.
If a violator is -.unable-ta^neet. Jthe assigned coit£>liance
deadline it must immediately notify the implementing agency and
provide that agency with documentation supporting the inability
to correct violations by the prescribed compliance date. A
decision to extend the compliance date should be made only when
supported by sufficient documentation. Failure to achieve full
physical compliance by the compliance date or a failure to notify
the implementing agency of the inability to correct violations
should result in an escalation to formal enforcement. The first
day in exceedance of compliance date is to be considered the
evaluation date for the purpose of escalating the action to a
formal enforcement response. For liability and penalty
assessment purposes, however, nothing in this ERP should preclude
the assessment of penalties for any violations which occur during
the correction period.
VI. EPA ACTION IN AUTHORIZED STATES
States with authorized RCRA programs have the primary
responsibility for ensuring compliance with the RCRA program
requirements. However, EPA retains the authority to take
independent enforcement action in authorized States in accordance
with Section 3008(a) (2) of RCRA. Pursuant to this Section, EPA
may take direct action after notice to the authorized State. EPA
authority to initiate an independent enforcement action iB not
limited to the examples set forth, the Agency may take direct
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12
action after consideration of all pertinent factors and
consultation with the State.
Notwithstanding Section 3008(a)(2) of RCRA, EPA will
generally take civil enforcement actions in authorized States
only under the following circumstances:
o The State requests that EPA pursue a federal
action and provides justification based on unique,
case specific information;
o The State is not authorized to take action or
State authority is limited;
o The State fails to take timely and/or appropriate
action;
o Cases involving issues that could establish a
legal precedent or in which federal involvement is
needed to ensure national consistency;
o Cases involving multi-state, multi-regional
"national violators
o Cases involving interstate pollution problems
associated with watersheds, air basins or other
geographic units that cross state lines; or
o Cases brought to prevent non complying companies
from obtaining an economic advantages over their
competitors, thereby maintaining a "level playing
field" for the regulated community.
The previous Sections described the criteria for timely and
appropriate action in response to violators in two (2) distinct
categories (SNC and SV) . The response times set forth in Section
V. B. establish clear guidelines for a Region or State to follow
during a formal enforcement process. If a State fails to take
formal enforcement action within the standard response time, the
State must provide the Regional office with adequate
justification for consideration of an alternative schedule.
The Memorandum of Agreement (MOA), Memorandum of
Understanding (MOU), or other agreement between EPA and each
State should detail a process for notifying the State of EPA
intent to initiate an independent enforcement action. The
Regional office may need to conduct its own case development
inspection, and prepare additional documentation before
proceeding to initiate an action.
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13
A State may find it necessary and advantageous to refer
specific cases to the Region for federal enforcement. If a State
decides to refer a case to EPA for federal enforcement, this must
be completed within 90 days of the original Evaluation Date. For
the purposes of establishing a new Evaluation Date, the date of
the referral to EPA is considered the Evaluation Date. The State
should provide all case development information to the Region as
part of the referral package. This should facilitate a reduction
in the time needed for Regional case development.
-------
Timeline For Enforcement Pursuant to
The Resource Conservation artd Recovery Act
D:-vO
EvJ u.lt: HI
r-z-fin
Enbit'fin'jiH
App::oriat-;?
Dsy 1
Uriila'AfrJ or lnU^
I My 0
Dcia
IftyUK..
Cf.J'" ¦ '
d-/ ;ig
' Rr^iralt:.
AG f.i DOJ
Nolo: All days are calendar days measired from day 0.
-------
3
-------
SESSION 3
TOPIC: SUMMARY OF ENVIRONMENTAL STATUTES
Time: 1 hour 45 minutes
PURPOSE
Key Points
List of Visuals 3-1
3-2
3-3
3-4
3-5
3-6
3-7
3-8
3-9
List of Handouts 3-1
i MARCH 2000
Provide an overview of the major statutes under which EPA has
authority.
Discuss inspection activities under each statute.
While each statute is different, they have many features in common.
Inspectors should be able to recognize major violations of other EPA
programs and refer them, as appropriate.
Summaiy of Environmental Statutes (Title Slide)
Statutoiy and Regulatory Process
Major Statutes Implemented by EPA
Common Statutory Features
Typical Enforcement Options
Selected Provisions of 40 CFR
Selected Provisions of 40 CFR (continued)
Authorities Granted Under Federal Environmental Laws and
Regulations for Administrative Investigations
ESRC CD-ROM
Summaiy of Authorities
-------
Summary of
Environmental Statutes
Statutory and Regulatory Process
• People
¦ Congress
• "Agency"
¦ Regions/states/tribes/locals
Major Statutes Implemented by EPA
i
-------
Common Statutory Features
¦ Set national standards
¦ Administered through regulations, policies,
delegation and permits
¦ Agency authority for inspection, monitoring,
testing, information, and emergency
response
¦ Determining violations and seeking
correction, remediation, relief
¦ Fines, penalties, and jail
Typical Enforcement Options
s Notice of violation
¦ Civil administrative and judicial complaints
¦ Emergency action
¦ Injunctive relief
¦ Criminal action
• Debarment
Selected Provisions of 40 CFR
2
-------
Selected Provisions of 40 CFR
(continued)
tttMO NPOapntVft
MI-M7
IU-U0
sun
MUR
40M71 CW*«
m-IU Imbi
Autftortttw Ormnfd LMdf Fttrml EnvinxunfiUl L«w»
and Ragutrtora for Admtnlstrrtv* IrrrtstigMtlon*
CAA
RCRA
CERCLA
EPCRA
CWA
TSCA
FIFRA
ftt
J
-------
Authorities Granted Under Fe nrtronmental Laws and Regulations
for Administrate..
-------
4
-------
SESSION 4
TOPIC: INSPECTOR ISSUES
Time: 1 hour 15 minutes
Purpose
Key Points
• Provide an overview of the roles and functions performed by inspectors
that will be covered in more depth during the course.
• Provide information about issues related to confidential business
information and ethics that are of concern to inspectors.
• Present techniques for handling press and other public inquiries related
to an inspection.
• Provide awareness of the inspector's liability for false statements.
• Inspectors are involved in virtually every aspect of the compliance and
enforcement program.
» The inspection is a team effort.
• Inspectors have access to confidential data and must handle such data as
its confidentiality requires.
• When the inspector is faced with a question of ethics, the rule of thumb
is, when in doubt, don't!
• When dealing with the press, emphasize the positive.
List of Visuals
List of Handouts
4-1 Inspector 1 ssues (Title Slide)
4-2 Inspector Issues
4-3 to 4-IT (3 Role of the Inspector
4-6 to 4- P
-------
Inspector Issues
4-1
Inspector Issues
Role of the inspector
Responsibilities of the
team leader and team
members
Confidential business
information
Ethical considerations
Techniques for handling the
press and the public
«
V
Role of the Inspector
All stages end Aspects of
Complicrice end E nfor cement
Progrcm
1
-------
Role of the Inspector
•Official
Representative
V
Official
Representative
Role of the Inspector
¦Official representative
•Fact-finder
¦
4-5
Role of the Inspector
•Official representative
•Fact-finder
¦Enforcement case
developer
\ v
Enforcement Case
Developer'
-------
Role of the Inspector
"Official representative
¦Fact-finder
¦Enforcement case
developer
¦Provider of
enforcement presence
Enforcement
Presence
1
4-7
Role of the Inspector
¦Official representative
¦Fact-finder
•Enforcement case
developer
•Provider of enforcement
presence
¦Technical educator
K2BMHt
Technical Educator
Role of the Inspector
¦Official representative
•Fact-finder
•Enforcement case
developer
¦Provider of enforcement
presence
¦Technical educator
¦Technical authority
44
Technical Authority
3
-------
Role of the Inspector
•Official representative
¦Fact-finder
¦Enforcement case developer
¦Provider of enforcement
presence
•Technical educator
¦Technical authority
¦Compliance Assistance
4-10
Role of the Inspector
Compliance Assistance
¦Tier I - Sharing
standardized information
and references
Role of the Inspector
Compliance Assistance
•Tier II - More technically
complex and site-specific
• Detailed technical
information/discussion
of individual facility
-------
Role of the Inspector
Compliance Assistance
technically complex and
site-specific
' Assisting owner/operator
in operating facility or in
making design/operation
changes
0 Consulting services to
facility
4-IJ
Responsibilities of the Team Leader
and Team Members
r Fr
Hhy Responsibilities
Responsibilities of the Team Leader
and Team Members
¦ Planning
¦ Specific tasks
¦ Broad perspective
¦ Work as a team
• Complete report
•V*
-r.
h ' .Yf
r W
~•IS
-------
Team Leader
Working with
management, technical
experts, legal specialists:
IDENTITY THE
SCOPE!
Team Leader
¦Identify Resources
People
Equipment
v
Money
Files end Dcfa Bases
Team Leader
Problem
Objective
-------
Team Leader
Gulden ce
Trdning
Team Leader and Team Members
¦COMMUNICATION
Team Leader
When developing schedule
for inspection activities,
keep in mind such
questions as:
•What tasks need to be
performed
¦How long will each task
take
¦When do the tasks need
to be completed
4-11
-------
Team
Report
•Team Leader assigns
writing responsibilities
° sections
° schedules
— -
•Team Members prepare
appropriate sections on
schedule
¦Team Leader prepares
executive summary
4-23
Follow-up
CONFIDI
8
-------
Confidential Business Information
How many have
received TSCA
CBI training?
4-23
Confidential Business Information
WHAT IS IT?
¦ TSCA CBI vs confidential information
claimed pursuant to 40CFR Part 2
° (also FIFRA and proposed RCRA CBI)
¦ Proprietary data
° Chemical formulations
° Special process operations-special techniques
¦ Financial information-lists of customers
° Anything that might give another company a
competitive advantage
Confidential Business Information
WHAT IS IT - continued
• Anything the company claims as CBI
¦ Receipts must be provided for CBI material-
TSCA receipts are preprinted
¦ Agency can declassify after requiring the
company to justify based on four separate
areas (see 40 CFR Part 2)
*-27
9
-------
Confidential Business Information
•TSCA CBI has very
stringent handling
requirements
"All CBI must be properly
secured
Confidential Business Information
•Only authorized
personnel can see
the data
Confidential Business Information
•Access log is
maintained
m
*1.
10
-------
Confidential Business Information
•Limits are imposed on
copies made
4-JI
Confidential Business Information
aj
i'
]rt generated
also is CBI
A. E
/
/ >; -?»
/
/v.
%
: ./
*-32
X
/
/
•si
-------
ETHICS
When in Doubt, Don't!
¦ Integrity and impartiality
¦ Conflict of interest
¦ Standards of conduct
% r93*
" Consult with your ethics official first
Dealing with the Press
and the Public
Emphasize
The
Positive!!
The Reporter's Viewpoint
Goal: A usable story
Differences among:
¦ Newspaper
D Television
0 Radio
'-if |j
' ;'V
v».. ¦
^ .j. Y>4
i I ¦
ijM
¦ IM
-------
Talking with the Press
¦ Know what you want to say
¦ Use the interview as an opportunity to say it
¦ Be professional
¦ Don't say too much
¦ Don't speculate
%
-------
HANDOUT 4-1
INSPECTOR'S LIABILITY
Inspectors must make sure they are honest, forthright, and live up to the Boy Scout law in all their dealings
with the regulated community. One senior inspector conducted an inspection at a facility and found major
repeat violations. The inspector wrote the report and was responsible for either negotiating a settlement or
preparing for trail. During discovery, the inspector provided information about education, work
experience, and other facts, as requested by the defense attorney. The inspector's credentials were
extensive and impressive; however, because of comments made during a deposition, the inspector's
educational background was checked. The inspector had stated that he had a doctoral degree when, in fact,
he had only taken courses toward such a degree. As a result of that dishonesty, the inspector was removed
from the case, was placed under house arrest (was allowed only to go to work and return home), and
ultimately was fired.
In another case, two inspectors were picked up at the airport by a courtesy shuttle. One of the inspectors
claimed taxi fare, while the other did not When questioned about the claimed taxi fore, the inspector
admitted falsely claiming the fare and resigned.
During a major cleanup activity, an oo-scene coordinator aided a contractor in obtaining a contract,
accepted special favors, and falsified information on travel vouchers. Acting on a tip, the OIG and OCI
initiated an investigation, documented the illegal activity, and had the individual arraigned in federal court
The case is still pending.
During a criminal investigation at a federal facility, evidence showed that three senior civilian employees
knowingly and willingly had disposed of hazardous waste. Since h was a government facility and the
government brought charges against the employees, they had to hire their own attorneys for the trial. The
employees were found guilty, given suspended sentences, and fined. After being found guilty of a felony,
they lost their government pensions, in addition to expending most or all of their life savings on legal fees.
Since inspectors are gathering evidence to collect fines or put people in jail, all inspectors must ensure that
they are honest and above reproach; otherwise, they are subject to fines, dismissal, or imprisonment
1
MARCH 2000
-------
5
-------
SESSION 5
TOPIC: INSPECTION PLANNING
Time: 90 minutes
Purpose
Stress the importance of planning and advance preparation.
Key Points
List of Visuals
List of Handouts
• Present information about key planning activities
• Plan in advance what to look for, how to look, and what
documentation to collect: saves time and money and ensures a
thorough inspection.
• Be Familiar with inspection options including Multimedia Inspection,
Process Based Inspections, and Environmental Management System
Evaluations
5-1 Inspection Planning (Title Slide)
5-2 Planning the Inspection
5-3 Goal of Inspection Planning
5-4 Know What To Look For
5-5 Know How To Find It
5-6 Know How To Collect, Document, and Preserve
Evidence
5-7 Be Safe and Efficient in the Field
5-8 Reviewing EPA Records
5-9 to 5-24 Project Planning
5-25 to 5-27 Multimedia Inspections
5-28 to 5-39 Process Based Inspections
5-40 to 5-57 Environmental Management Systems
5-1 Generic Inspection Check List
5-2 Sample Project Plan
April 2000
-------
Inspection Planning
M
Planning
from AJice in Wonderland
¦"Would you tell me, please, which way I ought
to go from here9
¦ "That depends a good deal on where you want
to go to, "said the cat
¦"I don't much care where, "said Alice
•"Then it doesn't matter which way you go,"
said the cat.
Planning the Inspection
• When plans went awry
¦ importance of planning
• Key planning activities
• Defining scope and objectives
• Check lists
• Reviewing EPA records
-------
Goal of Inspection Planning
Identify all activities necessary to gather
information to assess whether a facility is in
compliance and to use as evidence in possible
enforcement action
HOW TO ACCOMPLISH GOAL?
BE PREPARED'
Know What To Look For
¦ Identify type of inspection
¦ Compliance evaluation
0 Routine
0 For cause
0 Oversight
¦ Define objective of inspection
¦ Decide focus of inspection
Know How To Find It
¦ Review records and permits
¦ Know compliance histor)
• Talk with attorneys and other inspectors
• Contact state and local officials
2
-------
Know How To Collect, Document,
and Preserve Evidence
• Know what nontechnical evidence
is needed
• Identify the kind and quantity of physical
samples needed
¦ Identify' necessary equipment and check
condition
¦ Prepare QA/QC plan for documentation, chain
of custody, transportation
Be Safe and Efficient in the Field
• Develop safety plan
¦ Use personal protective equipment
• Define tasks of all members of
inspection team
¦ Arrange logistics in advance
0 Travel
o Pay
0 Transportation
D Lodging
° Special equipment
Reviewing EPA Records
• Become familiar with the facility
• Discover inadequacies in the information
• Minimize inconvenience to facility personnel
¦ Clarify technical and legal issues before entry
¦ Develop inspection plan
3
-------
Development of the Project Plan
* Foundation and purpose of the
project plan
Steps in developing the project plan
Team-building considerations
• Review of basic elements
Ml
Elements of a Project Plan
• Objectives
Background
• Tasks
• Policies and procedures
Safety
Resources
Schedules
• Modifications of the plan
4
-------
Identify the Overall Project
Objectives:
Focus on wh) ¦ facility is
targeted
Reasons for selecting a facility
Determine the desired outcome
Create a statement of objectives
Gather Background Information:
Background information is cnicial for developing
a project plan
Identification of Tasks
What activities must be
accomplished to meet the
inspection objectives
-------
Policies and Procedures
• Organization Standard Operating Procedures
(SOP's)
• Special procedures applicable to this inspection
• Policies and Procedures of other organizations
• e g Federal EPA State environmental agency,
Tribal considerations. US Attorney, DOJ, State
Attorney General, other organizations
Safety
¦Safety Plan
•Requirements of Specific
Organization
•Safety Equipment Required
¦Special Safety Considerations
Resources
• Team Members for
onsite inspection
¦ Laboratory Support
• Administrative Support
Money
• Time
6
-------
Buildina the Team
* Expertise needed
• Size considerations
• Development of the team
• Management support
Necessary Skills and Qualifications
• Knowledge of policies and procedures
• Familiarity with a range of media
• Knowledge of technical issues
• Investigatory skills
• Recent experience
• Communication skills
• Experience
Development of an
Inspection Schedule
• Importance
- To the client
- To the team
- To the facility
• Principles
7
-------
Milestones in
Schedule Development
• Pre-inspection planning meetings
• Inspection dates
• "In" briefings
• "Out" briefings
• Due dates of reports
Final Steps
* Reevaluate the team
* Finalize the written project plan
* Conduct a preinspection team meeting
».r
Notification
• Procedures (announced or unannounced)
• Necessity of a letter of notification
• Information requested in a notification
letter
• Notification of state regulatory officials
• Notification of the laboratory
• Time factors
8
-------
EVOLUTION OF INVESTIGATION
COMPLEXITY
^ MULTIMEDIA COMPLIANCE INSPECTION
SINGLE-MEDIA COMPLIANCE INSPECTION
Overview: Multimedia Inspections
and Enforcement
• Define multimedia
• Define holistic approach
• Advantages and disadvantages of teams
• Advantages and disadvantages of
multimedia inspections
• Four categories of inspections
• Targeting and resources
• Team skill requirements
Industry Comments
• Reduce the number of visits by inspectors
• Easier to get questions answered and address
problem issues
• Inspectors develop better understanding of
facility operations or problems
• More thorough inspections
i.r
9
-------
PROCESS-BASED
INSPECTIONS
"Process-Bited Investigations Guide"
March 1997
EP A-JS0I9-97 -001
NEIC Library: (303)236-5111 *2S7
EVOLUTION OF INVESTIGATION
COMPLEXITY
w PROCESS-BASED INSPECTION
MULTIMEDIA COMPLIANCE INSPECTION
___ SINGLE-MEDIA COMPLIANCE INSPECTION
10
-------
Process-Based Inspection
Initially focuses on/subsequently based on
• comprehensive understanding of facility
processes
Includes
• tracking raw materials into and through plant
¦ identifying by-product, co-product and products.
• identifying wastes generated
• determining how wastes are ultimately managed
»i|
Process-Based Inspection
Purpose
¦ obtain indepth knowledge of facility
operations
* use knowledge to make more informed
investigative evaluations and
determinations
Why Conduct Process-Based
Inspection??
Often only method to
¦ Determine complete universe of regulated
facility wastes/activities
¦ Evaluate accuracy and completeness of
facility self-reporting data/permit
application information
¦ View large or complex facility 'holistically*
vn
u
-------
PROCESS-BASED INSPECTION
Raw czN
Materials
Product/
Co-product
Process-Based Inspection Tools
• Knowledge of process
operations
¦ Process flow diagrams
¦ Material balance sheets
¦ TRI reports (EPCRA 313)
• Process observations
-------
So tell me about
your EMS
-------
EVOLUTION OF INVESTIGATION
COMPLEXITY
. _ ® EMS EVALUATION
PROCESS-BASED INSPECTION
. . MULTIMEDIA COMPLIANCE INSPECTION
SINGLE-MEDIA COMPLIANCE INSPECTION
EPA EMS Policy Statement
March 1998
"Implementation of an EMS has the potential to
improve an organization's environmental
performance and compliance with regulatory
requirements EPA supports and will help
promote the development and use of EMSs"
Innovations Task Force Report
July 1999
Action Item 2: Promote the use of EMSs
Objective: We will encourage organizations to use
EMSs that improve compliance, pollution prevention
and other measures of environmental performance
Taak 2: We will promote the use of EMSs to
address known compliance and performance
problems
14
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EMS Definition
ISO 14001
The part of the overall management
system., for., implementing., the
environmental policy
Policy
Review F"annin"
Implement/
Operate
Check/
INDUSTRY WITHOUT AN EMS
Environmental
Requirements1
Raw :—
Materials
Produc
INDUSTRY WITH AN EMS
Environmental
Requirements
IS
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COMPLIANCE-FOCUSED
ENVIRONMENTAL MANAGEMENT SYSTEM
DEFINITION
"A system for identifying pertinent
environmental requirements - statutes,
regulations, permits, enforceable agreements,
etc - and translating them into sustainable
compliance activities at a facility."
NEIC 1996 parting tot stgn
NEIC EMS Evaluations
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Causal Analysis
Answers "why" noncompliance
occurred ffc J
V*w.
kTJ
Aids in developing solutions
to prevent recurrence
I
Compliance-Focused EMS
"Measuring Stick"
Contained in August 1997 Publication
"NEIC Compliance-Focused EMS -
Settlement Agreement Guidance"
ww.es.epa.gov/oeca/oceft/neic/12elemen.pdf
COMPLIANCE-FOCUSED EMS
FIRST C ARE PRIMARY ELEMENTS ;
n<
1 Management Policies and Procedures t—
2 Organization, Personnel, and Oversight
3 Accountability and Responsibility
4 Environmental Requirements
5 Assessment, Prevention and Control
6 Environmental Incident and Non-Compliance
Investigations
17
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COMPLIANCE-FOCUSED EMS
SECOND 6 ARE SUPPORT FUNCTIONS
7 Environmental Training, Awareness, and
Competence
8 Environmental Planning and Organizational
Decisionmaking
9 Maintenance of Records and Documentation
10 Pollution Prevention Program
11 Continuing Program Evaluation
12. Public involvement/Community Outreach
NEIC EMS Evaluation Objectives
Evaluate EMS vs. 12 CFEMS Elements
Determine underlying causes of
noncompliance
Obtain information for
settlement purposes
Causal Analysis Method _,
Identify the problem (i.e., violation)
Identify the direct causes immediately
preceding the problem
Identify the contributing or "root"
causes using the 12 CFEMS elements
18
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Causal Analysis Example
Permit
exoaeflance
ELEMENTS THAT MOST FREQUENTLY
CAUSE VIOLATIONS
1 environmental requirements
S. ASSESSMENT fREVENTlON AND CONTROL
7 ENVIRONMENTAL TRAINING, AWARENESS
AND COMPETENCE
9 MAINTENANCE OF RECORDS AND
DOCUMENTATION
19
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Avoid the Engineer" Paradigm
To the engineer, all matter in the
universe fits into two categories
(1) things that need to be fixed, and
(2) things that will need to be fixed
after you've had a few minutes to
play with them
20
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GENERIC INSPECTION CHECK LIST
OBJECTIVES
- What is the purpose of the inspection?
TASKS
- What records, files, permits, and regulations will be checked?
- What coordination with laboratories, other programs, attorneys, and state or local governments
is necessary?
- What information must be collected?
PROCEDURES
- What specific processes of the facility will be inspected?
- What procedures will be used?
- Will the inspection require special procedures?
- Has a QA/QC plan been developed, and is it understood?
- Has a safety plan been developed, and is it understood?
- What are the responsibilities of each member of the inspection team?
RESOURCES
- What personnel will be required?
- What equipment will be required?
SCHEDULE
- What will be the time requirements?
- What will be the order of inspection activities?
- What will be the milestones (What must be done, compared with what is optional)?
1
July 1997
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PROJECT PLAN
MULTI-MEDIA COMPLIANCE INVESTIGATION
XYZ COMPANY. MIDTOWN. ANYSTATE
INTRODUCTION
The XYZ Company operates a plant at 1234 An ywhere Road in the middle part of Midiown,
Anysiate [Figure 1], EPA Region XX requested that NEIC conduct a multi-media comphanc e
investigation of the XYZ plant. The specific objectives of the investigation are to determm e
compliance with:
• Water pollution control regulations under the Clean Water Act (CWA), includin g
wastewater pretreatment requirements and Spill Prevention and Contro 1
Countermeasures (SPCC) regulations
• Hazardous waste management regulations, under the Resource Conservation an d
Recovery Act (RCRA) and the Anystate Administrative Code (AAQ
• Underground Storage Tank (UST) regulations
• Air pollution control regulations under the Clean Air Act (CAA), Federa 1
Implementation Plan (FIP), and the Federally approved portions of the Stat e
Implementation Plan (SIP)
• Toxic Substances Control Act (TSCA) PCB regulations
• Superfund Amendments Reauthorization Act, Title m. Emergency Planning an d
Community Right-To-Know Act (EPCRA) regulations
Compliance with other applicable environmental regulat ions may be determined by the NEIC.
Region XX personnel will evaluate compliance with TSCA Sections 5. 8.1 2, and 13 during the NEIC
inspection, and report their findings separately.
BACKGROUND
XYZ began operating the plant in 1492. Compounds A, B, and C; chemicals D, E, and F ;
pesticides G and H, and special containers for these materials have been manufactured on site. I n
1942, some operations (formerl y under the Middle Division) were acquired by a company known as
"Newage, Inc." The remaining XYZ plan I currently manufactures water soluble specialty items, and
conducts research and development.
The XYZ plant employs a total of about 1.300 people, in a Primary Division, a Secondar y
Division, a Tertiary Division, and R and D Laboratory. The Primary Division manufacture s
compounds A, B. and C (240 tons in 1990). Raw materials for the compounds are purchased from
Subject to revision
(03/92)
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F-2
an outside source. The Secondary Division makes chemicals and pesticides under numerous brand
names (180 tons in 1990), and the Tertiary Division makes special containers for these materials (3
million containers in 1990). Research and development are conducted by R and D Laboratory.
The EPA Region XX Environmental C ompliance Division. Midtown District Office (MDO),
conducted a multi-media inspection of the XYZ plant during the first quarter of 1991. The MD 0
inspection report identified concerns with wastewater control, hazardous waste management ,
documentation, and spill prevention control.
Approximately 1.2 million gallons of wastewater per day are discharged to the Midtow n
Wastewater Treatment Plant (MWTP) of Midtown, Anystate. There are two direct Nationa I
Pollutant Discharge Elimination System discharges (001 and 002) to the Midtown River at thi s
facility. Additionally, sewered plant effluent discharge is regulated by the MWTP pretreatmen t
standards, and the Federal effluent limitations and standards for the Compounds, Chemicals ,
Pesticides and Containers point source category. The R and D Laboratory conducts the Company's
effluent analyses.
Violations of the MWTP pretreatment ordinance effluen t limitations have occurred for solids,
and the toxic standards. MWTP is concerned with data indicating the discharge of solids and toxics
J, K, and L from the plant. XYZ also may have modified their pretreatment plant without obtaining
a construction permit required by the Anystate Environmental Resources Department (AERD).
XYZ submitted the original RCRA Part A permit application on November 15, 1980. The
application listed 19 hazardous waste management units, including 4 container storage areas, 1 0
storage tanks, and 5 storage surface impoundments. AERD is responsible for monitoring hazardous
waste activities.
The facility's June 1990 contingency plan lists 1 4 above ground and 22 underground tanks on
site. The tanks range in size from 2,000 to 50,000 gallons, with the majority between 5,000 an d
20,000 gallons. These tanks are located in a tank farm area and near production areas.
The plant emits both volatile organics and particulates. There is no volatile organi c
constituent emission control equipment. Particulate emissi ons are controlled by three dust collectors.
Five wet scrubbers are used to control fugitive particulate emissions when mixing bags of dry raw
materials in reaction vessels. Air emissions are regulated by "Anystate Permits and Air Pollutio n
regulations including AERD Operating Permits. EP A also promulgated a FIP on February 14, 1991.
On August 31, 1983, EPA Region XX conducted a PCB sampling inspection at the plant
XYZ was fined for viol ations, including cracks in the floor of the PCB storage area, not conducting
monthly inspections, no annual document, and not properly marking PCB transformers.
The Toxic Release Inventory (TRI) for this plant lists emissions of A, B. C, and D. The TRI
also lists various inorganics, including E. F. G, and H.
INVESTIGATIVE METHODS
Investigation objectives will be addressed by:
(03/92)
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F-3
• Compilation and review of EPA, AERD, and MWTP daiaba.se and file information
• Meetings with EPA Region XX personnel to discu ss investigation specifics including:
objectives, logistics, and potential sampling locations
• An on-site inspection
Meetings with Region XX personnel took place (date) The on-site inspection, scheduled to
begin (date), will include:
• Discussing plant operations with facility personnel
• Reviewing and copyi ng, as appropriate, facility documents including operating plans
and records
• Visually inspecting plant facilities including processing, material storage, and waste
handling facilities
• Sampling and analysis of appropriate waste streams and/or any un known/unauthorized
discharges to assist in compliance determination, as follows'
(a) MWTP will col lect and analyze wastewater samples for organic constituents
during the week of (date). AllQA/QC will be the responsibility of MWTP.
(b) NEIC will collect wastewater samples for v olatile organic constituent analysis
during the on-site inspection. NEIC will conduct the associated analysis.
After completing the on-site inspection, NEIC investigators will br ief appropriate EPA
Region XX Program and Office of Regional Counsel per-sonnel regarding preliminar y
findings.
A draft report, including any analytical data, will be written by NEIC personnel and
transmitted to EPA Region XX personnel for review and comment A final report will be
completed about two weeks after Region V comments are received. If analytical data are not
available by (date), they will be presented in an addendum to the report.
NEIC personnel will be available for any additional support required (negotiations ,
litigation, etc.) until noncompliance issues are resolved.
DOCUMENT CONTROL PROCEDURES
NEIC document control procedures *" will be followed during the inv estigation. TSCA
"Notice of Inspection" and "Confidentiality" forms will be completed during the opemn g
conference. Documents and r ecords obtained from the Company will be uniquely numbered
NEJC Policies and Procedures Manual, revised August 1991
(03/92)
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F-4
and listed on docu-mcnt logs. Photograph logs will also be maintained A copy or (h e
document and photograph logs, w ith a Receipt For Samples/Document form, will be offered
to the Company prior to completion of the on-site inspection. Any documents declared to
be confidential business information pursuant to 40 CFR Part 2 will be so noted on the log
and secured appropriately.
SAFETY PROCEPURES
Safety procedures to be followed during the on- site inspection will comply with those
described in the attached safety p Ian [Appendix A], and established NEIC safety procedures.
These procedures are contained in EPA 1440 - Occupational Healt h and Safety Manual (1986
edition), Agency orders and applicable provisions of the NIOS H/OSHA/USCG/EPA Occupa-
tional Safety and Health Guidance Manual for Hazardous Waste Site Activities. Th e
Company's safety policies will also be reviewed and followed.
TENTATIVE SCHEDI It .F.
(date) Region XX will notify facility of inspection (verbally and in writing)
(date) Initiate on-site inspection
(date) Brief Region V regarding preliminary findings
(date) Draft report to Region V
(03/92)
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F 5
appendix
NEIC
SAFETY PLAN
FOR
HAZARDOUS SUBSTANCES RESPONSES AND HELD INVESTIGATIONS
The OSHA Hazardous Waste Site Worker Standards (29 CFR 1910.120) and EPA protocols require
certain safety planning efforts prior to Field activities. The following format is aligned with thes e
requirements. Extensive training and certifications are required in addition to this plan
PROJECT: NEIC Reporting Code-
Project Coordinator: Date:
Branch Chief: Date: ;
On Scene Coordinator or Supervisor
Health and Safety Manager
Approval: Date:
DESCRIPTION OF ACTIVITY
If any of the following information is unavailable, mark HUAH; if covered in project plan, mark "PP".
Site Name:
Location and approximate size:
Description of the response activity and/or the job tasks to be performed:
Duration of the Planned Employee Activity:
Proposed Date of Beginning the Investigation:
Site Topography:
Site Accessibility by Air and Roads:
(03/92)
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F-6
HAZARDOUS SUBSTANCES AND HEALTH HAZARDS
INVOLVED OR SUSPECTED AT THE SITE
Fill in any information that u known or suspected
Areas of Concern Chemical and Identity of Substance
Physical Properties
Explostvity:
Radioactivity:
Oxygen Deficiency:
(e.g.. Confined Spaces)
Toxic Gases:
Skin/Eye Contact Hazards:
Heat Stress:
Pathways from site for hazardous substance dispersion:
WORK PLAN INSTRUCTIONS
A. Recommended Level of Protection: A B C D
Cartridge Type, if Level C:
Additional Safely Clothing/Equipment:
(03/92)
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3
Monitoring Equipment to be Used:
F-7
CONTRACTOR PERSONNEL:
Number and Skills
CONTRACTOR SAFETY CLOTHING/EQUIPMENT REQUIRED.
Have contractors received OSHA required training and certification?
(29CFR 1910.120)
Yes Not Required
(If "yes", copy of training certificate(s) must be obtained from contractor)
B. Field Investigation and Decontamination Procedures:
Decontamination Procedures (contaminated protective clothing, instruments, equipment, etc.):
Disposal Procedures (contaminated equipment, supplies, disposal items, washwater, etc.):
(03/92)
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F-8
IV. EMERGENCY CONTACTS
Hospital Phone No.:
Hospital Location:
EMT/Ambulance Phone No.:
Fire Assistance Phone No.:
NEIC Health and Safety Manager Steve Fletcher - 303/236-5111
FTS 776-51II
Radiation Assistance: Wayne Bliss, Director
Office of Radiation Programs
Las Vegas Facility (ORP-LVF)
702/798-2476
FTS 545-2476
(03/92)
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6
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SESSION 6
TOPIC: ADMINISTRATIVE ISSUES
Time: 30 minutes
PURPOSE • Respond to questions concerning administrative procedures
Note: This session is not long enough to cover all administrative
issues. Further, this session concentrates on federal
administrative issues; state employees should check with
their individual administrative officers to determine their
specific requirements. Nevertheless, this session is
generic enough to apply in most cases to both federal and
state inspectors.
Key Points • Anticipate administrative needs in advance and obtain the
proper forms, authorizations, and signatures, and meet other
requirements.
• An inspector can be held financially liable for unauthorized
purchases.
List OF visuals 6-1 Administrative Issues (Title Slide)
6-2 Administrative Issues
6-3 Administrative Issues
6-4 Procurement
6-5 Administrative Issues
6-6 Pay Issues
6-7 Administrative Issues
APRIL 2000
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Administrative Issues
ADMINISTRATIVE ISSUES
•Planning
• Procurement
• Travel & Reimbursement
¦Pay Administration
• Special Cautions
ADMINISTRATIVE ISSUES
¦ Anticipate administrative needs
• Obtain proper forms, authorizations &¦
signatures
* Advance planning a must, but
« Qimge m travel plms may be Decesury
c Unrnnrrpmrl pjjTjusa may be necesmy
-------
ADMINISTRATIVE ISSUES
PROCUREMENT
• Supplies (ice, sampling equipment, etc.)
¦ Document copies
¦ Photographic processing
¦ Shipping
¦ You may be held liable for unauthorized
purchases III
ADMINISTRATIVE ISSUES
¦ Cash advance
* Reservations
¦ Airliiies
• Hold
• Ccr
¦ Use of cash
¦ Comrilrtr travel voucfaen promptly
¦ Receipts
* Know your procedures
ADMINISTRATIVE ISSUES
PAY ISSUES
• Overtime or comp time for
« Work
• Tnvcl
e TfUUHj
¦ Special pay
" Know your procedures
2
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ADMINISTRATIVE ISSUES
¦ Use of Government
equipment:
• Can
° Telephones
° Computus, fax
copiers, etc
¦ Meals
• Airline benefits
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TOPIC:
SESSION 7
SOURCES OF INFORMATION
Time: 45 minutes
Purpose
Key Points
List of Visuals
List of Handouts
• Acquaint the participants with the wide range of information that is
available to the inspector before the inspection.
• Prior planning, including extensive review of all sources of information, is
crucial to the successful and professional accomplishment of an
inspection.
7-] Sources of Information (Title Slide)
7-2 Sources of Information (general)
7-3 Think Paper and Electronic
7-4 Federal, State, and Local Files (facility-specific)
7-5 Federal, State, and Local Files (continued)
7-6 Reconnaissance Visit
7-7 Media Program Databases
7-8 Compliance Databases
7-9 http.//es.epa.gov
7-10 IDEA
7-]] Envirofacts
7-12 Envirofacts
7-13 OTIS
7-14 OECA
7-15 Office of Compliance
7-16 EPA Inspector Information Exchange Web Site
7-16 NE1C
7-17 NETI
7-18 NEIC Library
7-19 Commercial Information Sources
7-20 RAIN home page
7-1 Sources of Information
7-2 OTIS and other information based Web Sites
7-3 New EPA Inspector Information Exchange Web Site
JULY 2000
-------
Sources
of
Information
Sources of Information
(general)
1
• Statute and regulation publications
¦ Policies, data, and guidance from all
government levels (incl. cross-
agency)
¦ Case histories and precedent
(dockets)
* Division libraries and central filings
i J
¦ Trade associations
and
Electronic
1
-------
Federal, State, and Local Files
(facility^pecific)
¦ Permits, applications, exemptions, waivers
¦ Process diagrams, waste stream flow charts,
and facility maps
¦ Self-monitonng data, records, and reports
o including annual and per •incident reports,
manifests
* Prior inspection reports
o Including cross-program issues
Federal, State, and Local Files
(facility-specific) (continued)
¦ QA documentation
° Prior sampling test results
° Lab certification
¦ Enforcement documents
* Facility responses to enforcement actions
¦ Citizen complaints
Reconnaissance Visit
r
* Done to increase on-site inspection
° Especially if facility is very complex; or
• Tbcrc is not enough info m files
¦ Inspector may meet with ownenfopentor far
logistical planning
¦ But not used with an unannoin
-------
Media ProgramDatabases
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opcs IL^
• RCRAlnfo P V
J
¦ 1 Rlis
¦ CERCL1S
11
Compliance Databases
• IDEA
" ENVIROFACTS
» OTIS
" Sector Facility Indexing
http://es.epa.gov/
3
-------
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6
-------
COMMERCIAL INFORMATION
SOURCES
• AutoTrak
¦LEX1S/NEX1S
• CBDlnfo
¦ STN
•DIALOG
•TOMES
• Dun & Bradstreel
• Westlaw
iiw a*
i
1
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-------
PUBLICLY AVAILABLE EX' L INFORMATION SYSTEMS
CURRENTLY. jSFBLE BY NEIC
HAND
System
Description
Application
Chemical Information
System (CIS)
Colorado Alliance of
Research Libraries
(CARL)
DataTimes
Knight-Ridder Information
Services, Inc.
Dun & Brad street
Groundwater On-Line
(GWOL)
NEXIS/LEXIS
The CIS is a collection of scientific and regulatory
databases containing numeric, textual, and some
bibliographic information in the areas of toxicology,
environment, regulations, spectroscopy, and chemical
and physical properties.
The CARL system includes the catalogs of the member
libraries, an index of more than f0,000 periodicals, a
full-text encyclopedia, Choice book reviews, and a
bibliography of GPO publications.
DataTime9 provides on-line access to numerous full-text
databases, including newspapers, wire services, and Dow
Jones News/Retrieval.
The DIALOG system contains more than 330 databases
covering a variety of disciplines: science, technology,
engineering, social sciences, business, and economics.
"Hie databases contain more than 120,000,000 records
and are regularly updated to provide the most recent
information.
Dun & Bradstreet, a credit-reporting firm, provides
business information reports tor privately arid publicly
owned companies and government activity Teports that
list federal contracts, grants, fines, and debarments for
specific companies.
The National Groundwater Information Center database
is a bibliographic database containing references to
materials on nydrogeology and water well technology,
with emphasis on reports or projects sponsored by EPA.
NEXIS/LEXIS contains the full text of more than 600
business and general news files, including the
Washington Post and New York Times. Statutory and
case law are provided for computer-aided legal research.
NEIC uses the CIS to locate mass spectral
information; environmental fate information;
formulation ingredients for commercially available
products, such as pesticides; and waste disposal
methods for hazardous substances.
CARL is searched by NEIC staff for general
reference, to locate books, and to identify articles and
documents.
DataTimes is a source of national environmental
news. Newspaper databases from all regions are
updated daily.
NEIC uses the DIALOG databases to obtain: (1)
expert witness information, including biographies,
publications, and congressional testimony; (2) up-to-
date pollution control technology for hazardous
waste, air, and water; and (3) business information
such as corporate officers, subsidiaries, and line of
business.
NEIC uses the Dun & Bradstreet system to locate
corporate information, such as business done by the
company, company history, financial condition,
subsidiaries, and corporate officers for privately held
companies.
NEIC accesses GWOL to locate publications on
groundwater topics and to verify or locate
groundwater experts.
NEIC uses NEXIS/LEXIS to keep informed of the
latest EPA and environmental news stories and to
track the corporate and financial status of U.S.
businesses involved in environmental litigation.
7
MARCH 2000
-------
PUBLICLY AVAILABLE EXTT \L INFORMATION SYSTEMS
CURRENTLY AC jSIBLEBYNEIC
HANDOr I
System
Description
Application
National Library of
Medicine (NLM)
Scientific and Technical
Information Network
(STN)
WESTLAW
The National Library of Medicine system contains more
than S million references to journal articles and books in
the health sciences published since 1965.
The STN system contains databases covering chemistry,
science, and engineering that are regularly updated to
provide the most recent information. STN has strong
coverage of European and Japanese scientific databases.
The WESTLAW system contains legal information,
including the full text of cases from the Supreme Court,
U.S. courts of appeals, U.S. district courts, and state
courts. It contains Shepards' Citations, regulatory
information from the Code of Federal Regulations,
Federal Register, and U.S. Code and expert witness
information from the Forensic Services Directory.
NEIC uses the NLM system to obtain: (I)
information about toxicity and environmental health
effects for individual chemicals or groups of
chemicals, (2) physical and chemical properties of
specific compounds, (3) analytical methodology
references, and (4) carcinogenic bioassay information
from the National Cancer Institute.
NEIC uses the STN databases to obtain: (1)
chemical structures and synonyms for a chemical
compound, (2) analytical methods and techniques,
and (3) toxicity of a chemical compound.
NEIC can acquire source information and location,
service areas, geographic areas, and historical
information. Information on noncompliance and
enforcement actions also can be obtained.
NEIC uses WESTLAW to identify precedent cases,
to locate all cases decided by a certain judge or all
cases represented by a certain attorney, and to locate
possible expert witnesses..
MARCH
-------
CJTtS tixni
URLrhttp:/intranet.epa.gov/oeca/oc/eptdd/teb/otis
07/11/2000 12:36 PV
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Welcome to OTIS
Subscribe to
OTIS Update
News
Online
Targeting
Bivtromappar For
Complanc* Analysis
3rd Annual National Targeting Workshop
Presentation files will be linked soon.
Information
System
What's New
Search
Welcome to the Online Targeting information System (OTIS)' This website is
maintained by the Enforcement Planning, Targeting, and Data Division within
the Office of Compliance to assist Regional and headquarters staff in using
information systems to target for inspections, enforcement pnonties, and compliance activities.
Browse the following list for key tools that are available on the site, or click on the tabs above to find
more information about targeting pertaining to particular areas of interest (e.g., Clean Water Act).
Please note that data on this site are for U.S. EPA use only, and are not available on the public
Internet. Data on the site are from the program databases via the Integrated Data for Enforcement
Analysis (IDEA) system. Your comments are welcome and can be sent to
barrette .michael @ epa.gov.
Available OTIS Tools
H
IDEA Web Query
The IDEA Web query provides IDEA functionality on a web browser and generates compliance data in real-time based on
selections including facility name, sector, compliance status, and enforcement history Oata are available at the facility level
that allow users to view information about the nature ol violations that occurred and to rank facilities for inspection or
enforcement priority Each media currently displays a separate query interface (Water-CWA. Air-CAA, and RCRA) Ongoing
enhancements are planned tor the IDEA Web Query tools
SNC Tracker On-line Search
The SNC Tracker provides a quick way to view tacMes in a state or Region that are currently listed as SNC (or HPV) The
interface Iooks at me most receni information in the IDEA system, and provides either a single media or cross media result
based upon selections of CAA (AFS), CWA (PCS), and RCRA (RCRIS) data The site can be searched by state. Region, or
environmental program of concern and may be used to plan multimedia inspections or cases against facilities with multimedia
compliance issues This feature replaces the capability of me CWA- and MultiMedia SNC Trackers as well as the planned
CAA-HPV and RCRA-SNC Trackers
Get Compliance Report
IDEA oata are available in a web browser by clicking the *Get Compliance Report' button m the top nght comer of the OTIS
screen Tnis feature lets you specrfy a facility name or permit number and generate a detailed report including data from AFS.
RCRIS. PCS and TRIS New features include data on TRi releases by chemical and 5-year option tor displaying enforcement
actions and inspections
BETA Version OTIS Tools
EnviroMapper for Compliance Analysis
The newest EnviroMapper site gives users a dynamic way to use maps to target facilities by compliance status and/or tme
since last inspected This site will allow you to map RCRA, Clean Air Act (CAA). and Clean Water Act (CWA) facilities in a
given geographic area (Beta version for comment • please provide feedback)
Geographic Analysis Tool
Use this tool to assess environmental conditions by county, and check to see whether enforcement presence is high or low by
county The tool is designed to identity geographic areas that may be npe tor more compliance monitoring Sort county
rankings by media, or multimedia, and use the website to provide color maps This product is the result of a EPA/Regional
Workgroup which supported the MOA process (Beta version for comment • data pulls completed in October, 1996)
Sector Analysis Tool
Which sectors in your Region or state have the highest noncompliance rates or pollutant releases'' Use this tool to view
rankings that show inspection coverage, violation rates, and emission* data for 113 sectors Data was used to support FY'OO
MOA national sector pnonties (Beta version for comment - data pulls completed in October, 1998).
07/11/2000 12:56 PM
-------
Coming Soon to OTIS
The Targeting and Evaluation Branch is currently developing a new set of capabilities for OTIS thai will be launched in
October. 2000 (Version 3) Please contact Michael Barretie it you would like to provide input dunng the process of defining
new features
Leave OTIS to Search Other Internet Sites
EPA Sector Facility Indexing Proiect
Provides detailed compliance and release data tor 5 industry sectors
EPA EnviroFacts Warehouse
Allows basic searcning tor facility-level information in multiple databases
TRI Explorer
Provides web-based query and analysis (unctions tor the 199B Toxics Release Inventory data set
RTK Net
Provides data searching from multiple EPA systems
EPA Emergency Response Nolificalipn System (ERNS^
View information on reported spills
AIRSWeb
View air pollutant release data
ORE Enforcement Alert
is a new informational newsletter published by the Office of Regulatory Enforcement that in forms and educates the public and
regulated community of important environmental enforcement issues, recent 1 rends and significant enforcement actions
EPA Surf vour Watershed
Office of Water Website lists information on watershed quality
Environmental Defense Fund Scorecard «4|
Provides geographical search capabilities focused on TRI release data
Secunties and Exchange Commission (EDGAR! ptrrp^*^l
Use this site to find corporate disclosures of environmental liability information, and to vertty that EPA sanctions over
Si00.000 nave been reponed to SEC
FreeEDGAR
Site allows you to perform text searches into SEC documents to look (or corporate information Provides more functionality
than the Security and Exchange Commission site
OPPT Environmental Indicators Model
View EPA environmental indicator oata aggregated nationally or by state, county or zip code based upon the TRi-based risk
screening model that OECA has adopted for enforcement targeting
OECA Data Systems and Models
Provides descnptions and links to searchable databases and models used by OECA
EPA EnviroMapoer
Maps several types ol environmental information, including onnking water, toxic and air releases, hazardous waste, water
discharge permits, and Supertund sites
National Atlas ol the United States
Interactive maps with environmental, biological, geological and demographic layers
OSHA Statistics and Data
Access query tools that locate OSHA inspections conducted witin a particular establishment or within a particular industry
07/11/2000 12:56 PM
-------
group
Leave OTIS for Regional Enforcement, Compliance, or Targeting Data on the Internet
Region 1 Data and Software
Proviaes TRI data tor New England States
Region 2 Geographic Information Systems
Information on Regional GIS projects, data and software
Reoion 3 Databases and Software
Provioes linics to searchable databases and environmental maps
Region 4 Geographic Information Systems and Information Resources
Regional databases and GIS applications
Region 5 Enforcement Action Database
Regional enforcements actions tor FY 2000 by name, state, or statute
Region 5 Enforcement Reports
Summary of Regional enforcement activity by fiscal year (1992-1998) or type (SEP. Compliance Orders, penalties, or trends)
Region 6 Comparative Risk Publications
Contains Regional analyses covering human Health Risk, Environmental Justice Index, Comparative Risk Report, and
Federal Facilities Risk Index, plus links to national sues
Region 8 Geographic Information Systems Data
Inventory ol GIS web and mapping links plus (inks to Region 8 state and Federal environmental data sites
Leave OTIS for State Enforcement, Compliance, or Targeting Data on the Internet
California Geotracker
Geographic Information System with online access lo regulatory data about underground fuel tanks, pipelines ami drinking
water systems in me State of California
Pennsylvania EFACTS
(Environment, Faality. Application, Compliance Tracking System)
If you would like us to add a link to this site, please send a message to rover ehzabelh&eoa. nnv
What'# New EPAgM/orii Search Contact Ue TEBHonw OECAHome 1
Site Map Feedback Offices Regions EPA Home Envirolente j
- ~ __ '•
Last Updated May ts. 2000
URL http^/intranet.epa gov/oeca/oc/otis/otis_welcome html
07/11/2000 12:56 PM
-------
p Q A Umtrt S)xn
EnwronmwitalProtection
WLin Apwr,
Office of Enforcement
and Compliance Assurance
About IDEA
Getting Started
Data Sources
Pulldlng Queries
IDEA Reports
User Documentation
Support Services
FAQ
The Integrated Data for Enforcement
Analysis system (IDEA) is a
comprehensive single-source of
environmental performance on
regulated facilities within EPA. With
IDEA you can obtain a
comprehensive historical profile of
inspections, enforcement actions,
penalties assessed, toxic chemicals
released, and emergency hazardous
spills for any EPA regulated facility.
This single point of access provides
information from the Agency's Air,
Water, Hazardous Waste, Toxic
Chemical Release Inventory, and Emergency Response Notification
Systems. IDEA can be used to-
• produce the compliance history on a specific facility,
• retneve data for performing multimedia analysis of regulated
facilities,
• identify a group of facilities that meet a user's specific cnteria; and
• produce aggregated data on selected industnes.
IDEA Home OECA Home EPA Home Envlro$en»e
Search 5lteMap What's New7 Contact Us
Last Updated April 13, 2000
URL: http.//www epa gov/oeca/idea/
07/11/2000 1:08 PM
-------
AboutIPEA
Getting Started
Pata Sources
Building Queries
IDEA Report®
Ueer Poeumentation
Support Services
FAQ
vvEPA
UnrtfO Enwvnnwnul
Protectee Aowj
Office of Enforcement
and Compliance Assurance
Getting Started
To gain access to IDEA, all users must have a user ID and a way to
access the EPA mainframe. Steps for getting started vary according to
the type of user.
Select the user group that best describes you to learn more about
gaining access to IDEA.
• EPA Employee
• Federal or State Employee
• Member of the Public
IDEA Home OECA Home EPA Home Envfro$enee
Search Slt« Map What'eNew? Contact Ua
Last Updated: April 13, 2000
URL- http://www.epa gov/oeca/idea/stan.hunl
07/11/2000 1:08 PM
-------
c/EPA
llnwd St»M Divurrximxujl
?tol«tton i
-------
v>EPA
Uniufl Jam tnvronrrwnul
Protfeoon Htm-,
Office of Enforcement
and Compliance Assurance
M3il
About IDEA
Getting Started
Data Sources
Building Queries
IDEA Reports
User Documentation
Support Services
FAQ
Getting Started
State and Other Federal Agency Employees
These instructions are specifically for State or other Federal Agencies.
Before you get started, you must:
1. Obtain a mainframe user ID and account.
2. Determine which access method and interface is appropriate for
your use.
3. Determine if vou qualify for state-sensitive access (state-sensitive
access allows you access to more data, for example, the
Occupational Safety and Health Administration (OSHA) system).
Once you have selected and installed the appropnate IDEA software, you
must have a mainframe user ID. Please note if you already have a
mainframe user ID and password there are no additional requirements
for accessing IDEA and/or IDEAWin as any valid mainframe user
ID/account will work. If you do not have an ID you must obtain one by
following instructions for obtaining a mainframe user ID (see link at top of
page).
Other Federal Agencies and State Environmental Enforcement
Personnel may qualify for state enforcement data access. To decide
whether or not you qualify for state enforcement data access, read the
instructions for determining if you qualify for access (see link at top of
page).
IDEA Home OECA Home EPA Home Env1ro$ense
Search Site Map What's New? Contact Us
Last Updated. April 13, 2000
URL- hup://www.epa.gov/oeca/idea/siate.html
07/11/2000 1:09 PM
-------
Envirofacts
Text Version
IN THE NEWS
AWARDS
&EPA
UmadSm
biwuiiaiaf Huutuun Agncy
Warehouse
A single point of access to select U S EPA environmental data
Read about the environmental databases in Envirofacts.
Select an Overview
Overview!of Available Data Yi
Query the database and generate reports.
Select a Query Form
Generate! Reports from Data J
Produce maps of environmental information.
Select a Mapping Tool
. V.Maps On Demand „ ^
Facility Linkage Application
Envirofacts Warehouse Website
URL http.//intranet.epa.fov/enviro
This page was updated June 07, 2000
URL:http:/intranet.epa.gov/enviro
-------
RCRAInfo Design Team Updates
EPA's Home Page
OSW Partnership Web
Tuesday, July 11,2000
What Can You Find on This Site?
On this site you can find all of the late-breaking news concerning the RCRAInfo
project, including manuals, guides, and presentations
Work continues as we move the Resource Conservation and Recovery
Information System (RCRIS) and the Biennial Reporting System (BRS) from a
mainframe-based FOCUS database to a web-enabled Oracle platform
RCRAInfo are y
"point and click'1
General Documentation
Who is on the Design Team7 05/23/2000
What is the RCRIS Proiect Scope?
What is the BRS Proiect Scope?
The RCRAInfo High Level Design
RCRAInfo High Level Design - Response to Comments
Cover Memo for the Response to Comments
RCRAInfo National Training Materials
Invitation to RCRAInfo Training 05/23/2000
Draft Agenda 05/23/2000
Registration Forms - PDF and WordPerfect 05/23/2000
Hotel Logistics 05/23/2000
Technical Documentation
Structure Charts
SeClJHty 05/25/2000
Upd Handler (Part 1. Part 2) 07/10/2000
Permitting 07/02/2000
Corrective Action 07/02/2000
CM&E (Pan 1. Part 2) 07/02/2000
National Biennial Report (Part 1. Part 2. Part 3> 07/02/2000
Table Lists (English version of the structure charts)
Security 05/25/2000
Hanger 05/25/2000
Permitting 05/25/2000
Corrective Action 06/2B/2000
CM&E 06/28/2000
National Biennial Report 06/28/2000
RCRIS / BRS to RCRAInfo Crosswalks
Handler 05/19/2000
Permitting 05/19/2000
Corrective Action 05/19/2000
CM&E 06/28/2000
National Biennial Report 06/28/2000
Guides. Guidance, and Manuals
Translator Guide - draft version 3 02/09/2000
RCRAInfo Final File Specification Guide for 1999 Hazardous Waste 11/1999
Report Submissions (Summary of Changes)
URLrhttp://www.epa.gov/oswfiles/rcrainfo
07/11/2000 12.39 PM
-------
RCRAInfo User Acceptance Testing GuidP
The Placemats - Legal Status. Operating Status, and Universes 05/25/2000
Cpnversion Issues for RCRIS to RCRAInfo Final Data Conversion
Survey: PDF or WordPerfect
Reporting in RCRAInfo
Reports List 05/24/2000
Functional Specifications for RCRAInfo National Reports 06/08/2000
Building RCRAInfo WPh Rpnorts
11999 Biennial Reporting Cycle
1999 Biennial Report Implementation Schedule 05/23/2000
RCRAInfo Status and Plans
RCRIS to RCRAInfo Final Data Conversion Schedule 07/02/2000
Bnefing for the ASTSWMO Conference 04/27/1999
Briefing for the Regional Branch Chiefs Meeting 04/29/1999
RCRAInfo: The Paradigm Shifts. A presentation by Design Team members
Steve Cobb (AL) and Mira Neumiller (CO)
New Bnefing for the ASTSWMO Conference 07/10/2000
Submit comments, suggestions, or questions about this site to the RCRAInfo HelpDesk
Unless otherwise noted, all documentation contained on ttiis site is maintained in Adobe Acrobats PDF format You ca
[ viewer at Abode's web site - httpV/www.adobe.com EPA personnel may already have tfiis software installed on their P<
available through their local LANs Due to the size of some of these files. It is recommended that you download the doc
rather than trying to read them on-line
07/11/2000 12:39 PIv
-------
TEXT VERSION
OCEFT Main Page
^1.4
O E C A
murffifaiBMl ad
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HEICHonwffigf
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HEI^rary
|pM$emns
nr
"5-EPA
National
Enforcement
Investigations
Center
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Resources
Field
Activities**^
About NEIC
Forensics
Laboratory
Search
EPA Home
Stteltop OECA Feedback j
Last Modified Fnday, January 28. 2000 15 09 37
Page maintained by Kimberty O'Neill. GCI
httpy/www epa gov/oeca/oceft/neic/
URL:http://es.epa.gov/oeca/oceft/neic
07/11/2000 12-40 PM
-------
NEIC Library
Web Sites for Inspectors
EPA/Environment Sites
NEIC Weh Site
http://www.epa.gov/oeca/oceft/neic
Information ahout NEIC* background and organization. Link* to enforcement publications and
relevant Internet information.
EPA Wei Site
kttp-.//ww .epa.gov/
Contain! hasie information ahout the EPA, pre** releases, offices, program*, databases and a calender of event*.
EPA Intranet Site
http://1ntranet.ep4.gov/agcy1ntr
Internal information for EPA, includes technical document*.
Envirofacts
http:// ww.epa. gov/ doc»/enviro/h tml/ef_home.html/
K U.S EPA relational database that integrate* data from four major EPA program ryitem*. permit compliance
item (PCS),CERCLIS, TRIS. RCRIS
Environmental Information on the Internet
http:// spot. Colorado .eduZ—johem/envnci .htm
This ute it comprehensive listing of environmental information sites compiled hy Peggy Johe of Univenity
of Colorado- Boulder.
Regional Associations Information Network
http://ww.epa .gov/ oeca/neti/ ranuntr.html
An information resource designed for environmental regulatory and enforcement professionals, The site ic
password protected and is for use hy government personnel only. You can sign up on the weh. 1
7TN2000- TTN Bulletin Bn,rrl
http://ttnwww.rtpnc.epa.gov/
^ch interface for TTNBBS, includes AIRS, CHIEF, CAAA, NATICH BBS and more.
Internet Ltafltt Stnti-009
"reaud by K. O 'Neill, CCI
W8
1
-------
Government/Regulatory Information
CFR-Titlc 40
http.//ww.tpt.gov/docs/epacfr4Q/chapt-1 .info
The CFR in PDF format. Use Adobe Acrobat Reader to view and print.
FedWorld
li ttp ://www. fedworl d .g ov/
A aearchable database of government agency vet «itet, as well u linlu to a variety of sites and databases.
Fed Law
http://www.legal.gsa.gov
References for people conducting Federal legal researck.
OSHA
http://ww.oika-ilc.gov/
Information on OSHA standards, technical links and training.
Thomas
http.7/thomas .loc.gov
Congressional information on the well, including the text and legislative histories of bills from the 103-105
Congresses.
People, Company and Place Finders
Fourl 1
http://www.Fourl l.com
Find email addresses.
MapQuest
http://www.mapquert.com
Allows you to locate an address by generating a street map.
Switchboard
http://www.switcktoard.com
Find listed phone numbers and addresses by name, city or state.
Chemical
Chemfinder
h ttp ://ckemfinder .camsoft.com
Searches various environmental databases for chemicals by name, CAS number, molecular weight,
and formula.
Vermont SIRI MSDS
http://ha2l.siri.0rg/msdsVermont SIRI MSDS
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Sector Notebook Project
Nonferrous Metals
This report is one in a series of volumes published by the U.S. Environmental
Protection Agency (EPA) to provide information of general interest regarding
environmental issues associated with specific industrial sectors. The documents were
developed under contract by Abt Associates (Cambridge, MA), and Booz-Allen &
Hamilton, Inc. (McLean, VA). This publication may be purchased from the
Superintendent of Documents, U.S Government Printing Office. A listing of available
Sector Notebooks and document numbers is included on the following page
All telephone orders should be directed to:
Superintendent of Documents
U.S. Government Printing Office
Washington, DC 20402
(202) 512-1800
FAX (202) 512-2250
8:00 a.m. to 4:30 p.m., EST, M-F
Using the fonn provided at the end of this document, all mail orders should be
directed to:
U.S. Government Printing Office
P.O. Box 371954
Pittsburgh, PA 15250-7954
Complimentary volumes are available to certain groups or subscribers, such as public
and academic libraries, Federal, State, local, and foreign governments, and the media.
For further information, and for answers to questions pertaining to these documents,
please refer to the contact names and numbers provided within this volume.
Electronic versions of all Sector Notebooks are available free of charge at the following
web address: www.epa.gov/oeca/sector. Direct technical questions to the "Feedback-
button at the bottom of the web page.
Cover photograph courtesy of Reynolds Alummum Recycling Company, Richmond, Virginia.
Special thanks to Terry Olbrysh for providing photographs.
SIC Codes 333-334
September 1995
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07/11/2000 12.32 PM
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We are ir ted in your
comments, .suggestions to
make the EPA Inspector web site a
better one. Please fekl.free to use
the on-line comment box to make
your voice heardr You may also
contact Rafael Sanchez,
Sanchez.rafael @epa.gov, for
additional Information.
EPA Inspector \ te
URL:
intranetepa.gov/oeca/oc/metd/
Inspector/
New EPA Inspector
Information Exchange
Web Site
r
&
O E C A
Olllce el Erhmnwel eid
umipiiimMviiHu
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The EPA Inspector Web Site is a
single comprehensive Intranet
resource Tor EPA Inspectors where
relevant, up-to-date Information
about inspections, heafth & safety,
policy & regulatory Issues}
technologies, compliance assistance
and training can be quickly found.
The Inspector web site has been
created as a pilot project by the
OfTice of Compliance as way to foster
and facilitate communication In the
Inspector community.
The pilot project will run for
approximately nine months. During
that time we will evaluate the web site
for usage, content, number of files
downloaded and In general, user
involvement. The results of the
evaluation process will help us
Identify new avenues and
opportunities to better provide
compliance assistance to EPA
inspectors. Depending on the
feedback we receive from the users
we will determine whether to continue
with this effort or try something else.
We are committed to provide you
with the most up-to-date and relevant
Information about inspectors and
Inspection activities. With this in
view, the Inspector web site has
gathered a wealth of information to
help you In your Job as an EPA
inspector. As you navigate
throughout the web site, you will find
a smorgasbord of Inspector and
inspection-related information and
useful EPA and external links.
To foster timely communication, we
have created a message board for you
to post, respond and search for
messages about Inspectors and
inspection-related Issues. In this way,
information about inspections can be
shared with your colleagues in a
timely and expeditious manner.
So far we have created the following
discussion topic areas (Other
discussion forum can be created as
required):
/ Matters of Urgency
~ General Issues About Inspections
~ Emerging Non-Compliance Trends
~ Compliance Issues about Air
~ Compliance Issues about Water
~ Compliance Issues about RCRA
~ Small programs & other
Compliance Issues
/ EPA ORDER 3500.1
~ Policy and Regulatory Issues
/ Health and Safety
~ Training
Finally, to help you find fellow
inspectors in a particular area of
expertise we have created an
interactive EPA Inspector Directory.
The directory will allow you to pull
information about EPA inspectors on
the fly. The EPA directory is a user-
friendly database where queries
about inspector credentials and
location can be made. The EPA
directory can be updated by the user
as often as required.
Interested? Then bookmark the
following URL:
intranet.epa.gov/oeca/oc/metd/
inspector/
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SESSION 8
TOPIC: ENTRY, OPENING CONFERENCE AND SITE INSPECTION
Time: 60 minutes
PURPOSE • Explain the extent and limits of EPA's authority to enter and inspect
facilities
• Explain EPA policy and practice governing consensual entry
• Explain procedures for proper, lawful entry
• Provide guidance for handling sensitive situations regarding entry
• Discuss the role of the inspector tn securing a warrant and conducting an
inspection under a warrant.
• Discuss the issues and procedures to be covered during site entiy.
• Discuss the issues to be covered during an opening conference.
• Discuss the issues to be covered during the site inspection
Provide suggestions regarding inspection techniques.
Key Points • It is EPA policy to obtain a warrant when the owner has denied consent to
entry.
• State, Local, and Tribal policy on entry and warrants may be different;
discuss
The opening conference is held to advise personnel of the facility of the
objectives of the inspection and to discuss and arrange for logistics and
scheduling of inspection activities
• The general site tour provides inspection team members an orientation and
identifies and verifies activities that require further evaluation.
List of Visuals
8-1 Entry, Opening Conference and Site Inspection (Title Slide)
8-2 Entry, Opening Conference and Site Inspection—Session Overview
8-3 Entry, Opening Conference and Site Inspection (Summary of Federal
Environmental Acts)
8-4 - 8-9 Entry, Opening Conference and Site Inspection—Entry
8-10-8-12 Entry, Opening Conference and Site Inspection—Entry
8-13-8-19 Entry, Opening Conference and Site Inspection—Opening
Conference
8-20 - 8-21 Entry, Opening Conference and Site Inspection—Site Inspection
List of Handouts
8-1 Summary of Federal Environmental Acts
MARCH 2000
-------
Entry, Opening Conference,
and Site Inspection
Entry, Opening Conference,
and Site Inspection—Session Overview
• Entry procedures
° Summary of statutes
° Legal bases or authority
° Warrants
• General "How To"
procedures for
° Site entry
° The opening conference
° The site tour
Entry, Opening Conference,
and Site Inspection
Summary of Federal Environmental Acts
/
-------
Entry, Opening Conference and Site
Inspection —Entry
Entry, Opening Conference and Site
Inspection —Entry
» Consensual entry
Entry, Opening Conference and Site
Inspection —Entry
• Consensual entry
¦ Absence of express
denial - consent
2
-------
Entry, Opening Conference and Site
Inspection —Entry
1 • Denial of entry
I D EPA policy is 10
I obtain a warrant
1.1
Entry, Opening Conference and Site
Inspection —Entry
Warrantless entry
0 Emergencies
0 Heavily regulated
industries
0 "Open fields" and "in
plain view"
Entry, Opening Conference and
Site Inspection—Entry
¦ If denied entry
° Be tactful
° Use reason and logic
° Record observations
» DO NOT THREATEN
0 Contact supervisor
»•
3
-------
Entry, Opening Conference and Site
Inspection—Entry
¦ Warrants
0 When facility has denied access
° If full consent is withdrawn during inspection
° May be done in advance of inspection
0 Inspector and attorneys work as team
Entry, Opening Conference and Site
Inspection—Entry
• Warrants
0 Need to identify specific information needs
° Limits inspection to specifics ui warrant
¦ Other tools for gathering information
Entry, Opening Conference and Site
Inspection—Entry
• Proper site entry procedures
° Drive-by and ofT-site observations
• Lock for obvious concerns
• Fvnilunxe youraclf wnh layout
0 Normal working hours
4
-------
Entry, Opening Conference and Site
Inspection—Entry
° Use main gate or
entry
0 Contact person in
charge
* Plint manager environmental
manager owner etc
0 Identify yourself with
your credentials
Entry, Opening Conference and
Site Inspection—Opening Conference
¦ After initial site entry
¦ Introduction and
credentials
¦ Explain
° Authority
0 Purpose
0 Scope of inspection
° Estimated tune to
complete
Entry, Opening Conference and
Site Inspection—Opening Conference
Discuss Confidential
Business Information
(CB1)
° Their right to claim
CBI
• Use good proemition
i Provide paperwork
Identify special
safety concerns
-------
Entry, Opening Conference and
Site Inspection—Opening Conference
Explain
¦Documentation methods
° Notes
° Copies
E Photographs
D Samples, etc
Entry, Opening Conference and
Site Inspection—Opening Conference
Explain'
•Inspection process
D Facility processes
° Records review
" Site tour
° Closing conference
• Summary of finding*
Entry, Opening Conference and
Site Inspection—Opening Conference
¦ Start of main information collection
° General operations overview
» Obtain map
¦ Orient vouneV with North
° Identification of regulated areas
° ldentificaiion of recent changes
° Review of specific records
6
-------
Entry, Opening Conference and
Site inspection—Opening Conference
• Recommend process
based approach
¦ Raw materials m
11 Detailed
understanding of
process operations
° Product out
0 Waste management
units
a
Entry, Opening Conference and
Site Inspection—Opening Conference
Develop "Must See" list
¦ Key process operations
¦ Waste management areas
¦ Areas with past violations
¦ Areas with suspected violations
Entry, Opening Conference
and Site Inspection—Site Inspection
• Detailed "on-the-ground" In
inspection—Directed By You ! I
• Follow process flow
¦ Evaluate compliance with mediaj
regulations
• Evaluate "Must See" items
• Watch for newly regulated units
7
-------
Entry, Opening Conference
and Site Inspection—Site Inspection
• Review records and
documents
¦ Identify follow-up activities
° Interviews
° Sampling locations
" Additional inspection needs
¦ Document findings
0 Names, notes, photos,
samples, etc
8
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SUMMARY OF FEDERAL I JNMENTAL ACTS REGARDING
RIGHT OF ENTRY, INSPEL.. «ONS, SAMPLING, TESTING, ETC.
pill
I'feep
syaSMSSSJefts
iiiggi
IPfPI
is!
Clean Water
Act/308(a)
Yes, authorized
by Administrator
Required
Not required
Yes (effluents that the
owner is required to
sample)
Yes
Not
required
Not
required
Not
required
FIFRA/8(b)
(books &
records)
Yes, designated
by Administrator
Required
Written notice
required, with reason
and suspected
violation noted
No
Yes
N/A
N/A
N/A
9(a) (inspections
of
establishments)
Yes, designated
by Administrator
Required
Written notice
required, with reasons
for inspection
Yes
See 8
Required, if
requested
Required
Required
jromptly
Clean Air
Act/I 14(a)
Yes, authorized
by Administrator
Required
Not required, except
notification of the
state for SIP sources
Yes
Yes
Not
required
Not
required
Not
required
RCRA/3007(a)
9005(a)
Yes, designated
by Administrator
Not required
Not required
Yes
Yes
Required, if
requested
Required
Required
promptly
SDWA/1445(b)
Yes, designated
by Administrator
Required
Written notice
required; also must
notify state, with
reasons for entry, if
state has primary
enforcement
responsibility
Yes
Yes
Not
Required
Not
required
Not
required
TSCA/1 l(a,b)
Yes, designated
by Administrator
Required
Written notice
required
(The act does not mention
samples or sampling in
this section, but it does
state that an inspection
shall extend to all things
within the premises of
conveyance)
Yes
N/A
N/A
N/A
CERLC A/104
Yes, designated
by President
Not required
Not required
Yes
Yes
Required, if
request
Required
Required
promptly
1
MARCH2
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9
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SESSION 9
TOPIC: EVIDENCE
Time: 60 minutes
Purpose
Key Points
List of Visuals
List of Handouts
• Introduce the rules of evidence and their relevance to the activities of the
inspector.
• Provide guidance on documenting evidence to help ensure its admissibility
in a court proceeding.
• Present procedures for recording and documenting observations
• Present tips for improving techniques
• Many of the procedures being taught in this course are based on
considerations related to evidence, they are designed to ensure the
admissibility of information collected during an inspection and to enable
the inspector to provide credible testimony in a court proceeding.
Photographs are excellent evidence.
9-1 Evidence (Title Slide)
9-2 Evidence
9-3 Evidence Definition
9-4 Types of Evidence
9-5 FRE 901 Authentication and Identification
9-6 FRE 401: Definition of "Relevant Evidence"
9-7 FRE 602: Lack of Personal Knowledge
9-8 "Who Cares If..."
9-9 Collection Conditions and Surroundings
9-10 General Identity and Sameness
9-11 Precautions To Ensure Identity
9-12 Present Conditions That Vary
9-13 Representativeness of Item
9-14 Connecting the Chain of Custody
9-15 Inspector's Written Documentation
9-16 FRE 612. Writing Used To Refresh Memory
9-17 FRE 803 Hearsay Exceptions 803(5): Recorded Recollection
9-18 FRE 803 Hearsay Exceptions 803(6). Records of Regularly
Conducted Activity
9-19 Chain of Custody
9-20 Evidence Is in "Custody" If...
9-21 Basic Chain-of-Custody Procedures
9-22 FRE 406: Habit, Routine Practice
9-23 Photographs/Video
None
MARCH 2000
-------
Evidence
Evidence
Session Overview
• Identifying evidence
¦ Documenting evidence
¦ Ensuring admissibility
*.1
Evidence Definition
"Any type of proof legally
presented at a trial .. ..for the purpose
of inducing belief in the minds of the
court or jury "
1
-------
Types of Evidence
¦Testimonial
¦Real
"Documentary
¦Demonstrative
FRE901: Authentication and
Identification
"... a condition precedent to admissibility is
satisfied by evidence sufficient to support a
finding that the matter in question is what its
proponent claims"
FRE 401: Definition of "Relevant
Evidence"
"... evidence having any tendency to make the
existence of any fact that is of consequence
to the determination of the action more
probable or less probable than it would be
without the evidence."
2
-------
FRE 602: Lack of Personal
Knowledge
"A witness may not testify to a matter unless
evidence is introduced sufficient to support a
finding that the witness has personal knowledge
of the matter. Evidence to prove personal
knowledge may, but need not, consist of the
witness's own testimony
*7
"Who Cares If..."
Who cares if what you are holding (in your
hand in court) is contaminated "gunk"
unless you can show that particular "gunk"
came from the particular sue involved in
this case, not from somewhere else0
11!
Collection Conditions
and Surroundings
• What activities were performed at the site''
• Why the sample was taken9
¦ How the item was discovered9
¦ What physical items were identified in the
immediate vicinity0
Aids Notations in field logbook
Photographs of area and exact
location of sample
3
-------
General identity and Sameness
¦ Item has the same characteristics as the item
collected by the inspector
Aids Routine documentation procedures
Sample tags with signature of the
inspector and date
Notations in logbook about color,
consistency, and other sensory
perceptions
Precautions To Ensure identity
¦ Other precautions taken to ensure later
identification
Aids Assignment of sample number
Initiation of cham-of-custody
procedures
Present Conditions That Vary
¦ Any features or conditions about the item
being offered in evidence that vary from what
was collected
Aids Full descnption in logbook
4
-------
Representativeness of Item
* Establishes the relationship to other items
of the item offered as evidence
Aids Notations in logbook an sampling
strategy used to select the
particular sample plan
Sampling plan
Ml
Connecting the Chain of Custody
• The meticulous process of showing the
succession of persons who handled or
had access to the evidence
Aids Cham-of-eustody forms
Testimony regarding adherence to
routine sampling secunty measures
Inspector's Written
Documentation
¦Field Logbook
¦Inspection Report
-------
FRE 612: Writing Used To Refresh
Memory
"... if a witness uses a writing to refresh memory
for the purpose of testifying, either —
(1) while testifying, or
(2) before testifying...
an adverse party is entitled to have the writing
produced at the heanng, to inspect it, to cross-
examine the witness thereon, and to introduce
in evidence those portions which relate to the
testimony of the witness..."
FRE 803: Hearsay Exceptions 803(5)
Recorded Recollection
"A memorandum or record concerning a matter
about which a witness once had knowledge
but now has insufficient recollection to enable
the witness to testify fully and accurately,
shown to have been made or adopted by the
witness when the matter was fresh in the
witness's memory and to reflect that knowledge
correctly..."
FRE 803: Hearsay Exceptions 803(6)
Records of Regularly Conducted
Activity
"A memorandum, report, record or data
compilation, in any form, of acts, events,
conditions, opinions, or diagnoses, made
at or near the time by, or from information
transmitted by, a person with knowledge,
if kept in the course of regularly conducted
business activity, and it was the regular practice
of that business activity to make the
memorandum, report, record, or data
compilation..."
6
-------
Chain of Custody
Used to trace the possession of
evidence from the time it was
obtained, until the time it was
introduced as evidence
Evidence Is in "Custody" If..
¦ Ii is in the actual possession, control, and
presence of the inspector
• Ii is in the inspector's view
¦ li is in a storage place lo which
only the inspector has access
¦ It is in a storage place to which
only the inspector and identified
others have access
Basic Chain-of-Custody
Procedures
• Establish custody
¦ Prepare documentation of the evidence
¦ Ensure custody during transit
¦ Note if the seal is found broken
*11
7
-------
FRE 406: Habit; Routine Practice
"Evidence of the habit of a person or of the
routine practice of an organization, whether
corroborated or not and regardless of the
presence of eyewitnesses, is relevant to prove
that the conduct of the person or organization
on a particular occasion was in conformity with
the habit or routine practice."
Photographs/Video
• Keep log in notebook
• Don't take photos of sampling
activities
• Film vs. Digital?''
• Video recordings
*¦11
That's all
' • J HOW 00 I CCT j fn*
~ wuiNTvnon It I aoAEOOtx IC tu lot j
I outer mwM"
/A1
xZr or J« v^pj fiij i l .
1
-------
QUESTIONS??
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SESSION 10
TOPIC: INTERVIEWING
Time: 1 hour 30 minutes
Purpose
Key points
Present basics of planning, conducting, and documenting interviews.
Demonstrate interview techniques through role-play, which demonstrates
things not to do.
Improve trainees' interviewing skills through discussion of techniques and
practice.
interviewing is an important but often overlooked technique in an
inspection.
Good interview techniques enhance verbal and interpersonal relations
skills.
An awareness of how verbal indicators and active listening are key
ingredients in effective interviewing.
LIST OF VISUALS
10-1 Interviewing (Title Slide)
10-2 The Matn Purpose of Interviewing
10-3 Basic Interviewing Questions
10-4 Four General Modes of Communication
10-5 Five Components for More Effective Interpersonal Communications
10-6 Communication Barriers
10-7 Communication Barriers (continued)
10-8 Communication Barriers (continued)
10-9 John Wooden Quote
10-10 Time and Place
10-11 Time and Place (continued)
10-12 Physical Environment
10-13 Proxemics
10-14 "Preparing" for the Interview
10-15 Five Steps of a Law Enforcement Interview
10-16 Types of Questions to Use
10-17 Avoid
10-18 Listening
10-19 How To Be an "Active Listener"
10-20 Non-Verbal Communication
10-21 Evaluating Non-Verbal Communication
10-22 View Any Behavior in Context with the Individual's
10-23 Best Young Achiever Quote
MARCH 2000
-------
Interviewing
The Main Purpose of interviewing
Information
Basic Interviewing Questions
• Who?
¦ What''
¦ When?
¦ Where?
- Why0
• HoW?
-------
Four General Modes of
Communication
¦ Verbal
• Non-verbal
¦ Written
¦ Symbolic
Five Components for More Effective
Interpersonal Communications
¦ Self-concept (most important)
PMJII
¦ Listening skills
* fj|
¦ Clarity of expression
I MB
* Coping with angry feelings
• Self-disclosure
Ift)
Communication Barriers
A communication barrier is something we do or
say that:
¦ Makes the other person less willing to
communicate
• Causes the other person to become defensive
¦ Unnecessarily irritates the other person
2
-------
Communication Barriers (continued)
¦ Making premature comments
and evaluations
* Making statements that are too
general or excessively Arm
¦ Interrupting others
* Talking too much
* Repeatedly telling others what
to do
Communication Barriers (continued)
¦ Talking down to people
¦ Asking loaded questions
¦ Administering punishment through sarcasn
¦ Placing emphasis on blame
• Arguing
¦ Displaying irritating listening habits
"It's what you learn after you
know it all that counts."
John Wooden
IM
3
-------
Time and Place
¦ First consideration —
¦ Announced or unannounced''
¦ Second consideration —
0 Whose territory''
» Outs'' Theirs'' Neutral''
10-16
Time and Place (continued)
¦ General rules
° Victims Cm. witnesses second, and suspects last
° Separate witnesses
° Friendly witness
° Hostile or reluctant witness
" Suspects
° Attorneys present
Ifrtl
Physical Environment
General Rules
• Eliminate as much noise as possible (physical,
psychological, and semantic)
¦ Eliminate communication barriers (desks,
tables, crossed amis/legs, personal items, etc.)
¦ Use proxemics to your advantage
• Remember—Set the stage
«»i:
-------
Proxemics
Intmate 0 to 1.5 feet
Personal 1.5 to 4 feet
Social 4 to 12 feet
Public 12 to 25 feet
"Preparing" for the Interview
< ¦ What is the objective/purpose'7
• What do 1 know?
¦ What bo I want to know9
• What are the elements of the crime/situation''
• What is the background of the interviewee?
¦ Determine the potential for Miranda
¦ Select the lead/primary interviewer, if it is
possible to have two interviewers
¦ Differences between one- and two-person
interviews
Five Steps of a
Law Enforcement Interview
¦ Identification:
• Questions:
o ID—yourself
° General
» ID—interviewee
° Specific
° ID—purpose
• Summary
¦ Rapport
¦ Gose
1*1)
5
-------
Types of Questions
To Use
¦ General or open-ended
¦ Specific or direct
¦ Backward reaching
¦ Empathetic/sympathetic
¦ Opinion
?
Avoid
¦ Leading questions
¦ Negative questions
¦ Compound questions
¦ Complex questions
tfrl'
Listening
People give meaning to words
Feelings more important than
mere words
"Active" listening includes:
° Hearing/noticing both verbal and
noo-vcrt>Bl message, tone, and
inflection
The "listener" usually maintains
the most eye contact
6
-------
How To Be an
"Active Listener"
¦ Remain neutral
¦ Give your complete attention
¦ Ask about their statements
¦ Restate their main points
¦ Put their feelings into words
¦ Get agreement
Non-Verbal
Communication
Kinesics
Body Movement ;
Oculesics/Pupillometrics
i
Eye Movement
Proxemics
Distance/Space
Haptics
Touch
Evaluating Non-Verbal
Communication
¦ Factors to be considered
° Culture
» Content
o Change from the norm
0 Clusters of behavior
7
-------
View Any Behavior in Context with
the Individual's
Religion
• Culture
IfrS
Best Young Achiever Quote
Elizabeth Bnnton, 13-year old Girl Scout,
explaining how she sold 11,200 boxes of
cookies:
'You have to look people m the eye and
make them feel guilty *
Recognize that guilt is a tool to be used. Most
people warn to do well
8
-------
-------
SESSION 11
TOPIC: ON SITE RECORDS REVIEW
Time: 60 minutes
Purpose
Key Points
List of Visuals
List of Handouts
• Present key elements of reviewing records.
Ability to follow the paper trail is a key skill of the inspector.
11-1 On Site Records Review (Title Slide)
11-2 Records Inspection
11-3 and 11-4 Problem A
11-5 and 11-6 Problem B
11-7 Problem C
11-8 Problem D
11-9 and 11-10 Overview of Steps in Sampling Records
11-11 Sampling Techniques
11-1 Sample Manifests
11-2 Problems in Sampling Strategies
i
MARCH 2000
-------
On Site Records Review
ii i
Records Inspection
" Conduct of records reviews
¦ Records sampling techniques
Problem A
A company has not submitted any reports of
exceeding the discharge limits imposed in its
permit Your inspection of the facility indicates
poor operation and maintenance of pollution
control equipment, leading you to suspect that
the equipment may have failed You want to
determine whether there were any excursions
that should have been reported to EPA.
1
-------
Problem A
¦ What records would you look at1
• What would you be looking for?
¦ What evidence would you attempt to collect''
Problem B
EPA has a tip that a company has begun
manufacturing and distributing a new chemical
(di-benzo-homble) before completing the
remanufacture review process required under
TSCA or FIFRA
II )
Problem B
¦ What kinds of records and documents
would you look for?
¦ What other evidence might there be1
¦ How would you approach an inspection
to determine whether a company was
making a new product if EPA had no up9
2
-------
Problem C
A company's records ol storage of hazardous
waste are sloppy and incomplete You easily can
document the violation of recordkeeping
requirements, but you suspect the company is
storing waste for much longer than the period
allowed
Problem D
A citizen has notified EPA that a dredging
company allegedly has disposed of dredged
material into wetlands owned by the town of
Clarksville
¦ What records might help to confirm this
allegation''
¦ What evidence would you attempt to collect''
Overview of
Steps in Records Sampling
" Determine the objectives of the records
review
• Identify the total population
¦ Select the sampling method
3
-------
Overview of
Steps in Records Sampling
¦ Determine the sample size
¦ Conduct the sampling
• Document the sampling methodology
Sampling Techniques
* Random sampling
¦ Systematic or interval sampling
¦ Stratified sampling
* Block sampling
¦ Judgmental sampling
4
-------
HANDOUT 11-1 c
Sample Manifest 3
TEXAS WATER COMMISSION
P.O. Bo* 13087. Capitol Station
Auttin, Taxas 78711-3087
pm*m m m not If*** far «m an «w« (il «*cm mow i
Farm apprwatf. 0MB No. lOSMOn. a>p«*! M-30-tl
UNIFORM HAZARDOUS
WASTE MANIFEST
I Generator ( US EPA 10 No
C01680090071
tnlormauon in tha thaOad areas
<* not required by Federal b«t
Maniiest
Document No
P«9« 1
^¦625A304ifl
B/Sutl
kate^tabaporwrY
sl'fki i ' !•
3 Generator s Name and Mstitno Address
U.S. E.P.A., H.E.I.C.
Building 53. Boi £522^ Dggv^lpleral Center
4 Generators mono (303) 236-5 111
S Transporter 1 Company Name
Rolling Chemrok. Inc.
US fA 10 Number
J PEP982565947
7. Tnnspontr 2 Company Nama
Matlock, Inc.
• US EPA 10 Number
I DED981110166
I Oetigruied Facility Nama and Sua Address 10 US EPA
MyiciSic'iiSsss1 Scr,ice (u)'lnc-
US EPA 10 Number
Baton Rouge, LA 70807
ILQD010395127
11 US DOT Desertion (including Proper Shipo«ng Name. Haiard Class, and 10
Number)
Waste Flammable Liquids, n.o.s., 8,
UNI993, PG II
Waste Corrosive Liquids, n.o.s., 3,
UNI760, PG II
Hazardous Waste, Liquid, n.o.s., 9,
NA3082, PG II
" Hazardous Waste, Solid, n.o.s., 9,
NA3077, PG II
>*r.' • u
tpdeliverahli? return to generator. If snlliwi in Louisiana rmim-r the TV^mubmh cf Public
Safety. Avoid ingestion, inhalation. ana dan contact.
•• OtNtPATOPI CtWTIflCATIONiHnnOi Osctiieweidwaemamsaf—roMormmaarefuayendeccurmtianriosaseinayiraai'Ww^aamaandart
* I em a lerye eweauy
eoonervwcottypreciiceb
future tfveet *e humen
LOW-Hlaiaimaaawwwytanaoiar.i
n »«iiaia»«iunniyr\
ef «raa»« a»|m>»
¦ anaem cun—me»e«a«t««a ma HMOawenmas we present ana
¦»et a »ead lean enenwwmum my lOiMtaneraMsn and select
Printed/Typed Mama
Joe Badludc
17. Transpcrtar 1 Actnowrtadgoment of Receipt ol Materials
Month Dor
102 I 27 I 87
Primed/Typed Nama
Sam Goodluck
It Trenaponer 2 Atanowtadpsmant of Receipt of Matanoll
Primed/Typed Nama
II Discrepancy lnd«cei«n Space
qg_
Month Day toor
Itg 127187
Data
Signature
Month Dor v—'
1—1—1
Prmied Typed N,
Sam Noluck
12
SO fec»My /VoMowrTrensponer Green-Genere tor's first copy
(Re* tuo«*t)
-------
HANDOUT 11-2
PROBLEMS IN SAMPLING STRATEGIES
1. Regulations require that all employees of Dumpstump, Inc., complete a training course — within
two months of being hired - on how to handle hazardous material safely. Your task is to
determine whether the company has complied with these regulations. EPA records indicate that the
company employs 525 people. You plan to review records and then conduct follow-up interviews
with several employees to verify those records. You have approximately one hour to complete the
records review portion of this task.
Dumpstump officials tell you that each employee's personnel file includes a record that shows that
the required training has been completed. Company officials show you a file cabinet that they say
contains all of the personnel files, organized in alphabetical order by name of the employee. There
are 389 files.
What factors would be important to support a reasonable conclusion about compliance at the firm?
What are the potential biases in the files? How might the discrepancies between the number of
personnel files and EPA's records of the number of employees be explained? Is there a particular
categories) of employee that you want to focus on? Is there any category of employee that you
want to exclude? Which sampling method or methods could you use to select specific records for
review? How would you select the individuals to be interviewed?
2. The Spewforth Company is required to submit a written report to EPA if it has had a minor
discharge exceeding the limit established in its permit; the reports must be submitted within five
working days of the end of the month. Reports of major discharges must be filed within five days
of their occurrence. Spewforth's permit requires the company to take and analyze samples of
discharge from three locations twice a week and to maintain records of the sampling and results of
analysis for review by EPA upon request
For the past 24 months, EPA has received only one monthly report about a minor exceedance; no
major discharge has been reported. The last inspection of the facility took place more than two
years ago. Although EPA has no direct knowledge that discharge exceedances have occurred,
neighbors have complained that orange-colored, smelly liquid comes out of the pipe occasionally -
but no dates have been reported.
The company keeps logs of its sampling activities and analytic results. Your period of interest is
the previous two years. Since three samples are (supposed to be) taken each week, the logs are far
too extensive to allow for review of all entries. How would you go about selecting log entries for
review?
1
MARCH 2000
-------
12
-------
SESSION 12
TOPIC: SAMPLING AND LABORATORY ISSUES
Time: 90 minutes
Purpose
Key Points
• Explain the importance of physical samples as evidence
• Present considerations involved in ensuring that samples meet quality
requirements
• Provide an overview of the sampling process from planning through
disposal of contaminated equipment
• Provide a basic understanding of the functions of a laboratory and the
relationship between the laboratory and the inspector
Note. This session is not intended to teach inspectors how to sample but
to provide a basic understanding regarding sampling issues
• Physical samples are collected to establish the presence and concentration
of regulated substances and the extent of contamination.
• Sampling data help determine whether a violation exists (for example,
exceeding a standard) and, if so, the gravity of that violation (for use in
determining penalties).
• Before the inspection is conducted, sampling objectives and data quality
requirements and the methods by which they will be met must be
established in a quality assurance project plan per EPA Order 5360.1,
change 1 (July 1998)
• Standard collection should be followed or deviations noted in field
notes/log book
• Chain-of-custody procedures MUST be followed.
• Inspectors should be aware of capabilities and limitations of laboratory.
• Laboratory personnel can be a valuable source of technical expertise.
• Advance planning for laboratory work helps ensure prompt analysis.
i
APRIL 2000
-------
Physical Sampling
•
Policy considerations in sampling
•
Technical considerations in sampling
•
Common sampling errors
•
Quality assurance and quality control
•
Documentation of samples and chain of custody
•
Management of samples in the field
•
Laboratory Issues
General Guidelines for Sampling
• Take a sample when one is needed to prove a
violation
• Sample only when there is reason to suspect
the substance is present
• Always attempt to verify the presence of the
substance by a means in addition to sampling
-------
When To Sample
• No data
• Insufficient data
• Data in doubt
• Data for event
• Required
; - v iJ; • ¦ 'iiic-
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• .. : , .• • ""W't *: / , - . . v
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-------
Quality Assurance/Quality Control
EPA Order 5360.1 chg 1
Requirements
• Applicability to Environmental Programs
- Order applies to following environmental
programs
• direct measurement of environmental
conditions or releases including.
-sample collection
-analysts
-evaluation, and
-reporting of environmental data
Quality Assurance/Quality Control
EPA Order 5360.1 chg 1
Requirements
• Applicability to Environmental Programs
- Order applies to following environmental
programs
• the use of environmental data collected for
other purposes or from other sources
(secondary data) Including:
- industry surveys
- compilations from computerized data
bases
Quality Control
• Quality control consists of a set of
TECHNICAL activities that must be
performed to DOCUMENT whether the
desired DATA QUALITY is being
produced
3
-------
Quality Assurance
• Quality assurance is a system of activities at
the:
• Planning
• Implementation
• Review
• stages of a data gathering project to ensure
that data collected for EPA ate of the
quality needed and claimed
Quality Assurance
Project Plan (QAPP)
• Must be prepared for every sampling
inspection
• Two types
- Routine
- Nonroutine
Quality Assurance
Project Plan (QAPP)
• Verifies what and how you are conducting
sampling
• ensures that data collected for EPA are of
the quality needed and claimed (DATA
QUALITY GOALS)
4
-------
Quality Assurance and
Quality Control Samples
• Replicate
• Split
• Spiked
• Preservative
blanks
Changes in the QAPP
• Can the original objectives still be met?
• Can the sampling still be done with the
existing equipment?
• Is it safe to sample?
Can the evidence you
collect stand up in a
court of law?
-------
Transportation to Site
• Driving is Easier than Flying
• Some Things just
Won't Fly
• Coordinate Time
of Arrival
Representative Samples
Inspector must insure all samples
are representative-taken and
analyzed using appropriate
SOP (QAPP)
I I
L
6
-------
Representative Sampling
Factors
• Operating conditions
• Types of waste
• Statistical
considerations
• Temporal
considerations
• Spatial considerations
Evaluating Drum Populations
• Monitor Ambient Air
• Check Accessibility
• Observe Labels and Markings
• Open Drums to Examine Contents and
Perform Field Tests
7
-------
' ^1. \
4?
i" ti'- s.
-
X
I
#
Drum Sampling Techniques
• COLIWASA [NO Glass thiefl for liquids
• Split Spoon Coring of Solids
• Pitard Method
• Examples
-------
TankCQllWASA
CCA IVVA.SA
Bacon
9
-------
Soil Sampling
• Review historical photos, if available
• Visually inspect site for the obvious
• Use field measurements to locate
contamination
• Select a suitable sampling method
CfcTffi »]M» Lt
-------
A'.KIVI
Grui'LlWttf
Thii?
Walled
Tub~
SflMJJpQOp
Tools for Evaluating
Wastewater Discharges
• Grab Samples
• Automatic Sampling
• Continuously Recording pH meter
• Flow Meters
When are Grab Samples
Appropriate?
• Samples of Opportunity
• Intermittent Flows
• Facility Batch Treats Wastewater
• Instantaneous Readings are Necessary
-------
Advantages of Using Automatic
Wastewater Samplers
• May be placed hours in advance
• Monitor discharge over time
• Triggered by flow, pH, conductivity, or
time
12
-------
Continuously Recording pH
Meters
• Provide a record over time of
instantaneous readings
• Good method for detecting pattern of
discharge
• May be stand alone device or module of
an automatic sampler
Flow Meters
• Some permit discharge limits are flow
dependent
• Another good method for detecting
patterns of behavior
• Can be used to trigger automatic sampler
Safety Plans
• Identify Team Members
• List Emergency Information
• Discuss Anticipated Hazards
• Detail Workplan and Related Safety
Measures
• Describe Monitoring Plan
• Decontamination and Disposal Plans
13
-------
What is a Confined Space?
• Size and Shape Must Permit a Person to
Enter
• Restricted Entry and Exit
• Not Designed for Continuous Occupancy
• Hazardous Atmosphere of Poor
Ventilation
• Any Other Safety Hazard
What are Hazardous
Atmospheres?
• Oxygen Level Below 19.5% or Above 23.5%
• Flammable Gas or Vapor Level Above 10%
of LEL
• Toxic Substance Level Above TLV
• Combustible Dust Level Obscuring Vision at
5 Feet or Less
• Any Atmosphere IDLH
Atmospheric Monitoring
Equipment
• Oxygen Meter
• Combustible Gas Meter
• Hydrogen Sulfide Meter
• Carbon Monoxide Meter
• Hydrogen Cyanide Meter
• Radiation Meter
• Volatile Organic Vapor Detector
14
-------
Confined Space Entry Permit
• Identifies the Site
• Describes Confined Space to be Entered
• Lists Entrants and Back-ups
• Outlines Pre-entry Preparation
• Describes Rescue Plans
r~
Common Sampling Errors
• Calibration
(continued)
15
-------
Common Sampling Errors
• Calibration
• Maintenance
• Forgotten equipment
• Misreading
• Miscalculations
(continued)
Common Sampling Errors
• Mislabeling
• Transposing of
data
• Poor field notes
• Loss of samples
16
-------
17
-------
L
18
-------
Field Documentation
•Sample Documentation
•Field Notebooks
•Photographs
•Videotapes
•Chain of Custody
-------
Field Notes
• Record in a bound notebook
• Sign and date notes
• Be sure there is only one set of notes
• Remember notes may be discoverable by
defense
• Don't give facility a copy of notes
-------
Appropriate Field Notes
• General observations like time of entry
and weather conditions
• Field instrument identification and
calibration data
• Inventories of containers on site
• Detailed sample descriptions
O)
C
C
~UJ
S
2
©
Li-
ft Mr sf*
l&>.
H*
btc
m
f 3
x*s
f.
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Photo Log Reminders
• Roll and Frame Numbers
• Subject
• Site Name
• Date
• Photographer
-------
^ S? 4=1
T> Dt"
I": r
9
,2-
ProjectI 80C-0S
Sitai Thoro Products, Inc.
Looatioai Arvada, Colorado
Data I Novubtr 13, 1996
Subjacti Samples 02 and D3
Photographer: D. Staphanson
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-------
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23
-------
r
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9
i i
Chain-of-Custody Procedures
• Establishing custody
• Preparing documentation
• Coordinating the sample and documentation
• Ensuring continuity of custody during transit
24
-------
A Sample is in Custody if
• It is in your possession
• It is in your view after being in your
possession
• It was in your possession and you locked it
up
• It is in a designated secure area
Sample Holding Time
Prompt analysis is the most positive
assurance against error from sample
deterioration
Preservation and Holding
Times
• If preservatives are
used,record in
field notes
• Ice down samples
before transporting
to lab
• Be aware of
holding times
25
-------
Packing and Shipping Samples
49 CFR 172.702 states in part:
Everyone "who performs any function subject to
the requirements of this subchapter may not
perform that function unless trained in
accordance with the requirements of this
subpart..."
Each person who packs hazardous materials or
offers such materials for shipment must be
trained and recertified every two years
Shipping Hazardous Samples
1
• Special Training
• Shipping
Containers
• Labels
*¦: ~
• Air Bill Preparation
• Common Problems
-------
Laboratory Analysis
• Laboratory operations
• Laboratory capabilities
• Interpretation of analytical
results
Special Analytical
Considerations
Short Holding
Times
Chemist Available
to Receive
Samples
Sample Handling
• Maintaining physical custody
• Chain of custody documentation
• Sample storage
27
-------
Storing Samples
• Store samples with low levels of
contamination with like samples
• Store samples with high levels of
contamination with like samples
• Never store incompatibles together
• Store samples in secure area free from
exposure to conditions which could alter
them in any way
Relinquishing Samples to Lab
• Coordinate time of
delivery
• Check chain of
custody with chemist
• Discuss field
measurements
• Preservatives used
Report of Findings
• Describe field
activities
• Report analytical
findings
• Site maps and
sample location
• Include photos
28
-------
Litigation Support
• Exhibit Preparation
• Grand Jury
Testimony
• Depositions
• Trial Support
• Trial Testimony
29
-------
Hanaout xm-x
PROJECT NAMEi
PROJECT NUMBER i
PROJECT COORDINATORi
ACCOUNTABLE DOCUMENTS
RECEIPT FOR SAMPLE FORMS
(# )
CHAIN OF CUSTODY FORMS
(# )
SAMPLE TAGS (# )
LOG BOOKS (type & # )
CUSTODY TAPE {# )
CUSTODY LOCKS <# )
TSCA DOCUMENTS (# )
TSCA LOCKS (# )
I
SAFETY & FIRST AID EQUIPMENT
1 HARD HAT & FACESHIELD
RESPIRATORY PROTECTION
SAFETY GLASSES & INSERTS
RESPIRATORY CARTRIDGES
GOGGLES
TYPE NUMBER
EAR PROTECTION
MSA
RADIOS & CHARGERS
RACAL
FIRST AID KIT
SURVIAIR
PORTABLE EYE WASH
NORTH
I
FIRE EXTINGUISHER
COOLING VEST
S C B A
SPARE TANKS
5 MINUTE ESCAPE MASK
CASCADE SYSTEM
SAFETY HARNESS
LIFTING TRIPOD
[ TRAUMA KIT
OXYGEN
1
-------
PERSONAL PROTECTIVE EQUIPMENT
TYPE
SMALL
MEDIUM
LARGE
X-LG
SARNEX
COATED TYVEK
NON-COATED TYVEK
DISPOSABLE RAIN SUITS
RAIN SUITS
NOMEX HOODS
BUTYL APRONS
NUKE BOOTS
RUBBER BOOTS (steel toe)
CLOVES
NEOPRENE (corrosive)
NITRILE (solvents)
BUTYL RUBBER
VITON
POLYURETHANE
LATEX
LEATHER
COTTON
2
-------
INSTRUMENTS
V A/CHARGER & CAL. GAS
H N U,CHARGER & CAL. GAS
MONITOX SD HCN (CYANIDE)
PHOTOVAC-TIP & CHARGER
P H METER & RECORDER
DRAGER PUMP & TUBES
CONDUCTIVITY METER
POCKET DOSIMETER
| RAD MINI
BRUNTON COMPASS
METAL DETECTOR
GEIGER COUNTER
E M-34
WELL DEPTH SOUNDER
GAS TECH MODEL-86
GAS TECH MODEL-91
1 CHLORINE TESTER
PERSONAL SAMPLING PUMP
1 HEAT STRESS MONITOR
SOUND LEVEL METER
DECON EQUIPMENT
HASH TUBS
BUCKETS
SCRUB BRUSHES
DETERGENTS (type )
PLASTIC SHEETING
SOLVENT (type )
TRASH BAGS
PAPER TOWELS
MASK SANITIZER
DISTILLED WATER
I
STEAM CLEANER
3
-------
SAMPLING EQUIPMENT
DRUM THIEVES
COLIWASA
BAILERS
GLASS FUNNELS
GRADUATED CYLINDER
PLASTIC SCOOPS
1 STAINLESS SCOOPS
STAINLESS PITCHERS
STAINLESS BUCKETS
STAINLESS PANS
STAINLESS SPATULAS
PLASTIC SPATULAS
SPLIT SPOON SAMPLER
PORTABLE SAMPLER
POND SAMPLER
MANNING SAMPLER .
ISCO SAMPLER
CUBITAINER (DOSED)
BACON BOMBS
SLUDGE JUDGE
MANHOLE OPENER
CAKE PANS
DRUM OPENING KIT
V 0 A, S
ENTRENCHING TOOLS
QUART JARS (cases)
PICK & SHOVEL
GALLON JARS (cases)
P H PAPER
8 OZ JARS (cases)
FLOW METER (Ibco)
PLASTIC BOTTLES(4oz/8oz)
FLOW METER (Manning)
CUBITAINER (size)
4
-------
MISCELLANEOUS
PORTABLE COPIER/CARTRIDGES
DRINKING WATER CONTAINER
MEASURING TAPE (cloth)
MEASURING TAPE (steel)
ELECT. EXT. CORD (lqth )
GENERATOR & GAS CAN
REAMS OF PAPER
CAMERA AND FILM (35mm)
PORTABLE TOILET
FLASHLIGHT & BATTERIES
MEASURING WHEEL
BARRICADE TAPE
SURVEY FLAGS
ROPE (type /lqth )
PLUMB BOB
BOLT CUTTERS
RHODAMINE DYE
ISOPROPANOL
NITRIC ACID
ACETONE
HEXANE
DISPOSABLE CUPS
SHIPPING EQUIPMENT
ZIP LOCK BAGS LG SM
PLASTIC BAGS LG SM
PAINT CANS & CLIPS
SHIPPING LABELS (type)
BUBBLE WRAP
KIM WIPES
ICE CHEST
VERMICULITE
FED X FORMS
INK PENS
MARKER PENS
TAPE (DUCT)
TAPE (STRAPPING)
5
-------
NEIC SITE HEALTH AND SAFETY PLAr,
1.
2.
3.
4.
5.
Project Title:
Location:
Description of Field Activities:
Date of Field Activities:
NEIC Personnel:
General Information
Project Number
Project Leaders)
6. Contractor Personnel: Must be OSHA certified per 29CFR 1910.120.
Obtain list or personnel, duties or work to be performed, and copies of training certificates.
Emergency Information
7. Ambulance: Phone:
8. Hospital: (Emergency Room) Phone:
9. Emergency Route:
10. Fire Department: Phone:
11. Police: Phone:
12. Poison Control Center: Phone:
13. Site Emergency Notification/Evacuation Method:
14. NEIC Health and Safety Officer Steve Fletcher (303) 236*5111 ext 283
15. Radiation Safety Assistance:
Jed Harrison, Director (702) 798-2476
Office of Radiation Programs
Las Vegas Facility
Hazard Evaluation
1
-------
16. Check all known or potential hazards: Radiation Toxics Fire/Explosion
Corrosives Oj Deficiency Noise Physical Biological
Dusts Heat/Cold Stress
NOTE: DISCUSS HAZARDS AND PRECAUTIONS IN DETAIL IN WORK PLAN BELOW.
17. Specify unusual working conditions/limitations (excavations, confined spaces, lagoons,
elevated surface, weather, darkness, etc.)*:
* Attach specific hazard management plans, if applicable.
18. Potential Chemical Hazard:
Chemical
TLV/
1LDH
Route of
Exposure
Acute
Symptoms
Odor
Level
Odor/Visual Description
* Potential or confirmed carcinogen
Work Plan
] 9. List tasks, anticipated hazards checked above, and control measures which will be taken,
including levels of protection:
Task
Hazards
Level of Protection
(A, B, C, D) and Control Measures
20. Health Hazard Monitoring Plan:
1 Constituent
Type of
Sample
Frequency
Instrument
Notes
I
2
-------
I 111 I
Site Control/Security Measures:
22. Decontamination Procedures (personnel hygiene, contaminated clothing, equipment,
instruments, etc.):
23. Disposal Procedures (contaminated equipment, supplies, decontamination solutions, etc.):
Approvals
This site HASP has been reviewed and constitutes the minimum anticipated safety requirements for
personnel engaged in field activities at this project site. However, the Project Leader has the
authority to change these requirements, based upon the conditions present at the site.
Approved bv:
24. Project Leaden Date:
25. Branch Chief: Date:
Health & Safety Officer Date:
oITEHASPJRM:09/97
3
-------
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Example of the Sample Seal
UMTTD STATIS
ENVIRONMENTAL PROTECTION AOCNCY
inspectors seal
Sampt* No.
1
CM
t
•
o
I
Signal**
4
1
6
6
3
Prim Nam* an
d TW*
5
(1) Insert sample number
(2) Insert date sealed
(3) Print location of collector's station
(4) Signature of persons sealing the sample
(5) Print name (same as signature) and title of sealer
H
(6) When a seal Is broken for any purpose, initial here and enter the date- g
broken. Submit broken seal with sample records g*
e
LU
«>
net!
M
k
-------
Example of the Sample Tag
O
I
tM ~ NO ~
ANALYSES
BOO Mm
i crasinwif
W31
Mtoun
rtONwT
OoantaiQCAW
Prtwtr PWMML
TWRIVDVO
I..TTTT
>VT
Rtmaifcs:
E
Toqm.
IMWW
front
UNITED STATES ENVIRONMENTAL PROTECTION AQetCY
REGION 4
Crwtacwmrm Sovte— OM#ao
Co*«Q« Station Ao«d
Attytrm, OA 30613
O
m EPA
BACK g
0
O-
o
c
I
in
ISNETt
-------
ENVIRONMENTAL PROTECTION AGENCY
Office of Enforcement
RECEIPT FOR SAMPLES
NATIONAL ENFORCEMENT INVESTIGATIONS CENTEI
Building S3. Box 25227, Denver Federal Center
Denver, Colorado 80223
SAMPLERS: (Slgnitura)
PROJ. NO.
90Q
PROJECT NAME
Split Samples Offered
( ) Accepted ( ) Declined
Name of Facility
Facility Location
3TA. NO.
DATE
TIME
SPLIT
SAMPLES
TAQ NUMBERS
8TATI0N DESCRIPTION
NO. OF
CON-
TAINERS
REMARKS
I
J
r
('
(i
i:
i 1
I
I
Transferred by: (Stgnatum)
Received by° (Signature)
Telephone
Date
Time
Title
Date
Time
Distribute inai to Coordinator Field Flies; Copy to Facility
242
-------
CHAIN OF Cur"-«1Y RECORD
Danvti r»inr»do 80225
/ Handout 12
PRO J. NC
3JECT NAME
NO.
SAMPLERS: fStfntrw/
REMARKS
CON-
TAINERS
STATION LOCATION
TIM6
DATE
Data / Time Received by: (S/fnttvrr)
Relinquished by: (signtmnl
Received by*. iSigmtwt)
Relinquished by: tSftniturtf
Received by: tSignarurtt
Received by:
Date /Time
Relinquished by: fstgn*tur»j
Relinquished by: (Signttunl
Recalved for Laboratory by:
(Stjn*rur»)
Relinquished by: (Sifnnvn)
Oiitrftwtlon: Orlgtml Aeeemptnltf SMpfn«m; Copy to Coortflnttor flatd Flttt
N 3211
-------
Ranaoui
TABLE 2-34
CONTAINERS, PRESERVATION TECHNIQUES. AND HOLDING TIMES
FOR AQUEOUS MATRICES*
Name
Container1 Preservation
Maximum holding time
Inorganic Tests:
Chloride
Cyanldet total and
amenable
to chlorinetion
Hydrogen ion.(pH)
¦Nitrate
Sulfate
Sulfide
P,G
P,G
P.O
-P.X3
P.G
P.G
None required 28 days
Cool to 4°C; if oxidizing 14 days
agents present add 5 mL
0.1N NaAs02perLor
0.06 jg of ascorbic add
per L; adjust pH>12 with
50% NaOH.
See Method 9010 for
other Interferences.
None required 24 hours
rtoni to 48 hours
Coot to 4°C 28 days
Cool to 4°C, add zinc 7 days
acetate
Metals:
Chromium VI
Mercury
Metals, except chromium VI
and mercury
Organic Tests:
Acrolein and acryfonftrile
Benzidines
P.G
P.G
P.G
G. PTFE-lined
septum
G, PTFE-lined
cap
Chlorinated hydrocarbons G, PTFE-fined
Oioxins and Furans
Haloethers
Nttroaromatics and
cyclic ketones
Nitrosamines
cap
G, PTFE-lined
cap
G, PTFE-lined
cap
G, PTFE-lined
cap
G, PTFE-lined
cap
Cool to 4°C
HNOj^to"pH<2
HN031opH<2
Cool to 4°C,
0.008%-Na2SI0,3l
Adjust pH to 4-5
Cool to 4*C;
0.00856NaiS203s
Cool to 4°C,
0.008%' NajSjOj3
Cool to 4°C,
0.008% NajSjOj'
Cool to 4°C,
Offl)R%:NA.Riri13
Cool to 4*0,
0.008% Na2S,0,3,
store in dart
Cool to 4°C,
0.008% NajSjOj3,
store In dark
24 hours
28 days
6 months
14 days
7 days until extraction,
40 days after extraction
7 days until extraction,
40 days after extraction
30 days until extraction,
45 days after extraction
7 days until extraction,
40 days after extraction
7 days until extraction,
40 days after extraction
7 days until extraction,
40 days after extraction
(continued on next page)
TWO-46
Revision 4
January 1998
-------
TABLE 2-34 (continued)
Name
PCBs
Phenols
Phthafate esters
Polynudear aromatic
hydrocarbons
Purgeable aromatic
hydrocarbons
Purgeable Halocarbons
Total organic halides (TOX)
Radiological Tests:
Alpha, beta and radium
Container1 Preservation
Maximum holding time
28 days
28 days
7 days until extraction,
40 days after extraction
7 days until extraction,
40 days after extraction
7 days until extraction,
40 days after extraction
7 days until extraction,
40 daysafteuxtcaction
7 days untO extraction,
40 days after extraction
7 days until extraction,
40 days after extraction
14 days
14 days
28 days
6 months
Oil and grease G Cool to 4°C,
add 5 mL diluted HCi
Organic carbon, total (TOC) P, G Cool to 4°C,
store in dark2
Organochlorine pesticides G, PTFE-lined Cool to 4°C
Organophosphorus
pesticides
cap
Cool to 4°C
G, PTFE-lined
cap
G, PTFE-lined
Coolto4°C
cap'
G, PTFE-lined
Cool to 4°C,
cap
AD08%_Na2SjO3
G, PTFE-lined
Cool to 4°C
cap
G. PTFE-lined
Cool to 4°C,
cap
0.008% NajSjO,3,
store In dark
G, PTFE-lined
Cool to 4°C,
septum
0.008% NajSj03w
G, PTFE-lined
Coo! to 4°C,
septum
0.008% Na^O,3
G, PTFE-lined
Cool to 4°C, Adjust to
cap
pH<2 with HjS04
P.G
HNO,topH<2
Table originally excerpted, in part, from Table B, 48 FR 28, October26,1984, and revised as appropriate
forSW-446. See Chapter Three, Chapter Four, or the tndivfduaf methods for more Informafion.
' Polyethylene (P) or Glass (G)
Adjust to pH<2 with HjSO* HCI or soSd NaHS04. Free chlorine must be removed prior to adjustment
Free chlorine must be removed by the appropriate addition of Na^O,.
4 Adjust samples to pH 5-8 using NaOH or HzSO«.
TWO-47
Revision 4
January 1898
-------
TABLE 3-1.
SAMPLE HOLDING TIMES, RECOMMENDED DIGESTION VOLUMES AND
RECOMMENDED COLLECTION VOLUMES FOR INORGANIC
DETERMINATIONS IN AQUEOUS AND SOLID SAMPLES
Measurement
Digestion
Volume.
Collection
Volume
(mL)"
Treatment
Preservative
Holding Time"
InoroanteAnatvtes (except hexavalent chromium end mercury):
Aqueous
Total 100 600
Solid
Dissolved
Suspended
Total
Hexavafent Chromium:
Aqueous
Solid
Mercury:
Aqueous
Total
Solid
Dissolved
Total
100
100
20
100
2.5 fl
100
100
0.2 g
600
600
200 g
400
100 g
400
400
200 g
HNO, to pH <2
6 months
Filter on site;
HNO, to pH <2
6 months
Filter on site
6 months
6 months
24 hours
Store at 4*±2*C
until analyzed
One month
to extraction, 4 days
after extraction
Store at A'i 2*C
until analyzed
HNO, to pH <2
26 days
Fitter;
HNO, to pH <2
26 days
28 days
Store at 4*±2*C
until analyzed
Unless stated otherwise.
Either glass or plastic containers may be used.
Any sample volume reduction from the reference method's Instructions must be made in the exact
proportion as described in the method and representative sampling must be maintained.
CD-ROM
THREE-11
Revision 4
January 1998
-------
TABLE 4-1.
SAMPLE CONTAINERS, PRESERVATION, TECHNIQUES, AND HOLDING TIMES
VOLATILE ORGANICS I
Sample Matrix
Container
Preservative
Holding Time 1
Concentrated Waste
Samples
Method 5035: 40-mL vials with stirring bar.
Method 5021: See method.
Methods 5031 & 5032: 125-mLwldemouth
glass container.
Use Teflon-lined lids for all procedures.
Coolto4*C.
14 days Q
Aqueous Sample* With
No Residual Chlorine
Present
Methods 5030,5031, & 6032: 2 X 40-mL
vials with Tenon-lined septum caps
Coot lo 4*C and adjust pH to less than 2 with
HjSOi, HCI, or solid NaHSO,.
14 days
'Aqueous Samples WITH
1 Residual Chlorine Present
Methods 5030.5031. & 5032: 2 X 40-mL.
vlapSvfth Teflon-lined septum caffe
Colled sample In a 125-mL container which
has been pr»-presc|rved with 4 drops of 10%
sodium thlosulfate solution. Gently swirl to mix
sample and transfer to a 40-mL VOA vial.
Cool to 4*C and equal pH to less Wan 2 with
HjSO„ HCI. or soM NaHSO«.
14 days D
Acrolein and AcrytonRrfle
In Aqueous Sample
Methods 5030, 5031, & 5032: 2 X 40-mL
vials with Teflon-lined septum caps
Adjust to pH 4-5. Cool to 4*C.
14 days
Solid Samples
(e.g. soils, sediments,
sludges, ash)
Method 5035: 40-mL vials with septum and
stirring bar.
Method 5021: See method.
Methods 5031 & 5032: 125-mLwldemouth
glass container with Teflon-lined lids.
See the IndMdual methods.
14 days
FOUR-6
Revision 4
January 1998
-------
TABLE 4-1 (Continued)
SiEMfVOLMlLEORGANICS/ORGANOCHLORINE PESTICIDES/£cBs AND HERBICIOES
Sample Matrix
Container
Preservative
Holding Time B
| Concentrated Waste
B Samples
1j25-mL wtdemouth glass wtth Yeftorvflned
None
Samples ndracted
within 14 days and 1
ejdtracts analyzed Q
within 40 days A
following exfractloa |
Aqueous Samples With
No Residual Chlorine
Present
1-gal., 2 x 0.5-g«1., or 4 x 14. amber glass
container with Teflon-lined lid
Cool to 4*C
Samples extracted
within 7 day* and
extracts analyzed
wtthln 40 days
Mowing extraction.
Aqueous Samples WITH
Residual Chlorine Present
1-gal., 2 x 0.5-gal., or 4 X14, amber glass
container with Teflon-lined ltd.
Add 3-mL 10% sbdlum thlosutfate solution per
gallon (or 0.008%). Addition of sodium
thlosulfate solution to sample container may be
performed In the laboratory prior to field use.
Coo1t©4*C.
Samples extracted
wfthtn 7 days and
extracts analyzed
wtthln 40 days
following extraction.
Solid Samples
(e.g. soils, sediments,
sludges, ash)
2^0-mL wklemouth glass container with
Tpfton-flned (Id
Cool to 4*C
Samples extracted
within 14 days and
extracts anatyzed
wtthln 40 days
following extraction.
FOUR - 7 Revision 4
January 1998
-------
13
-------
SESSION 13
TOPIC: CLOSING CONFERENCE
Time: 30 minutes
Purpose
Key Points
List of Visuals
List of Handouts
• Explain the purpose, scope, and limitations of a closing conference.
• Provide an opportunity for inspectors to discuss preliminary findings.
• Resolve any outstanding questions or issues and verify information.
• Provide an opportunity to complete final paperwork (for example,
TSCA, CBI forms).
13*1 Closing Conference (Title Slide)
13-2 Closing Conference
None
t
March 2000
-------
Closing Conference
Closing Conference
¦ Forma} varies
¦ Preliminary (tentative) discussion of findings
¦ Resolve outstanding issues
• Complete paperwork
¦ Follow your agency's policy in regard to
providing notice of violations
-------
14
-------
SESSION 14
TOPIC: INSPECTION REPORT
Time: 90 minutes
PURPOSE
Key Points
• Explain the purpose and importance of the inspection report
• Discuss and evaluate the elements of a good inspection report
• Provide practical experience in report writing style.
• The inspection report should be factual, free of opinions and
conclusions.
• The report should explain in detail what happened during the inspection
and substantiate in full any potential violations.
• Your career may be evaluated upon how well you communicate
information.
LIST OF VISUALS
14-1 Inspection Report (Title Slide)
14-2 Inspection Report
14-3 Inspection Report
14-4 Inspection Report
14-5' Report Heading
14-6 Outline—Executive Summary
14-7 Outline—Executive Summary (continued)
14-8 Outline—Technical Report
14-9 Description of Facility
14-10 Regulatory Status and Compliance History
14-11 Inspection Methods
14-12 Sampling Activities
14-13 Information About the Closing Conference
14-14 Compliance Findings
14-15 Other Areas of Concern
14-16 Additional Information
14-17 Outline—Appendices
14-18 Handout* Evaluation Guide for Reports
14-19 Tips for Writing Inspection Reports
14-20 Consider the Audience for (each Section of) the Report
14-21 Be Accurate and Impartial
14-22 Write To Express—Not To Impress
14-23 Avoid the "It" Habit and Other Vague References
14-24 Be Simple and Concise
14-25 Be Coherent
14-26 Use Active Voice/Action Verbs
i
MARCH 2000
-------
14-27 Essentials of Good Report Writing
14-28 Who?
14-29 What?
14-30 When?
14-31 Where?
14-32 Why?
14-33 How?
14-34 Exercise: Review Sample Reports
LIST of Handouts 14-1 Inspection Report Evaluation Guide
14-2 Sample Inspection Reports
ii
MARCH 2000
-------
Inspection Report
Inspection Report
¦ Effective reports
• Purpose
¦ Objective
m inpoftnoc
Inspection Report
¦ Official files
¦ Check lists or narrative format?
• Remember
• VmtmKjbomI
-------
Inspection Report
• Typical Outline for Report
¦ Executive Summary...
° Technical Report...
• >l iiiimii 1«i ilT(r1i»ii»»rijh)
" Findings md Conclusions...
° Appendices _
Report Heading
• Type of inspection
¦ Name of site
¦ Address of facility
¦ Date of inspection
• Date of report
¦ Inspection team or participants
Outline - Executive Summary
¦ Introduction and overview
* Project objectives and scope of the inspection
¦ Summary of factual findings
¦ Grouped by ftasstc or process lme/wuttstream
¦ Potential violation (areas of ooooompiiaiioe)
ideatified
• May include (ot refer to later section on) areas
of concent
-------
Outline - Executive Summary
(continued)
¦ Provides a summary of information in the
technical report
¦ b upported folly by mfarraitioe in the technical
report
• Orahn bo jnfenn«aoB Out doc» not «ppc«r in
the technic*! report
fttf
Outline - Technical Report
¦ Description of the facility _
• Regulatory status and compliance history —
"Compliance Endings
¦ Inspection methods „
¦ Sampling activities detailed
¦ Discussion of areas ofxoncem —
Description of Facility
¦ Length of time at location
¦ Ownership
¦ Number of employees
¦ Hours of operation
• Products and services
¦ Description of processes end operations
¦ Medium-specific processes
¦ Waslestreams and waste management methods
¦ Environmental management system
-------
Regulatory Status and Compliance
History
• includes information about applicable:
° Regulations
o Permrtj
° Consent decrees
e Other documents
¦ Includes history of compliance
Inspection Methods
• Techniques
• Strategics
• Procedure
¦ Adjustments
¦ Chronological recount
Sampling Activities
• Sampling plan
¦ Location
¦ Chain of custody
¦ Variations
¦ Results
• Discussion
4
-------
Information About the Closing
Conference
¦ Answers the following questions:
" Who wis present?
¦ Wh* ww distasted?
e Whjl did «be facility agree to do?
• Identifies pollution prevention opportunities
¦ Discusses environmental justice issues
¦ Discusses compliance assistance
¦ Discusses other issues or concerns
Compliance Findings
* Answers the following questions:
• Where did you go tod whK did you wxl
¦ Who (fid yoa talk to 7
• Wh*t record! did you review?
¦ Whit did yon doc do?
¦ Wh*t questions were Mined tad who respocded?
¦ Includes photographs, copies, end all other
documentation.
¦ Includes sampling activities
Other Areas of Concern
¦ Noo-tegulatory observations
• Environmental concerns
¦ Community issues
-------
Additional Information
¦ Safety issues
* Access issues
¦ Compliance assistance
¦ Agency initiatives
• P2. EI. EMS, 33/50
¦ Laws of other agencies
Outline - Appendices
¦ Complex maps, diagrams
¦ Detailed testing, monitoring, sampling
metbods
• Raw data
• Raw test results and extensive analyses
Handout:
Evaluation Guide for
Reports
-------
clear
source
complete
Hps for Writing
Inspection Reports
tactual etc.
accurate
eondse audience
Consider the Audience
for (each Section of) the Report
¦ Audience of the Executive Summary
¦ Senior m*n»grmart unsbfc to read Ibc fuD report
• Noo-trrimtaim who m«y doc imdcmind the full
report
• Attorneys ad bdrviduali in other programs
Deeding m overview of the inspection tod -findings
• Technics] Report
fee case
¦ Findings
• AD enforcement personnel invotwd with fl* case
• Appendices
Be Accurate and Impartial
¦ Report feet as feet and hearsay as hearsay
¦ Did you see actual waste oS? OR only drums
labeled as "waste ofl"?
¦ Did you sec Jimmy dump the oamaiuer OR did
someone else tdl you that be did the dumping7
• Leave out nothing as if concealed or withheld
¦ Even If it may appear to weaken the cue
-------
Write To Express - Not To Impress
Problem:
Next I crossed the dark lot, where I discovered
many drums on a forklift headed for the hidden
warehouse.
Better
I observed drums being transported to the
warehouse.
Avoid the "It" Habit
and Other Vague References
Problem:
I inspected tank A, still B, and lagoon C. It was
^crverflowingand iu> &ecOiidarycontainmeflt was
inadequate.
Better
I inspected tank A, still B, and lagoon C.
Lagoon C was overflowing. The secondary
containment around lagoon C was not capturing
all the overflow.
Be Simple and Concise
Problem:
Write all your sentences as short as you possibly
can, and always avoid the use of complicated
terminology when possible.
Better
Use short sentences. Avoid complicated terms.
-------
Be Coherent
Problem:
It is considered that a detailed
examination is unnecessary at this time
Better
Detailed examination is sot necessary.
Use Active Voice / Action Verbs
Problem:
It is recommended that
Better
I recommend ~
What?
Who?
When?
Essentials
of Good Report Writing
Which?
Why?
Where?
How?
9
-------
Who?
Problem:
The degrc&scr mechanic
Better
Elvis Ferguson, the junior dsgreaser mechanic
working dining the inspection
What?
Problem:
If there had been a fire, no firefighter equipment
could have been carried id own thcTjairownisle.
Better
Hie aisle space between the drams was 16
inches.
When?
Problem:
Mr. Ferguson called me and told me die hose
bad ruptured at 1030. When I arrived, it
was overflowing.
Better.
Mr- Ferguson called me at 10 JO ajn. He told
me that the hose had ruptured at 10:15 un.
When I arrived at 11:00 the secondary
containment was overflowing.
-------
Where?
Prcbtem.
The tank behind the warehouse
Better
Hie 1,000-gallon tank used to store chloride
catalyst before it is recycled
Why?
Problem:
They ship drams to the warehouse because
the storage area is so small.
Better
Mr- Ferguson stated that 2 drums per day are takes
to tbe warehouse because storage area B is too
gmilL Measurements indicate that storage area B
is large enough to contain 6 drums. Plant records
indicate that 8 drums per day are generated by tbe
91 production tine.
How?
Problem:
Appropriate drums are used to avoid
common.
Better
The facility neutralizes hydrochloric acid
from detergent line U1 in plastic "poly"
drams.
-------
Exercise:
Review Example Reports
-------
HANDOUT 14-1
INSPECTION REPORT EVALUATION GUIDE
The organization and format of an inspection report can vary, according to the practice of the office or
program under which the inspection is conducted, the particular circumstances of the inspection, and the
individual writing style of the report writer. No matter what form the report takes, however, the report
and its attachments should answer the following questions.
Basic Inspection Information
Who prepared the Inspection report?
Who signed the inspection report,, and on what date?
Who performed the inspection (all participants)?
What is the name and location of the facility or site?
What is the mailing address and telephone number of the facility or site?
What is 1he name and title of the responsible official who was contacted?
What was the reason for the inspection (for example, routine, response to a complaint, or for cause)?
What are the names and tides of all of the government personnel who participated in the inspection?
Entry and Opening Conference
What are the facts about the entry (date, time, entiy Location, and agent in charge)?
Is there documentation that proper entry procedures were followed?
Were all required notices and credentials presented?
Is there documentation that facility officials were informed of their right to claim that information is
confidential?
Were there any unusual circumstances concerning gaining consent to enter (for example, reluctance,
attempts to limit the scope of the inspection, or attempts to place special requirements on inspectors)?
How were such circumstances handled?
Who was present at the opening conference? What topics were discussed?
1
MARCH 2000
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HANDOUT 14-1
Background of the Facility or Site
What is the type of facility or site?
What types of activities and operations take place at the facility or site?
Who owns the facility or site (for example, a corporation, an individual, a partnership, a federal or state
agency, or a nonprofit organization)?
How many years has the facility been in existence?
How many employees work at the site?
Have any major modifications been made at the facility? Are any modifications or expansions planned?
At what level of capacity is the facility operating? For how many shifts does it operate, and how many
hours per day and days per week? What relationship does this information have to die inspection that
was performed?
Which operations, processes, and activities at the facility were examined during the inspection?
Which operations, processes, and activities at the facility were not examined?
Inspection Activities
• Records Inspection
Is there a general description of how records are kept at the facility?
What was the purpose of reviewing records?
What records of the facility were reviewed?
How were the specific records selected for review (was an auditing technique used or were all
records reviewed)?
Are photocopied records or data manually copied from records adequately identified and
documented?
Were any suspected violations found? (Each should be fully documented, making sure that all the
information required for the section set forth below on suspected violations is included.)
• Physical Sampling
What was the inspector's sampling plan for the facility or site?
2
MARCH 2000
-------
HANDOUT 14-1
What physical samples were collected at the she?
Are the sampling techniques used explained adequately?
Are all samples clearly linked to an identification number, location, and purpose?
Are sampling conditions and other physical aspects of the sample (for example, color, texture, and
viscosity) described?
Were any deviations from the sampling plan or SOPs explained and documented adequately?
Are chain-of-custody procedures documented?
Are the results of laboratory analysis presented clearly?
How do the results of analysis of samples compare with limits set forth in the facility's permit?
• Dlnstratioiu and Photographs
Are photographs taken during the inspection included and properly documented?
Is there some information about the inspection that could be made easier to understand through the
inclusion of a diagranror sEetch7
If sketches, diagrams, or maps are used, is the scale or other relationship shown clearly?
• Interviews
What are the names and titles of officials of the facility and other personnel who woe interviewed?
Ate their statements summarized clearly?
What are the names and addresses of any other individuals who were interviewed or who were
witnesses?
• Closing Conference
Does the report include documentation that required receipts for samples and documents were
provided?
Does the report include documentation that officials of the facility were given an opportunity to
make confidentiality claims?
Does the report note statements the inspector made to officials of the facility about compliance
status, recommending actions to take, or other matters?
3
MARCH 2000
-------
HANDOUT 14-1
Documentation of Suspected Violations
The heart of the inspection report is really the documentation and substantiation of suspected violations,
which allows EPA to determine whether a violation occurred, how and why it occurred, and its
seriousness. This substantiating information includes all the evidence of various kinds that has been
collected. In an actual inspection report, some of the questions on the preceding pages might be
answered in the portion of the report that discusses the evidence collected and other particulars of each
suspected violation.
• Documentation of Suspected Violation
For each suspected violation, the inspection report should answer the following questions:
What regulation does the inspector suspect has been violated?
What information proves that the cited regulation applies to the facility or site?
According to the elements of the regulation, what information proves that the suspected violation
occurred?
What sampling methods (if appropriate) were used to determine that the violation occurred? Are
any deviations from sampling methods adequately explained?
What information shows that possible exemptions to the rule do not apply?
• Cause of Violation
Note: Not all programs require this information, but it may be useful, even when it is not
required, for such purposes as negotiating an appropriate remedy and penalty and planning
future inspections. Causal information must be stated carefully so that it does not provide
the violator with an excuse for the violation.
What information documents the possible cause of the violation (for example, direct observations
of gauge readings, production logs, physical appearance of materials,-or statements by facility
personnel)?
Is there any supporting information that confirms or disproves a possible claim of an upset or other
exempt activity?
• Other Mitigating and Aggravating Factors
The level of enforcement response is based on the seriousness of the violation. Amounts of civil
penalties are based on the gravity and circumstances of the violation, which is usually a calculation
of the extent of the violation (amount of material involved) and the extent of the actual or potential
harm that was or could be caused by the violation. The base penalty can be adjusted upward or
downward because of such factors as past compliance history or efforts made by the facility to
correct the violation.
4
MARCH 2000
-------
HANDOUT 14-1
The inspection report should contain information that will support the appropriate determination of
die seriousness and extent of the violation, as well as other information that might be useful in
calculating a penalty.
What is the seriousness of the violation (for example, amount of emissions, length of time of excess
emissions, nature of emissions, location of source, and perceived effect on the public)?
'What harm resulted or could result from the violation?
What efforts did the facility make to correct the violation?
How difficult will it be to comply (considering such factors as availability of technology, cost of
complying, and time required to correct the violation)?
What is the facility's past compliance history?
5
MARCH 2000
-------
HANDOUT 14-2
SAMPLE INSPECTION REPORTS
This handout contains samples of actual inspection reports; only the names have been changed. Each
report is of acceptable quality, although each has both strong and weak points.
Using the Inspection Report Evaluation Guide, evaluate the sample reports.
• How well does each of these reports meet the criteria in the evaluation guide?
• What are the strengths of each report? What problems can you identify?
• Which report provides the strongest support for case development? The weakest? Why?
• If you were the supervisor of report writer A, what comments would you make on the report?
To writer B? To writer C?
1
MARCH 2000
-------
HANDOUT 14-2 A-
INSPECTION REPORT A: CASTINGS MANUFACTURING, INC
RCRA SAMPLING INSPECTION
This company manufactures steel castings for the railroad industry. The manufacturing facility occupies
forty acres on the northeast side of Bigcity. The 12-1 fl acre landfill owned by the company is located in
Rural County near Bubbatown to the southeast of the intersection of 4th and Main.
The purpose of this sampling inspection was to determine if waste generated and disposed of by this
facility at its Bubbatown landfill is RCRA hazardous waste. Hie main wastestream in question is a
mixture of electric arc furnace (EAF) dust and sand wash slurry. This dust/slurry mixture is claimed to
be nonhazardous by the facility. Other wastestreams of interest are from the five other dust collectors at
the facility.
On August 6,1986, Jim Sleuth, Sam Tweed, and Mike Heard of the USEPA Regional Office and Jean
Parker of the USEPA Regional Waste Management Division, conducted an unannounced sampling
inspection at the above-mentioned company. We arrived at the company landfill on 8/6/86 at 0915 to
wait for a truck to arrive from the company's manufacturing facility in BigcTity. A truck did arrive aF092S
but it was not hauling the type of waste desired to sample during the dump. It was later determined that
this load contained dust collector fines. At 094S another truck arrived at the landfill but it also was not
hauling the dust/slurry mixture desired to sample. At this time, Mr. Apple and Mr. Banana of the
company arrived at die landfill to inquire about the purpose of our inspection. We informed them that we
wished to sample'the dust/slury mixture asltwas teingdumped into th£ landfill: Mfr-Banans did not
know if any of this mixture would be disposed of that day and he asked us to return with him tolhe
Bigcity facility where he could determine when disposal of that material would occur. Before leaving for
the landfill, samples 86EF10S01 and S02 (see Table 1) were collected of the two loads that were dumped
that morning. These samples were split with the facility.
At 1115 a meeting was held with Mr. Cake, assistant works manager and Mr. Donut at the Bigcity
facility. It was determined that the sand wash system was not generating any slurry that day and that we
could not sample the EAF dust/sand slurry mixture until the following day. We then proceeded to collect
samples S03-S06.
On August 7,1986, Mr. Sleuth, Ms. Parker, and Mr. Heard returned to the facility In Bigcity and
collected samples S07-S10 (see Table 1). It was observed that a tanker truck of sand wash slurry was
mixed with a load of EAF dust at the facility. This truck was followed to the landfill, where it was
sampled while it was dumped. Before being dumped a core of the top ten to twelve inches of the load
was taken in a 2" diameter plastic tube; eight to ten inches of this material all appeared to be dry EAF
dust The bottom two inches were damp EAF dust (mixed with slurry). The contents of this core were
used for sample S14. As the truck was dumping, five jars (one quart in size) were collected of the
material coming out of the truck. The first two (chronologically) were composited and split as sample
S13, the third jar was discarded and the last two jars were composited and split as sample S12. At the
very end of the dump a quantity of dry EAF dust was observed to float out on top of the discharge. A
sample of this dry material (SI 1) was collected from the top of the dumped material after h was on the
ground. All samples collected except D09, S14, and S15 were split with the facility. The sampling
results can be found in Attachment 1. Samples D09, SI 1, and S14 were all found to exceed the EPA
toxicity limit of 1 ppm for cadmium and 5 ppm for lead.
2
MARCH 2000
-------
HANDOUT lf-2 A
Figure 1 - Landfill
August 647, 1986
NO SCALE
Lat* Dnti.
UtoAKiA/Q
yV0 ^*4
**rkSr
ovmtee /- *
(r/i-jiM)
Fill
-------
HANDOUT itf-lj-
TABLE I
Sample Locations
August 6 17, 1966
STA.
HO.
MTE
1986
TIKE
COMPOSITE
STATION
GRAB LOCATION
SOI
6-6
1006
X
Waste pile from load 12
so;
8-6
1030
X
Haste pile from load 11
so5
£.6
1327
X Carrier blast dust collector
S04
B-6
1338
x *fl0c*oiit~4ust collector
S05
£.6
1415
x Cabinet blast dust collector
SOS
8-6
1425
X Tumblast dust collector
307
1045
ii Sootn tnd-^and^systen -
SO?
8-7
1100
X Sand wash and wet scrubber slurry
S09
8-7
1100
X EAF dust (duplicate)
510
8-7
1300
X EAF dust
Sll
8-7
1420
X After duap (dust/slurry alxture)
S12
8-7
1418
X
Ust half of dunp *
S13
8-7
1414
X
First tulf of-tfmp "
S14
8-7
1410
X Core of load •
S15
8-7
1700
Blank
4
SEPTEMBER 1995
-------
ANAlVTICAt ftESULTS OF AUGUST 6 A ltd 7. 1986, SAMPLING
(•If retails ire In bum)
Simple
ftunfter
J3L
JL.
JL
Cr
Pb
• At
Se
J!i_
fluoride
Phenol
Cyanide
Haxlmum Contaminant Level
for IP Tonicity!
5.0
ioo.o
1.0
5.0
5.0
5.0
1.0
0.2
86CR10
SOI
<0.006
0.04?
<0;0l
<0.000
<0.07
<0.00*
<0.02
<0.0001
0.04
2.?
<1.0
SO?
<0.006
0.058
<0.01
<0.008
<0.0?
<0.002
<0.02
<0.0001
0.0?
6.8
<1.0
SO)
<0.006
0.078
<0.01
<0.008
<0.0?
<0.002
<0.02
<0.0001
0.1
4.6
<1.0
SOI
<0.006
o.tso
<0.01
<0.008
<0.07
<0.002
<0.02
40.0001
0.1
37.8
2.0
SOS
<0.006
0.049
<0.01
<0.008
<0.07
<0.002
<0.02
<0.0001
0.2
15.2
<1.0
SOS
<0.006
0.114
<0.1
0.08
<0.7
<0.002
<0.002
<0.0001
0.1
7.3
<1.0
so?
<0.006
0.116
<0.01
0.00892
<0.7
0.006
<0.002
<0.0001
0.2
68.2
2.0
SOS
0.006
0.114
<0.01
<0.008
<0.0?
I
3-
I
*
I
I
o
cn
s
tlmum contaminant level.
-------
HANDOUT 14-2 g
INSPECTION REPORT B: GRITTY WRECKING
December 2,1987
NESHAP Asbestos Demolition Inspection — Gritty Wrecking,
Urban, Michigan (A24535.00)
K. Eagle, Environmental Engineer
THRU: J. Medium
Engineering Section SAC
ATTB: S. Boss
This is the first in a series of inspection reportsintendcStoprovldc a complete discussion of a NESHAP
inspection (asbestos removal) at the former Consolation Company ("the facility") located at 1S21 East
First St., in Smallervitle, MI. The inspection was conducted on October 22,23,26-30, and November 2,
1987. An initial inspection of demolition occurring at the facility was conducted on October 22 and 23,
1987. On October 26-27, additional visits were made to the site to obtain measurements of the amount of
suspected "Sriibte Mntainiiig^^HflKFACM):stiilin1hcriaoHity indto obtain wrrect^
information is to which buildings were involved in the demolition project' Mr. Linus Lip of the EDO
was on she October 29,30 and November 2,1987, to oversee the entire asbestos abatement and to
observe deposition of the ACM waste after removal.
Background information about the facility, notification, amount of asbestos present, work practices,
worker safety and equipment, and waste handling at the facility are discussed in this repot Actual ACM
removal by an asbestos abatement contractor occurred October 29,30, and November 2,1987, and all
discussion of work practices, worker safety and equipment, amount of asbestos removed, waste handling
at the facility and waste transport and disposal by the abatement contractor will be forwarded in a second
report by Mr. Lip. Information about samples taken, sample analyses, and pictures of the site is provided
in the attachments (Attachment 4 - Summary of Samples Taken; Attachment 5 - Sample Analyses from
Laboratory, Attachment 6 - Pictures of Site).
Background
It is estimated that the facility was constructed in the early 1900s. The entire complex includes
approximately 35 buildings and encompasses 365 acres. The portion of the facility inspected included
buildings 2 through 8 at the west end of the complex, located at the corner of East First and East Front
Streets (Attachment 1 - Diagram of Complex). East of the facility is an industrial area and approximately
one quarter mile to the west begins a residential neighborhood. Downtown Smallerville is located
approximately one mile west of the facility. The city of Smallerville owns the complex and was
contracting out groups of buildings for demolition.
4
MARCH 2000
-------
HANDOUT 14-2 $
On the morning of October 22,1987, a call was made to the EDO from a contractor who had bid on this
particular job but did not win the contract. The contractor stated that he had bid $90,000 to do the
project, which would have included the asbestos removal necessary. He continued that Gritty Wrecking
of Urban, MI, has won the contract with the city with a bid of only $24,000. He said the buildings were
"full of asbestos" and that the project could not possibly be completed properly at that low a cost I left
that afternoon to inspect the site in Smallerville for possible noncompliance with NESHAP regulations
regarding asbestos removal prior to demolition.
Notification
Attached is the building permit (Attachment 2) obtained from Michael Edifice, Director of Building and
Zoning for the city of Smallerville, stating the buildings to be demolished by Gritty Wrecking per the
contract between Gritty Wrecking and the city of Smallerville (Attachment 3), and including the terms
for the handling of asbestos in the subject buildings.
No notification of demolition or intent to remove asbestos was submitted to any appropriate Michigan
agency or the federal government by Gritty Wrecking prior to beginning work.
Amount of Asbestos Present
Upon my initial inspection on October 22,1987,1 observed approximately 4S-S0 linear feet of pipe
lagged with dry, suspected FACM in Building 2. In addition, I observed large amounts of dry, suspected
f ACM lagging and-debris-Tn4h4Mubble^)e]ow pipes in the-same -building;^On October 23,1987rI
returned tothe site and entered Building-2-with P. Gradey,5uperintendenLfor Gritty -Wrecking, to
observe one of Gritty's employees removing asbestos. Inside I observed approximately 25 linear feet of
suspected ACM in the immediate area. Mr. Lip and I returned on October 26,1987, and entered what
was left of buildings 2 through 7. Within these buildings we measured an additional 230 linear feet of
suspected FACM lagging. There also was an open labeled asbestos waste bag filled with dry pipe
lagging in Building 3, and diy, suspected FACM lagging and debris on the floors, walls, and fixtures in
the buildings. We also observed seven bags of pipe lagging and three bags of a dry, suspected FACM
sheet material outside against a fence on the she. Hie asbestos abatement contractor (Scrub Abatement)
later estimated that there was at least 100 linear feet of lagging in those bags. When we entered the
buildixigagain on October 28,1987, we found an additional 8 feet of pipe lagged with suspected FACM
in Building 8.
Scrub Abatement had later been contracted by Gritty Wrecking to properly remove all of the asbestos in
the buildings involved in the demolition project. Their notice of intent to remove asbestos stated that 397
linear feet had been found which did not include the material in Building 2 noted previously since most
of that building had been demolished prior to Scrub's assessment
5
MARCH 2000
-------
HANDOUT 14-2 g
Inspection
Thursday. October 22.1987
As stated previously, a call was made to the EDO on the morning of October 22, 1987, regarding the
possibility that violations of the NESHAP, specifically asbestos removal, might have been occurring.
Acting on the information obtained, I went to Smallerville, Michigan, to inspect the facility in question. I
arrived at the site at 1615 EDT on October 22,1987, and found no demolition occurring although there
was a front-end loader there. I immediately observed pipes with dry, suspected FACM lagging in the
partially demolished Building 2. As I walked closer to Building 2,1 observed large amounts of white,
friable, suspected ACM in the rubble. I estimated that 45-50 feet of pipe contained suspected FACM
lagging in part of the Building 2 that was visible from the outside.
Five samples were taken from the material in the nibble and still on pipes (88EH01S01-S05), and four
were analyzed as positive for asbestos (Attachment S). Several pictures were taken of the building and
the suspected FACM (Attachments 4,5, and 6).
Friday. October 23.1987
On October 23,1987, at approximately 0915 EDT, I returned to the site to see if there was, in fact,
demolition in progress. I observed a man operating a front-end loader, knocking down Building 2. I also
observed a second man using a torch to cut pipes in the same building. ~ As the front-end loader was
knocking down Building 2,1 observed visible emissions. Sample 88EH01S06 was taken here later.
Shoi%4rfter,-thread ercperatef^eftBuilding^^nd proceeded iabegin-demolition on Building-4A>
I altered the site at 1140 EDT and spoke with the loader operator. He informed me that there was a man
inside the bail ding at that time removing asbestos from the pipes, but there was no foreman on the site at
that time and lie did not know when he'd return. I looked into the open end of Building 2 and saw a mm
using a torch but I did not eater at that time. I inspected the area of Building 2 where I had seen the
loader working and found much more pipe lagging in the nibble there than on October 22, but no more
lagging on the pipes above, which I had observed on those pipes the previous afternoon. I concluded it
had been knocked down during demolition.
A shot time later, the man that had been inside emerged from Building 2 wearing brown coveralls.
There was no sign of a respirator. He introduced himself as Emie McDoogle and produced his
certification paper for asbestos handling in Michigan. He informed me that he was not removing
asbestos but rattier cutting down the pipes containing suspected ACM, which were to be disposed of in
sections, pipe and lagging all together. He stripped off his coveralls, coated with white dust, hung them
over the back of his truck, and prepared for lunch.
I sampled the material (88EH01S06) where I had previously seen the visible emissions; it was later found
by the Central Regional Laboratory to contain 25%-35% amosite (Attachment 5). No foreman returned
to the site and I left at 1300 EDT.
I returned to the site at approximately 1430 EDT, and spoke with Paul Gradey, Superintendent from
Gritty Wrecking. He informed me that Emie McDoogle was inside removing asbestos. I asked him what
would be done about all of the pipe lagging laying in and around the rubble of Building 2 and he said he
did not know about that. I asked him where the bags of asbestos that were in the bade of his pickup truck
6
MARCH 2000
-------
HANDOUT 14-2 ?
were going and be said "in the river." Then he said they would be taken to Gritty^ shop in Urban until
they had a full load to transport to Payne Disposal in Oldville, Ml. He asked me if I wanted to see the
removal in progress inside and I followed him into Building 2. Inside I observed Mr. McDoogle
removing suspected asbestos from piles (contrary to what he'd told me) wearing his brown coveralls,
gloves, and dust mask. He had the pipes laying on the floor. He sliced open the dry lagging with a knife,
peeled the two halves off of the pipe, and stuffed them into a labeled asbestos waste bag. He was not
wetting the material and when I asked why, he said it was "wet enough." 1 observed visible emissions
when he removed the lagging from the pipe, but I did not sample the material. In that immediate area, I
observed approximately 25 feet of suspected ACM on pipes. I asked Mr. McDoogle if he had learned
about wetting the ACM, the glove bag technique, and protective equipment worn during asbestos
handling in his training course and he said yes. I left Building 2. I spoke more with Mr. Gradey outside
and a short time later I left die site.
The five samples I obtained on Thursday, October 22 and the sample obtained on October 23, from
where visible emissions were observed during demolition, were express mailed to the Central Regional
laboratory in Chicago at approximately 1630 EDT on Friday, October 23,19S7. As indicated previously,
analytical results are included in Attachment 5.
Monday. October 26.1987
On October 26,1987, at 1320 EST, Linus Lip of the EDO and I returned to the site. It was apparent that
a considerable amount of demolition work had occurred between Friday (October 23) evening and
Monday (October 26) morning despite Mr. Edifice's order to stop, because a large portion of Building 2
had been leveled.-No-one-was-on-site-butaoJaw was present besid& the-front-end loader
-------
HANDOUT 14-2 g
Wednesday. October 28.1987
On October 28,1987, at approximately 0800 EST, Linus Lip, Joe Lawstruck of the Office of Regional
Counsel, and 1 returned to die site on the comer of East First and East Front Streets. We entered the
facility through Building 2 to re-measure the amount of suspected FACM contained in all of the
buildings (2-8) that Gritty Wrecking was contracted to demolish. Including the 197 feet Mr. Lip and I
previously observed, we measured 286 linear feet of suspected ACM pipe lagging.
At 1030, Mr. Lip and I met with Mr. Lawstruck and Caroline Bemoose of the Air Compliance Branch;
Kenneth Chalk, Vice President of Operations for Gritty Wrecking and his lawyer Frank Gradey; Mr.
Edifice, Building Director for the city of Smallerville; the city of Smallerville's lawyer, Oliver Twist; and
the Assistant U.S. Attorney, Harry Marvel, at the U.S. Attorney's office in Urban.
At the meeting, all parties discussed potential violation of the NESHAP that occurred at the demolition
site and recommendations for the immediate correction of and compliance with NESHAP regulations
governing asbestos removal as h applied to this demolition.
Mr. Chalk agreed to contact Scrub Abatement, an asbestos abatement contractor, to begin removal the
following morning (October 29/1987) of all ACM in the buildings concerned. Mr. Lawstruck, Mr. Lip, -
and I agreed under lite condition that Mr. Lip or I were present throughout the ACM removal and
disposal.
At 1530 EST, Lany Lip spoke with Mr. Chalk and confirmed that Scrub Abatement would arrive on site
at 0730 on October 29 to assess the abatement job and begin removal of the ACM. Mr. Lip agreed to be
present on she for the entire ACM removal period which occurred on October 29,30 and November 2,
1987. The waste was transported to a landfill at 1530 EST on November 2, 1987.
A subsequent report will follow from Mr. Lip describing the actual amount of asbestos removed, work
practices, worker safety and equipment, waste handling at the facility, waste pickup, and waste transport
and disposal at the lunrifill Also, analyses of samples taken during ACM removal, and the field data
collection checklists, will follow in Mr. Lip's report.
8
MARCH 2000
-------
•iiiiin/iMXn.
n
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*" hmi iinMi
fSX>i
/ u »»niki ii
N -ft/Soli illiinLwn flto attmt
zjrri&r»ettttvr TJ¥
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i
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-------
Summary of Samples Taken
HANDOUT lV-2 f
SAMPLE NUMBER
TIME
SAMPLE DESCRIPTION SAMPLE ANALTSIS RESULTS
OCTOBER 22. 1987
68EH01S01 1647 EOT On red bricks
331-401 Anoslte
502 1655 EOT Ofl pipe
503 1705 COT On boards 1n rubble
S04
1730 EOT In rubble
321-351 Amosice;
81-121 Trenolite-ActlnoHte
201-251 Anoslte;
St-101 TremoHte-Actlnollte
351*401 Anoslte
S05
1736 EOT Brown fluff/
Negative
OCTOBER 23. 1987
88EK01S06 1210 EOT
Ubere visible emissions 251-351 Anoslte
observed during demolition
OCTOBER 26. 1967"
• -88EH01S07 1330 EST
Hanging on wall and on
floor Id building 2
S08 1343 EST Large vessel
S09 1630 EST Slumped on catwalk In
building 3
251-351 Anoslte;
11- SI Tremollte-ActlfloHte
51-101 Anoslte;
101-151 Chrjrsotlle
251-301 Anoslte
S10A 1640 EST Open bag In building 3 151-251 Anoslte
SlOft
1640 EST Open bag In building 3 Not Analyzed-Or/
Sll 1710 EST open bag outside -
sheet material
151-201 Anoslte;
11- 51 Chrysotlle
-------
Summary of Pictures Taken
HANDOUT lV-2 £
October 22. 1987:
EOT
Picture 1
1647
On bricks, outside Building 2, Sample SOI.
Picture 2
1647
Outside Building 2, In rubble.
Picture 3
16S5
Pipe lagging 1n Building 2, Sample S02.
Picture 4
170S
On boards, in rubble, 1n Building 2, Sample SO3
Picture S.
1710
In rubble, in Building 2.
Picture 6 17
1712
On ground in Building 2.
Picture 8
1715
Pipe lagging in Building 2.
Picture "9 I 10
1720
Building 2.
Picture 11
1730
On ground in Building 2, Sample S04.
Picture 12 I 13
1732
Pipes in Building 2.
Picture 14 - 21
1735-1815
Rubble in and around Building 2.
Picture 22
1820
View of demolition site from street.
October 23. 1987:
EOT
Picture 23 I 24 1210
Picture 25 ISIS
Building 2, where visible emissions were observed
during demolition, Sample S06.
Truck driven by Paul Garvaglla.asbestos bags In
back.?
October 26. 1987;
EST
Picture
Picture
Picture
Picture
Picture
PIcture
P1cture
Picture
Picture
Picture
Picture
26
- 31
132Q
Appearance of Building 2 after the weekend.
32
t 33
1330
Inside Building 2, Sample S07.
34
133S
Inside Building 3.
35
1343
Large vessel inside Building 3, Sample S08.
36
* 37
1345
Pipes In Building 3.
38
1400
Rubble outside Building 2.
39
*,40
1405
Outside Building 5A.
41
- 45
1410
Bags outside, against fence, Sampl« SI1.
46
1630
ACM slumped on catwalk in Building 3, Sample S09
47
( 48
1640
Open bag of dry FACH in Building 3, Sample S10.
49
1655
Pallets in Building 5.
-------
15
-------
SESSION 15
TOPIC: ENFORCEMENT PROCESS RESPONSIBILITIES
Time: 60 minutes
Purpose
Key points
List of Visuals
Describe what to expect when appearing as a witness
Present tips for testifying at a deposition or trial
Demonstrate questioning, examination, and cross-examination
Discuss role of inspectors in settlement and other negotiations
Provide tips for effective negotiations
Prepare well in advance. Don't volunteer information
Prepare carefully, know all the facts and options Resolve differences
internally, not in front of the other side
Understand negotiation; most cases are settled through negotiation, not
trials
15-1
Enforcement Process Responsibilities (Title Slide)
15-2
Trial/Hearing or Deposition
15-3
Common Misconceptions
15-4
The Legal Framework
15-5
Our Adversary System
15-6
Discovery Rules
15-7
Rules of Evidence
15-8
Hearsay
15-9
Keys to Effective Testimony
15-10
Documenting investigative Activities
15-11
Role of the Inspector/Witness
15-12
Expert Witness
15-13 and 14
Preparation for Testimony
15-15
Depositions
15-16
Depositions/Setting
15-17 to 19
Hearings/Trials
15-20
Trick Questions
15-21 and 22
Universal Witness Guidelines
15-23
Negotiations
15-24
Preparation for Negotiations' Role of the Inspector
15-25
Negotiation Fundamentals
15-26 and 27
Supplemental Environmental Projects
15-28
Categories of SEPs
15-29
Unallowable SEPs
1
JULY 2000
-------
Enforcement Process
Responsibilities
Trial/Hearing or Deposition
Testimony
Negotiations
Supplemental Environmental Projects
(SEPs)
Trial/Hearing or Deposition
Testimony
•Common Misconceptions
¦The Legal Framework
¦Keys to Effective Testimony
¦Depositions/T rials/Hearings
Common Misconceptions
•"This case will never go to trial, so why
wony about the details"
•"I know what I'm testifying on, so 1 don't
need to prepare"
•"If I get into trouble, my lawyer will protect
. _ »>
me
-------
The Legal Framework
"Adversary System of Justice
" Discover)' Rules
"Rules of Evidence
"Burden of Proof
Our Adversary System
"Investigation
0 Complaint/Indictment
"Discovery
"Trial/Hearing
Discovery Rules
"Civil Judicial Cases
" Documents
" Interrogatories
" Expert reports
o Depositions
"Civil Administrative Cases
"Criminal cases
o Rule 16/Jencks Act
° Brady Rule
114
2
-------
Rules of Evidence
•All Evidence Musi Be
0 Relevant
° Competent
° Authentic
•Expert Opinions Musi Be
° Relevant
0 Reliable
"Hearsay"
• Out of court statement offered in court to
prove the truth of the matter asserted
•General rule hearsay is not admissible.
•Numerous exceptions allow for admission of
reliable hearsay.
* Exceptions may apply to scientific data,
laboratory reports and public records.
Keys to Effective Testimony
•From outset, fully understand case and role
• Carefully document work during investigation
• Know limits of expertise
•Prepare for testimony
3
-------
Documenting Investigative Activities
•Assume you will need 10 reconstruct events at
trial-from first dav on case
¦As appropriate, include detailed information on
facility operations and processes
¦Fully describe protocols used, field
measurements, sampling and equipment
Role of the Inspector/Witness
¦ Fact witness
¦"Summary" witness
• Expert witness
•Consultant
Expert Witnesses
•Experts qualified based upon knowledge,
skill, experience, training or education
¦ Testimony permitted if n would be helpful
to trier of fact
•Proposed rules require that expert provide
opinions on scientific or technical matters
IMl
4
-------
Preparation for Testimony
¦ Work closely with counsel
¦Review pertinent records
0 Government files
0 Discovery from defendant
¦ Understand case
° Theory of case/ elements of proof
° Your role in proving elements
0 Weaknesses in evidence
Preparation for Testimony-2
¦Understand nature of proceedings
° Deposition
° TnaJ/Heanng
¦ Know audience/understand impact of demeanor
¦Be familiar with exhibits
¦Rehearse, but do not memorize testimony
Depositions
•Purpose of Deposition
° Obtain explanation of basis for case
® Discover expert opinions
° Prepare for cross-examination
¦ Legal Standards
° "(treasonably calculated to lead to the
discovery of admissible evidence "
° Privileges/instructions not to answer
° Depositions taken subject to objections
5
-------
Depositions /Setting
•Conference room
¦Court reporter/no judge
¦Counsel control conduct of deposition
¦Witness can confer with counsel
¦Testimony is under oath
IVH
Hearings/Trials
¦In general
0 First moment "an out of body experience"
° relax, listen to questions carefully
o Simplify presentation/translate into plain English
° use visual aids /refer to documents
¦Direct examination (government's case)
° Witness qualifications/expertise
¦ Descnpuon of work
° Opinion testimony (if an expert)
Heannas/Trials-2
¦ Cross-examination-purpose
° Impeach/discredit
¦ Expose inconsistencies/weaknesses
¦ Limit effect of direct testimony
¦Handling Cross-Examination
° Know case (both sides)
o Expect convoluted/leading questions
° Expect dtsnipuve antics by counsel
¦ Listen carefully/stay calm
» DO NOT VOLUNTEER'
¦ Admit lack of knowledge
6
-------
Hearinqs/Trials-3
¦Objective is to show that:
D Personnel were qualified
0 Chain-of-custod) was intact
° Appropriate sampling/analytical methods were
used
° Data obtained were reliable
0 Expert opinions were reliable
Trick questions
¦ Is there "anything else" or "ts that all0"
•Did you talk with your attorney (1 e the
government's attorney) before testifying?
¦Have you ever made a mistake?
• Isn't it possible that.. 9
Universal Witness Guidelines
¦Tell the truth
•Listen carefully
•DO NOT VOLUNTEER
•Do not answer convoluted /ambiguous
questions
7
-------
Universal Witness Guidelines-2
¦Do not speculate
•Be warv of opposing counsel's restatement
of testimony
•Use words not gestures
• Remain calm and courteous
Negotiations
Purposes of negotiations
• Management of
negotiations
Preparation for Negotiations: Role
of the Inspector
¦Complete investigation, collect information
¦Assist in the analysis of the information
¦ Participate in internal negotiations
¦ Assist in developing strategy and credible
proposals
-------
Negotiation Fundamentals
•Plan roles and approach
¦Plan for caucuses/external communications
¦Have inspector attend negotiations
Supplemental Environmental
Projects
¦To further EPA's goals to protect and enhance
public health and the environment
¦To obtain protection that might not occur
otherwise
Supplemental Environmental
Projects
¦ Pollution prevention
Environmental justice
-------
Categories of SEPs
• Public health
• Pollution prevention
¦ Pollution reduction
• Environmental restoration and protection
• Assessments and audits
• Environmental compliance promotion
• Emergency planning and preparedness
Unallowable SEPs
¦ General public education
¦ University research
• Projects unrelated to environmental protection
• Studies without commitment
¦ Projects funded by low-interest federal loans
or grants
)
-------
Handout 15-1
THE CASE OF THE UNMANAGED NEGOTIATION
Sam Acosta bss just become acting chief of the RCRA Enforcement Section. Previously, he was in the
RCRA State Programs Section. He finds a short action memorandum on his desk from Bill Sanders, a
RCRA inspector. The memorandum recommends that EPA issue an administrative order to a hazardous
waste treatment facility called Treatment Supreme (TS) for violations of interim status requirements related
to security of the site and manifests. Sanders wrote that during an inspection he observed that a 25-foot
segment of fencing along a highway at the back of the TS facility was missing. He also noted that TS had
failed to note discrepancies on manifests for 75 shipments of one waste stream, analysis of which
performed by TS did not confirm that the waste was as represented by the generator. He attached a copy
of the draft administrative order requiring restoration of tne fence, prohibiting further receipt of the waste
stream, and assessing a $25,000 penalty. Sanders noted that copies of the manifests and laboratory reports
were in the inspection file. Sanders has been detailed under an Intergovernmental Personnel Agreement
(IPA) to the state for a year.
Acosta signs off on the action memorandum and sends it to his boss. It eventually is sent to the Regional
Counsel's office for legal review and is assigned to Laura Smith. Smith's main job at EPA has been to
handle the legal aspects of construction grants for sewerage treatment facilities. This is her first
enforcement case. She is instructed that the program office is responsible for substantive determinations
and her role is to ensure the order is legally sustainable, to assist die program office in any resultant
negotiations, and to represent.the program office in any subsequent appeals^She reviews the order and
action memorandum and determines that the violations alleged are sufficient to support the remedies sought
and are supported in the action memorandum. She compares the draft order with agency guidance and
makes some changes to conform it to the guidance. She signs off on the order, and it is eventually issued.
Guy Laredo, attorney for TS, calls Smith to request a conference on the order; he hopes to negotiate a
mutualj^-acccptoble resolution ^Smith-indicates she must check Acosta's calendar, they arrange .three,
possible tunes, depending on Acosta's availability. She calls Acosta, settles on a date three weelcs hence,
and makes arrangements to meet with "Acosta that afternoon to review the case.
When Smith and Acosta meet, they review the action memorandum and order. Smith asks to see copies of
Sander's inspection report and the manifests at issue. She asks whether they can talk to Sanders, but Sam
says he has beat detailed under an IPA to the state. They agree that the case seems open and shut and that,
nnder EPA's penalty guidance, they can agree to mitigate the penalty only to $18,000. They agree that
Smith will be the spokesperson in the negotiations. They tell both of their superiors that they intend to
settle for the substantive relief set forth in the order and a penalty of from SIS,000 to $25,000. Their,
supervisors concur.
As the date of the meeting approaches, Smith attempts to meet again with Acosta, but, because they are
both out of the office much of the time, they do not connect The day before the meeting, Smith attempts to
anange for a conference room, but they already have been claimed. Instead, she arranges to meet in
Acosta's office, which is larger than has.
On the date of the meeting, Smith goes to Acosta's office five minutes before the meeting, telling the
receptionist to ring her there when Larado and TS arrive. Larado, however, is familiar with the EPA office
and proceeds directly to Smith's office, never coming near the receptionist. Smith's secretary is not there,
and no one knows where she is. Both negotiating teams remain in splendid isolation until Smith's secretary
returns, discovers the situation, and calls Smith. Smith returns to her office, meets the TS group — the
plant manager, chief chemist, staff attorney, consulting attorney, and customer's plant manager and
attorney — and escorts them to Acosta's office. There are only four chairs in Acosta's office. Acosta and
Smith scurry around to find four more chairs. Acosta sits at die desk, Smith sits beside it, and the TS
group crowds in front of the desk, filling all the space between it and the door. The room is not large
enough to hold them all comfortably.
Smith opens the meeting by introducing herself and Acosta and inviting the TS group to do the same. She
apologizes for the confusion and for the cramped quarters. She then outlines die violations alleged and the
12 MARCH 2000
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Handout 15-1
enforcement procedures. She emphasizes EPA's view of the importance and gravity of the violations and
states that EPA would like to determine whether there is a basis for settling the matter. She indicates the
substantive violations must be corrected expeditiously. Finally, she states that EPA "really would like to
get a penalty of around $18,000 to $20,000."
Guy Larado, the consulting attorney for TS, opens his argument by stating that TS explained both
situations to the EPA inspector when he was on site and that TS believes the complaint is a mistake. He
asks whether the inspector is coming to the meeting. Acosta says the inspector has been detailed under an
IP A to the state and is not available. Larado expresses dismay, since TS already has been through the
issue with the inspector.
Larado then said there was indeed a 25-foot section of fence missing the day the inspector was there, as a
result of an automobile accident on the highway. The fence was scheduled for repair within the week and,
in fact, was repaired two days later. The fence, incidentally, was a 10-foot-high, electrified, chain-link
fence, topped with concertina wire, a far more protective fence than was required or was customary in the
trade. He produced pictures of the fence; a notarized affidavit from the repair company stating when it was
repaired/and a copy of a letter to the inspector, with copies of the pictures and affidavit Acosta slated he
was satisfied that the violation had been corrected. Smith said that a penalty might be authorized legally,
but that, equitably, it should be mitigated to zero, since the hole in the fence had been caused by a third
parly beyond the control of TS. TS had scheduled its repair before the inspection and had repaired the
-fence immediately afterthe inspection, and the fence was for better than required by EPA's-iegulations.
Acosta then said, "Let's talk about the manifest violation."
Larado said TS also had discussed that issue with the inspector. The waste stream in question was being
delisted when the inspection took place and subsequently was delisted, so it was not a hazardous waste at
all. TS's customer produced a copy of the delisting document and the accompanying Federal Register
notice. iarado said that-TS had written the inspector, enclosing a copy of the delisting document and
notice. Smith asked Acosta whether copies of TS's letters to the inspector were in his files, because there
were none in hers. Acosta answered that he did not know, but looked through his file and found both
letters.
Larado said that TS could argue that, since the waste stream had been delisted by EPA, EPA acknowledged
that it was never really hazardous waste, and, therefore, TS never really violated the manifest requirements.
He said TS would forgo that argument for the sake of settlement, if EPA would acknowledge thai, because
the waste stream was not hazardous, the violations were technical and there was no damage done to the
environment or the regulatory scheme and a de minimis penalty, if any, was appropriate. He offered
$2,500. Acosta said that settlement was acceptable but that the violations found raised a question about
the integrity of TS's system for handling manifests and its waste analysis plan. Larado answered that
EPA's inspector had found no other problems, but TS would hire an auditor to review its system and would
follow the auditor's recommendations if defects were found. Acosta asked whether TS would agree to put a
requirement for that action in a consent order, and Larado agreed. Larado said that there appeared to be
agreement TS would settle for a $2,500 penalty and an agreement to audit TS's manifest system and
correct any deficiencies. At that point, Smith said she thought EPA's penalty policy would require more
than $2,500 for the admitted violations. Larado said Acosta already had agreed to the $2,500 figure.
Acosta said he had not agreed to the figure, and that he had agreed only that, because of die facts, a
relatively low penalty seemed appropriate. Larado asked how much, and Acosta asked Smith whether she
thought $5,000 would be enough. Sne said she did not know. Larado said TS would write a check for
$4,000 and deliver it immediately to settle the matter. Acosta said he did not think a settlement could be
reached so quickly, since it would require concurrence of senior staff. That process usually took at least
two weeks, ne said.
Larado, who, until this point, had been soft-spoken, polite, and charming, became red in the face and began
speaking in a louder voice, touched with anger. He protested that he had spoken at length with the
inspector about the importance of a quick resolution of the matter. TS was about to close major financing
to construct three new state-of-the-art incinerators in another EPA region end was required to certify &
clean regulatory bill of health to secure the financing. He said the inspector had assured him that, if EPA's
13 MARCH 2000
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Handout 15-1
negotiators could sign off on a settlement, die matter could be handled in a matter of days. Larado said he
was dumbfounded that EPA would hold up so important a matter when it agreed the violations were trivial
and of no consequence.
Acosta asked Smith whether she saw any reason not to agree to the settlement outlined. She said she had
not seen enough of the problems to be sure. Acosta said that, as far as he was concerned, the violations, as
explained, were technical; the solutions were adequate; and the penalty appropriate. Smith said he was the
client and if he was satisfied, she was. Larado then drew up a letter of agreement, which both parties
initialed, and Smith agreed to turn into a consent order that afternoon. That afternoon, Smith talked to
Sanders, the inspector, by phone. He confirmed that he had indicated the possibility of quick action if
agreement was reached, but said the agreement was inappropriate. The break in the fence indeed had been
caused by an automobile accident and had been repaired immediately after the inspection. But the break
had occurred four months earlier, and the repair was not ordered until after TS knew an inspection had
been scheduled. The fence was indeed far better than those around most disposal facilities. But installation
of the fence had been ordered by the state after previous fencing had proven inadequate to prevent repeated
damage by vandals. TS was correct that the waste stream involved in the manifest violations had been
delisted. But the real question was whether the shipments received really were of that waste stream, or
whether TS had been accepting a nonpermhted waste. Indeed, Sanders wondered whether he had made a
mistake in not recommending action against TS's customer for sending a waste to a disposal facility not
permitted to take die waste. He was surprised that Smith was unaware of those facts, because most of the
information was inthe handwritten notes that he was sure were in the file somewhere.
At this point, EPA's negotiating team recognized that it was in an embarrassing situation.
14
MARCH 2000
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HANDOUT 15-2
CRUSH AND DESTROY NEGOTIATION
L General Instructions
The facts presented below are based on actual EPA cases, but the information has been modified and
supplemented to facilitate this exercise. Participants should use only the information provided in this fact
sheet, along with their knowledge of the Clean Air Act and EPA regulations. While participants may have
only limited specific knowledge of the requirements, they can use the general principles of negotiation to
develop a strategy. Logical inferences may be made from the facts, lie objective of this exercise is to
reach agreement on a plan for conducting a negotiation with the defendant in the case described below. In
developing the strategy, consider.
• What items are negotiable and nonnegotiable for EPA
• Strengths and potential weaknesses in EPA's position
¦ The role (if any) of the state
• Options for specific remedial steps to be required
• Factors that could be considered in adjusting the amount of the penalty
EL Facts
A. The Company
Crush and Destroy, Inc. (C&D) demolishes industrial and commercial structures. It has been in business
about 20 years, operating in the state of Maryland. C&D is a closely held, family-operated business that
employs 10 people. CAD'S gross revenues, are approximately $400,000 per year, and its assets areslightly
less than $100,000. Two years ago, the company earned $40,000. Last year, C&D lost $20,000.
B. The Violations
Several months ago, C&D was demolishing sections of an apartment building. In doing so, it uncovered
friable (crumbly) asbestos material This fact became known to the tenants of the standing portions of the
building who, concerned about the well-publicized effects of asbestos, contacted EPA. Several days lata,
EPA sent an inspector to the she. Hie inspector observed C&D"s operation and noted several violations.
First, C&D workers threw dry asbestos waste material onto the back of an open truck and transported it to
a local landfill, where they dumped the material. These actions violated 40 CFR 61.147(e), which reauires
that asbestos waste material be kept wet until it is collected for disposal; and 40 CFR 61.152(b), which
requires that asbestos waste material be property contained, transported, and disposed of. Finally, in
violation of 40 CFR 61.146, C&D failed to notify EPA in advance of its demolition work at the apartment
building.
1
MARCH 2000
-------
16
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SESSION 16
TOPIC: MOCK TRIAL
Time: 45 minutes
PURPOSE • Introduce participant to die realities of what can result
from their inspection.
Key POINTS * Inspectors must be accurate and thorough in their
inspections and follow-up record keeping.
List of Visuals 16-1 Mock Trial (Title Slide)
1
MARCH 2000
-------
Mock Trial
-------
17
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SESSION 17
TOPIC: AGENCY/REGENCY INITIATIVES
Time: 60 minutes
Purpose • Allow the region or host organization to address EPA or Regional
initiatives not addressed elsewhere in the course
MARCH 2000
-------
Agency/Regency Initiatives
-------
18
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SESSION 18
TOPIC: INTRODUCTION TO CRIMINAL INVESTIGATIONS
Time: 180 minutes
PURPOSE * Introduce inspectors to criminal enforcement and explain how to
recognize potential criminal violations.
• Provide an overview of criminal litigation
i
MARCH 2000
-------
Introduction to Criminal
Investigations
Principal Differences Between Civil
and Criminal Enforcement
• Warrants based on "probable cause"
• Other constitutional guarantees
¦ Burden of proof 'beyond a reasonable doubt"
• More severe penalties: imprisonment or fine
"Red Flags" That Indicate Possible
Criminal] Activity
• Conflicting da»
¦ Conflicting stories
¦ Unsubstantiated data
• Deliberate actions
• Claims of ignorance about requirements
-------
19
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SESSION 19
TOPIC: WRAP-UP AND EVALUATION
Time: 60 minutes
PURPOSE • Answer any questions outstanding and to obtain an evaluation of the
overall course.
KEY Points • Students and instructors will identify any key points or areas that should
be addressed.
LIST OF VISUALS • 19-1 Wrap-Up and Evaluation (Title Slide)
List of HANDOUTS • Course Evaluation
i
MARCH 2000
-------
Wrap-Up and Evaluation
AJ&r U.S&A
i
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20
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m
ZPA S30-b- ?
Me Tod 1624 Revision B
c .PAANIC COMPO1
BV
Method 1625 Revision t
SEMIVOLATILE ORGANIC OMPOUNDS BY
I! 3 OF *: DiLl nc •; GC /!
U.S. I
Office of Watei RegulCfions and Standard
industrial Technology Division
mi
-------
Method 1624 Revision B
VOLATILE ORGANIC COMPOUNDS BY ISOTOPE DILUTION GC/MS
1 SCOPE AND APPLICATION
1 1 This method is designed to determine the volatile 1 4
toxic organic pollutants associated with the 1976
Consent Decree and additional compounds
amenable to purge and trap gas chromatography-
mass spectrometry (GC/MS)
1 2 The chemical compounds listed in table 1 may be
determined in municipal and industrial discharges by
this method The method is designed to meet the 2
survey requirements of EPA's Industrial Technology 2 1
Division (ITD) and the National Pollutants Discharge
Elimination System (NPDES) under 40 CFR 136 1
and 136 5 Any modifications of this method, beyond
those expressly permitted, shall be considered as
major modifications subject to application and ap-
proval of alternate test procedures under 40 CFR
136 4 and 136 5
1 3 The detection limit of this method is usually depen-
dent on the level of interferences rather than in-
strumental limitations The limits in table 2 represent
the minimum quantity that can be detected with no in-
terferences present
TABLE 1
Volatile Organic Compounds Analyzed by Isotope Dilution GCMS
POLLUTANT LABELED COMPOUND
COMPOUND
STORET
CAS
EGD
NPDES
ANALOG CAS
EGD
acetone
81552
67-64-1
516 V
de
666-52-4
616
V
acrolein
34210
107-02-8
002 V
001
V
d<
33984-05-3
202
V
acrylonitnle
34215
107-13-1
003 V
002
V
d3
53807-26-4
203
V
benzene
34030
71-43-2
004 V
003
V
de
1076-43-3
204
V
bromodichloromethane
32101
75-27-4
048 V
012
V
,3C
93952-10-4
248
V
bromoform
32104
75-25-2
047 V
005
V
,3C
72802-81-4
247
V
bromomethane
34413
74-83-9
046 V
020
V
d3
1111 -88-2
246
V
carbon tetrachloride
32102
56-23-5
006 V
006
V
,3C
32488-50-9
206
V
chlorobenzene
34301
108-90-7
007 V
007
V
d5
3114-55-4
207
V
chloroethane
34311
75-00-3
016 V
009
V
d5
19199-91-8
216
V
2-chloroethylvinyl ether
34576
110-75-8
019 V
010
V
Chloroform
32106
67-66-3
023 V
011
V
,3C
31717-44-9
223
V
chloromethane
34418
74-87-3
045 V
021
V
d3
1111 -89-3
245
V
dibromochloromethane
32105
124-48-1
051 V
008
V
,3C
93951-99-6
251
V
1 1-dichloroethane
34496
75-34-3
013 V
014
V
d3
56912-77-7
213
V
1,2-dichloroethane
32103
107-06-2
010 V
015
V
d<
1 7070-07-0
210
V
1,1-dichloroethene
34501
75-35-4
029 V
016
V
d2
22280-73-5
229
V
trans-1,2-dichlorethene
34546
156-60-5
030 V
026
V
d3
42366-47-2
230
V
1,2-dichloropropane
34541
78-87-5
032 V
017
V
de
93952-08-0
232
V
trans-1,3-dichloropropene
34699
10061-02-6
033 V
d4
93951-86-1
233
V
diethyl elher
81576
60-29-7
515 V
dio
2679-89-2
615
V
p-dioxane
81582
123-91-1
527 V
de
1 7647-74-4
627
V
ethylbenzene
34371
100-41-4
038 V
019
V
dio
25837-05-2
238
V
methylene chloride
34423
75-09-2
044 V
022
V
d2
1665-00-5
244
V
methyl ethyl ketone
81595
78-93-3
514 V
d3
53389-26-7
614
V
1.1,2,2-tetrachloroelhane
34516
79-34-5
015 V
023
V
dj
33685-54-0
215
V
tetrachlorethene
34475
127-18-4
085 V
024
V
,3C2
32488-49-6
285
V
toluene
34010
108-88-3
086 V
025
V
de
2037-26-5
286
V
1,1,1-lrichloroethane
34506
71-55-6
011 V
027
V
d3
2747-58-2
211
V
1.1,2-lrichloroethane
34511
79-00-5
014 V
028
V
,3C2
93952-09-1
214
V
trichloroethene
39180
79-01-6
087 V
029
V
,3c2
93952-00-2
287
V
vinyl chloride
39175
75-01-4
088 V
031
V
d3
6745-35-3
288
V
The GC/MS portions of this method are for use only
by analysts experienced with GC/MS or under the
close supervision of such qualified persons
Laboratories unfamiliar with the analyses of en-
vironmental samples by GC/MS should run the per-
formance tests in reference 1 before beginning
SUMMARY OF METHOD
Stable isotopically labeled analogs of the com-
pounds of interest are added to a 5 mL water sample
The sample is purged at 20-25 °C with an inert gas in
a specially designed chamber The volatile organic
compounds are transferred from the aqueous phase
into the gaseous phase where they are passed into a
sorbent column and trapped After purging is com-
pleted, the trap is backflushed and heated rapidly to
desorb the compounds into a gas chromatograph
(GC) The compounds are separated by the GC and
detected by a mass spectrometer (MS) (references 2
and 3) The labeled compounds serve to correct the
variability of the analytical technique
1
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TABLE 2
Gas Chromatography of Purgeable Organic Compounds by Isotope Dilution GC/MS
EGD
REF
MEAN
MINIMUM
NO
EGD
RETENTION
LEVEL (2)
(D
COMPOUND
NO
TIME (SEC)
(MQ/L)
181
bromochloromethane (internal slandard)
181
730
10
245
chloromethane-d3
181
147
50
345
chloromethane
245
148
50
246
bromomethane-dj
181
243
50
346
bromomethane
246
246
50
288
vinyl chloride-ds
181
301
50
388
vinyl chloride
288
304
50
216
chioroetnane-ds
181
378
50
316
chloroethane
216
386
50
244
methylene chlonde-d2
181
512
10
344
methylene chloride
244
517
10
616
acetone-ds
181
554
50
716
acetone
616
565
50
002
acrolein
181
566
50
203
acrylonitnle-da
181
606
50
303
acrylonitrile
203
612
50
229
l,l-dichloroethene-d2
181
696
10
329
1,1-dichloroethene
229
696
10
213
l,l-dichloroethane-d3
181
¦ 778
10
313
1,1-dichloroethane
213
786
10
615
diethyl ether-d10
181
804
50
715
diethyl elher
615
820
50
230
trans-1,2-dichloroethene-
-------
2 2 Identification of a compound (qualitative analysis) is
performed by comparing the GC retention time and
the background corrected characteristic spectral
masses with those of authentic standards
2 3 Quantitative analysis is performed by GC/MS using
extracted ion current profile (EICP) areas Isotope
dilution is used when labeled compounds are
available, otherwise, an internal or external standard
method is used
2 4 Quality is assured through reproducible calibration
and testing of the purge and trap and GC/MS
systems
3 CONTAMINATION AND INTERFERENCES
3 1 Impurities in the purge gas, organic compounds out-
gassing from the plumbing upstream of the trap, and
solvent vapors in the laboratory account for the
majority of contamination problems The analytical
system is demonstrated to be free from interferences
under conditions of the analysis by analyzing blanks
initially and with each sample lot (samples analyzed
on the same 8 hr shift), as described in section 8 5
3 2 Samples can be contaminated by diffusion of volatile
organic compounds (particularly methylene chloride)
through the bottle seal during shipment and storage
A field blank prepared from reagent water and
carried through the sampling and handling protocol
serves as a check on such contamination
3 3 Contamination by carry-over can occur when high
level and low level samples are analyzed sequen-
tially To reduce carry-over, the purging device and
sample syringe are rinsed between samples with
reagent water When an unusually concentrated
sample is encountered, it is followed by analysis of a
reagent water blank to check for carry-over For
samples containing large amounts of water soluble
materials, suspended solids, high boiling com-
pounds, or high levels of purgeable compounds, the
purge device is washed with soap solution, rinsed
with tap and distilled water, and dried in an oven at
100-125 °C The trap and other parts of the system
are also subject to contamination, therefore, frequent
bakeout and purging of the entire system may be
required
3 4 Interferences resulting from samples will vary con-
siderably from source to source, depending on the
diversity of the industrial complex or municipality
being sampled
4 SAFETY
4 1 The toxicity or carcinogenicity of each compound or
reagent used in this method has not been precisely
determined, however, each chemical compound
should be treated as a potential health hazard
Exposure to these compounds should be reduced to
the lowest possible level The laboratory is responsi-
ble for maintaining a current awareness file of OSHA
regulations regarding the safe handling of the
chemicals specified in this method A reference file
of data handling sheets should also be made
available to all personnel involved in these analyses
Additional information on laboratory safety can be
found in references 4-6
4 2 The following compounds covered by this method
have been tentatively classified as known or
suspected human or mammalian carcinogens
benzene, carbon tetrachloride, chloroform, and vinyl
chloride Primary standards of these toxic com-
pounds should be prepared in a hood, and a
NIOSH/MESA approved toxic gas respirator should
be worn when high concentrations are handled
5 APPARATUS AND MATERIALS
5 1 Sample bottles for discrete sampling
5 1 1 Bottle—25 to 40 ml. with screw cap (Pierce 13075,
or equivalent) Detergent wash, rinse with tap and
distilled water, and dry at >105°C for one hour
minumum before use
512 Septum—Teflon-faced silicone (Pierce 12722, or
equivalent), cleaned as above and baked at
100-200 °C for one hour minumum
52
521
522
5 22 1
Purge and trap device—consists of purging device,
trap, and desorber Complete devices are commer-
cially available
Purging device—designed to accept 5 mL samples
with water column at least 3 cm deep The volume of
the gaseous head space between the water and trap
shall be less than 15 mL The purge gas shall be in-
troduced less than 5 mm from the base of the water
column and shall pass through the water as bubbles
with a diameter less than 3 mm The purging device
shown in figure 1 meets these criteria
OPTION At
FOAM TRAP
EXTT 1/4 IN OD
«— U MM OO
INLET IN OD
OOT tM IN OD
10 MM GLASS FRIT
medium porosity
SAMPLE INLET
2 WAY SYRINGE VALVE
17 CM 20 GAUGE SYRINGE NEEDLE
8 MM 00 RUBBER SEPTUM
INLET 11' (NOD
U16 IN OD
/ STAINLESS steel
13X
MOLECULAR SIEVE
PURGE OAS FILTER
RJRGE GAS
1 FLOW CONTROL
FIGURE 1 Purging Device.
Trap—25 to 30 cm x 2 5 mm i d minimum, contain-
ing the following
Methyl silicone packing—one±0 2 cm, 3 percent
OV-1 on 60/80 mesh Chromosorb W, or equivalent
3
-------
5222
5223
Porous polymer— 15± 1 0 cm, Tenax GC
(2,6-diphenylene oxide polymer), 60/80 mesh,
chromatographic grade, or equivalent
Silica gel—8±10 cm, Davison Chemical, 35/60
mesh, grade 15, or equivalent The trap shown in
figure 2 meets these specifications
PACKING DETAIL
CONSTRUCTION DETAIL
5 MM GLASS WOOL
7 7 CM SILICA GEL
COMPRESSION
FITTING NUT
ANO FERRULES
14 FT 7fl/FOOT
RESISTANCE WIRE
WRAPPED SOLID
1SCMTENAXGC
1 CM 3% OV 1
j- 5 MM GLASS WOOL
THERMOCOUPLE/
CONTROLLER
SENSOR
ELECTRONIC
TEMPERATURE
CONTROL AND
PYROMETER
TUBING 25 CM
0105 IN ID
0125 IN OD
STAINLESS STEEL
523
524
FIGURE 2 Trap Packings and Construction to
Include Desorb Capability.
Desorber—shall heat the trap to 175±5°C, in 45
seconds or less The polymer section of the trap shall
not exceed 180°C, and the remaining sections shall
not exceed 220°C The desorber shown in figure 2
meets these specifications
The purge and trap device may be a separate unit or
coupled to a GC as shown in figures 3 and 4
CARRIER GAS
FLOW CONTROL
LIQUID INJECTION PORTS
COLUMN OVEN
OPTIONAL 4-PORT COLUMN
SELECTION VALVE
REGULATOR
9-PORT
VALVE
CONFIRMATORY COLUMN
TO DETECTOR
ANALYTICAL COLUMN
13X MOLECULAR
SIEVE FILTER
V 1.1 PURGING
11 OEVtCE
NOTE.
ALL UNES BETWEEN TRAP
AND GC SHOULD 8E HEATED
TO eo*c
FIGURE 3 Schematic of Purge and Trap
Device-Purge Mode
5 3 1
5 4
CARRIER GAS
FLOW CONTROL
LIQUID INJECTION PORTS
COLUMN OVEN
OPTIONAL « PORT COLUMN
SELECTION VALVE
REGULATOR
TRAP INLET
S-PORT
VALVE
CONFIRMATORY COLUMN
TO DETECTOR
ANALYTICAL COLUMN
PURGE GAS
FLOW CONTROL
13X MOLECULAR
SIEVE FILTER
|i PURGING
1 1 OEVtCE
NOTE.
ALL LINES BETWEEN TRAP
ANO GC SHOULD BE HEATED
TO arc
53
FIGURE 4 Schematic of Purge and Trap
Device-Desorb Mode.
Gas chromatograph—shall be linearly temperature
programmable with initial and final holds, shall con-
tain a glass jet separator as the MS interface, and
shall produce results which meet the calibration (sec-
tion 7), quality assurance (section 8), and perfor-
mance tests (section 11) of this method
Column—2 8 ± 0 4 m x 2 ± 0 5 mmid glass, packed
with one percent SP-1000 on Carbopak B, 60/80
mesh, or equivalent
Mass spectrometer—70 eV electron impact ioniza-
tion, shall repetitively scan from 20 to 250 amu every
2-3 seconds, and produce a unit resolution (valleys
between m/z 174-176 less than 10 percent of the
height of the m/z 175 peak), background corrected
mass spectrum from 50 ng 4-bromofluorobenzene
(BFB) injected into the GC The BFB spectrum shall
meet the mass-intensity criteria in table 3 All por-
tions of the GC column, transfer lines, and separator
which connect the GC column to the ion source shall
remain at or above the column temperature during
analysis to preclude condensation of less volatile
compounds
TABLE 3
BFB Mass-intensity Specifications
MASS INTENSITY REQUIRED
50
15 to 40 percent of mass 95
75
30 to 60 percent of mass 95
95
base peak, 100 percent
96
5 to 9 percent of mass 95
173
< 2 percent of mass 174
174
> 50 percent of mass 95
176
95 to 100 percent of mass 174
177
5 to 9 percent of mass 1 76
55
551
Data system—shall collect and record MS data, store
mass intensity data in spectral libraries, process
GC/MS data and generate reports, and shall
calculate and record response factors
Data acquisition—mass spectra shall be collected
continuously throughout the analysis and stored on a
mass storage device
4
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5 5 2 Mass spectral libraries—user created libraries con-
taining mass spectra obtained from analysis of
authentic standards shall be employed to reverse 6 5 11
search GC/MS runs for the compounds of interest
(section 7 2)
5 5 3 Data processing—the data system shall be used to
search, locate, identify, and quantify the compounds
of interest in each GC/MS analysis Software routines 6 5 12
shall be employed to compute retention times and
EICP areas Displays of spectra, mass
chromatograms, and library comparisons are re-
quired to verify results
5 5 4 Response factors and multipoint calibrations—the
data system shall be used to record and maintain
lists of response factors (response ratios for isotope 6 5 2
dilution) and generate multi-point calibration curves
(section 7) Computations of relative standard devia-
tion (coefficient of variation) are useful for testing
calibration linearity Statistics on initial and on-going
performance shall be maintained (sections 8 and 11)
5 6 Syringes—5 mL glass hypodermic, with Luer-lok tips
5 7 Micro syringes—10, 25, and 100mL 6 5 4
5 8 Syringe valves—2-way, with Luer ends (Teflon or
Kel-F)
5 9 Syringe—5 mL, gas-tight, with shut-off valve
5 10 Bottles—15 mL, screw-cap with Teflon liner
5 11 Balance—analytical, capable of weighing 0 1 mg
6 REAGENTS AND STANDARDS
6 1 Reagent water—water in which the compounds of in- ® ®
terest and interfering compounds are not detected by
this method (section 8 5 2) It may be generated by
any of the following methods
6 1 1 Activated carbon—pass tap water through a carbon
bed (Calgon Filtrasorb-300, or equivalent)
6 1 2 Water purifier—pass tap water through a purifier
(Millipore Super Q, or equivalent)
61 3 Boil and purge—heat tap water to 90-100 °C and
bubble contaminant free inert gas through it for
approx one hour While still hot, transfer the water to
screw-cap bottles and seal with a Teflon-lined cap
6 7
6 2 Sodium thiosulfate—ACS granular
6 3 Methanol—pesticide quality or equivalent
6 4 Standard solutions—purchased as solutions or mix-
tures with certification to their purity, concentration,
and authenticity, or prepared from materials of 071
known purity and composition If compound purity is
96 percent or greater, the weight may be used
without correction to calculate the concentration of
the standard
6 5 Preparation of stock solutions—prepare in methanol
using liquid or gaseous standards per the steps
below Observe the safety precautions given in
section 4
6 5 1 Place approx 9 8 mL of methanol in a 10 mL ground 6 7 2
glass stoppered volumetric flask Allow the flask to
stand unstoppered for approximately 10 minutes or
until all methanol wetted surfaces have dried In each
case, weigh the flask, immediately add the com-
pound, then immediately reweigh to prevent evapor-
ation losses from affecting the measurement
Liquids—using a 100 fil syringe, permit 2 drops of
liquid to fall into the methanol without contacting the
neck of the flask Alternatively, inject a known
volume of the compound into the methanol in the
flask using a micro-syringe
Gases (chloromethane, bromomethane, chloro-
ethane, vinyl chloride)—fill a valved 5 mL gas-tight
syringe with the compound Lower the needle to ap-
prox 5 mm above the methanol meniscus Slowly in-
troduce the compound above the surface of the
meniscus The gas will dissolve rapidly in the
methanol
Fill the flask to volume, stopper, then mix by inverting
several times Calculate the concentration in mg/mL
(ptglfiL) from the weight gain (or density if a known
volume was injected)
Transfer the slock solution to a Teflon sealed screw-
cap bottle Store, with minimal headspace, in the
dark at -10 to -20°C
Prepare fresh standards weekly for the gases and
2-chloroethylvinyl ether All other standards are
replaced after one month, or sooner if comparison
with check standards indicate a change in concentra-
tion Quality control check standards that can be
used to determine the accuracy of calibration stan-
dards are available from the US Environmental Pro-
tection Agency, Environmental Monitoring and Sup-
port Laboratory, Cincinnati, Ohio
Labeled compound spiking solution—from stock
standard solutions prepared as above, or from mix-
tures, prepare the spiking solution to contain a con-
centration such that a 5-10 mL spike into each 5 mL
sample, blank, or aqueous standard analyzed will
result in a concentration of 20 uglL of each labeled
compound For the gases and for the water soluble
compounds (acrolein, acrylonitrile, acetone, diethyl
ether, and MEK), a concentration of 100/^g/L may be
used Include the internal standards (section 7 5) in
this solution so that a concentration of 20 jug/L in
each sample, blank, or aqueous standard will be
produced
Secondary standards—using stock solutions,
prepare a secondary standard in methanol to contain
each pollutant at a concentration of 500 ixglml For
the gases and water soluble compounds (section
6 6), a concentration of 2 5 mg/mL may be used
Aqueous calibration standards—using a 25 txL
syringe,add 20MLof the secondary standard (section
6 7) to 50, 100, 200, 500, and 1000 mLof reagent
water to produce concentrations of 200,100, 50, 20,
and 10 /mg/L, respectively If the higher concentration
standard for the gases and water soluble compounds
was chosen (section 6 6), these compounds will be
at concentrations of 1000, 500, 250,100, and 50jug/L
in the aqueous calibration standards
Aqueous performance standard—an aqueous stan-
dard containing all pollutants, internal standards,
labeled compounds, and BFB is prepared daily, and
analyzed each shift to demonstrate performance
(section 11) This standard shall contain either 20 or
5
-------
100 /ig/L of the labeled and pollutant gases and
water soluble compounds, lO^g/L BFB, and 20M9/L
of all other pollutants, labeled compounds, and inter-
nal standards It may be the nominal 20 mq/L
aqueous calibration standard (section 6 7 1)
6 7 3 A methanolic standard containing all pollutants and
internal standards is prepared to demonstrate
recovery of these compounds when syringe injection
and purge and trap analyses are compared This
standard shall contain either 100 pg/mL or 500
jug/mL of the gases and water soluble compounds,
and 100 /jg/mL of the remaining pollutants and inter-
nal standards (consistent with the amounts in the
aqueous performance standard in 6 7 2)
6 7 4 Other standards which may be needed are those for
test of BFB performance (section 7 1) and for collec-
tion of mass spectra for storage in spectral libraries
(section 7 2)
7 CALIBRATION
7 1 Assemble the gas chromatographic apparatus and
establish operating conditions given in table 2 By
injecting standards into the GC, demonstrate that the
analytical system meets the detection limits in table 2
and the mass-intensity criteria in table 3 for 50 ng
BFB
7 2 Mass spectral libraries—detection and identification
of the compounds of interest are dependent upon the
spectra stored in user created libraries
7 2 1 Obtain a mass spectrum of each pollutant and la-
beled compound and each internal standard by
analyzing an authentic standard either singly or as
part of a mixture in which there is no interference bet-
ween closely eluted components That only a single
compound is present is determined by examination
of the spectrum Fragments not attributable to the
compound under study indicate the presence of an
interfering compound Adjust the analytical condi-
tions and scan rate (for this test only) to produce an
undistorted spectrum at the GC peak maximum An
undistorted spectrum will usually be obtained if five
complete spectra are collected across the upper half
of the GC peak Software algorithms designed to
"enhance" the spectrum may eliminate distortion,
but may also eliminate authentic m/z's or introduce
other distortion
7 2 2 The authentic reference spectrum is obtained under
BFB tuning conditions (section 7 1 and table 3) to
normalize it to spectra from other instruments
7 2 3 The spectrum is edited by saving the 5 most intense
mass spectral peaks and all other mass spectral
peaks greater than 10 percent of the base peak This
spectrum is stored for reverse search and for com-
pound confirmation
7 3 Assemble the purge and trap device Pack the trap
as shown in figure 2 and condition overnight at
170-180 °C by backflushing with an inert gas at a
flow rate of 20-30 mL/min Condition traps daily for a
minimum of 10 minutes prior to use
7 3 1 Analyze the aqueous performance standard (section
6 7 2) according to the purge and trap procedure in
section 10 Compute the area at the primary m/z
(table 4) for each compound Compare these areas
to those obtained by injecting one of the
methanolic standard (section 6 7 3) to determine
compound recovery The recovery shall be greater
than 20 percent for the water soluble compounds,
and 60-110 percent for all other compounds This
recovery is demonstrated initially for each purge and
trap GC/MS system The test is repeated only if the
purge and trap or GC/MS systems are modified in
any way that might result in a change in recovery
TABLE 4
Volatile Organic Compound Characteristic Masses
LABELED COMPOUND
ANALOG
PRIMARY M/Z'S
acetone
do
58/64
acrolein
dj
56/60
acrylonitrile
d3
53/56
benzene
de
78/84
bromodichloromethane
,3C
83/86
bromoform
,3C
173/176
bromomethane
da
96/99
carbon tetrachloride
,3C
47/48
chlorobenzene
d5
112/117
chloroethane
d5
64/71
2-chloroethylvinyl ether
d,
106/113
chloroform
,3C
85/86
chloromethane
d3
50/53
dibromochloromethane
,3C
129/130
1,1-dichloroethane
d3
63/66
1,2-dichloroethane
d.
62/67
1,1-dichloroethene
d2
61/65
trans-1,2-dichloroethene
d2
61/65
1,2-dichloropropane
da
63/67
trans-1,3-dichloropropene
a.
75/79
diethyl ether
dio
74/84
p-dioxane
de
88/96
ethylbenzene
dio
106/116
methylene chloride
d2
84/88
methyl ethyl ketone
da
72/75
1,1,2,2-tetrachloroethane
d2
83/84
tetrachloroethene
,3C2
164/172
toluene
da
92/98
1,1,1-trichloroethane
d3
97/102
1,1,2-trichloroethane
,3C2
83/84
tnchloroethene
,3C
95/1 36
vinyl chloride
d3
62/65
Demonstrate that 100 ng toluene (or toluene-da) pro-
duces an area at m/z 91 (or 98) approx one-tenth that
required to exceed the linear range of the system
The exact value must be determined by experience
for each instrument It is used to match the calibration
range of the instrument to the analytical range and
detection limits required
Calibration by isotope dilution—the isotope dilution
approach is used for the purgeable organic com-
pounds when appropriate labeled compounds are
available and when interferences do not preclude the
analysis If labeled compounds are not available, or
interferences are present, the internal standard
method (section 7 5) is used A calibration curve en-
compassing the concentration range of interest is
prepared for each compound determined The
relative response (RR) vs concentration (/^tg/L) is
plotted or computed using a linear regression An ex-
6
-------
ample of a calibration curve for toluene using
toluene-da is given in figure 5 Also shown are the
±10 percent error limits (dotted lines) Relative
response is determined according to the pro-
cedures described below A minumum of five data
points are required for calibration (section 7 4 4)
1 1 r
2 10 20 50 100 200
CONCENTRATION (ufl/L)
FIGURE 5 Relative Response Calibration Curve
for Toluene. The Dotted Lines Enclose a ±10
Percent Error Window.
7 4 1 The relative response (RR) of pollutant to labeled
compound is determined from isotope ratio values
calculated from acquired data Three isotope ratios
are used in this process
Rx = the isotope ratio measured in the pure pollutant
(figure 6A)
R = the isotope ratio of pure labeled compound
(figure 6B)
Rm= the isotope ratio measured in the analytical
mixture of the pollutant and labeled com-
pounds (figure 6C)
The correct way to calculate RR is
pp _ (Ry ~ Rm)(Rx 1)
(Rm-Rx)(Ry+1)
If Rm is not between 2Ry and 0 5RX, the method does
not apply and the sample is analyzed by the internal
standard method (section 7 5)
7 4 2 In most cases, the retention times of the pollutant and
labeled compound are the same and isotope ratios
(R's) can be calculated from the EICP areas, where
P _ (area at m,/z)
(area at m2/z)
If either of the areas is zero, it is assigned a value of
one in the calculations, that is, if
area of m,/z = 50721, and
area of m2/z = 0, then
R = 50721 = 50720
1
The m/z's are always selected such that Rx>Ry
When there is a difference in retention times (RT) be-
tween the pollutant and labeled compounds, special
precautions are required to determine the isotope
ratios
Ry, R„, and Rm are defined as follows
R, =
[area m,/z (at RT,)]
Ry =
—
[area m2/z (at RT2)]
_[area m,/z (at RT,)]
743
[area m2/z (at RT2)]
An example of the above calculations can be taken
from the data plotted in figure 6 for toluene and
toluene-ds For these data,
Rx =
_ 168920
1
Ry = —-
60960
n _ 96868
nm —
82508
= 168900
= 0 00001640
= 1 174
The RR for the above data is then calculated using
the equation given in section 7 4 1 For the example,
rr = 1 174 NOTE Not all labeled compounds elute
before their pollutant analogs
(A)
AREA=168920
¦ M/Z 98
• M/Z 92
(B)
AREA=60960
21
¦ M/Z 98
¦ M/Z 92
(C)
M/Z 92 . 96668
M/Z 98 " B2508
• M/Z 98
¦ M/Z 92
7 4 4
FIGURE 6 Extracted Ion Current Profiles for (A)
Toluene, (B) Toluene-dg, and (C) a Mixture of
Toluene and Toluene-dg.
To calibrate the analytical system by isotope dilution,
analyze a 5 mL aliquot of each of the aqueous
calibration standards (section 6 7 1) spiked with an
appropriate constant amount of the labeled com-
pound spiking solution (section 6 6), using the purge
and trap procedure in section 10 Compute the RR at
each concentration
7
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7 4 5 Linearity—if the ratio of relative response to concen-
tration for any compound is constant (less than 20
percent coefficient of variation) over the 5 point
calibration range, an averaged relative
response/concentration ratio may be used for that
compound, otherwise, the complete calibration
curve for that compound shall be used over the 5
point calibration range
7 5 Calibration by internal standard—used when criteria
for isotope dilution (section 7 4) cannot be met The
method is applied to pollutants having no labeled
analog and to the labeled compounds The internal
standards used for volatiles analyses are
bromochloromethane, 2-bromo-1 -chloropropane,
and 1,4-dichlorobutane Concentrations of the la-
beled compounds and pollutants without labeled
analogs are computed relative to the nearest eluted
internal standard, as shown in table 2
7 5 1 Response factors—calibration requires the deter-
mination of response factors (RF) which are defined
by the following equation
RF = (As x C|s), where
(A|S X Cg),
As is the EICP area at the characteristic m/z for the
compound in the daily standard
AIS is the EICP area at the characteristic m/z for the
internal standard
CIS is the concentration (/ig/L) of the internal stan-
dard
Cs is the concentration of the pollutant in the daily
standard
7 5 2 The response factor is determined at 10,20, 50,100,
and 200 ugll for the pollutants (optionally at five
times these concentrations for gases and water solu-
ble pollutants—see section 6 6), in a way analogous
to that for calibration by isotope dilution (section
7 4 4) The RF is plotted against concentration for
each compound in the standard (C^ to produce a
calibration curve
7 5 3 Linearity—if the response factor (RF) for any com-
pound is constant (less than 35 percent coefficient of
variation) over the 5 point calibration range, an
averaged response factor may be used for that com-
pound, otherwise, the complete calibration curve for
that compound shall be used over the 5 point range
7 6 Combined calibration—by adding the isotopically
labeled compounds and internal standards (section
6 6) to the aqueous calibration standards (section
6 7 1), a single set of analyses can be used to pro-
duce calibration curves for the isotope dilution and
internal standard methods These curves are verified
each shift (section 11 5) by purging the aqueous per-
formance standard (section 6 7 2) Recalibration is
required only if calibration and on-going performance
(section 11 5) criteria cannot be met
8 QUALITY ASSURANCE/QUALITY CONTROL
8 1 Each laboratory that uses this method is required to
operate a formal quality assurance program The
minimum requirements of this program consist of an
initial demonstration of laboratory capability, analysis
of samples spiked with labeled compounds to
evaluate and document data quality, and analysis of
standards and blanks as tests of continued perfor-
mance Laboratory performance is compared to
established performance criteria to determine if the
results of analyses meet the performance character-
istics of the method
8 1 1 The analyst shall make an initial demonstration of the
ability to generate acceptable accuracy and preci-
sion with this method This ability is established as
described in section 8 2
8 1 2 The analyst is permitted to modify this method to im-
prove separations or lower the costs of
measurements, provided all performance specifica-
tions are met Each time a modification is made to the
method, the analyst is required to repeat the pro-
cedure in section 8 2 to demonstrate method perfor-
mance
8 1 3 Analyses of blanks are required to demonstrate
freedom from contamination and that the compounds
of interest and interfering compounds have not been
carried over from a previous analysis (section 3) The
procedures and criteria for analysis of a blank are
described in sections 8 5
8 1 4 The laboratory shall spike all samples with labeled
compounds to monitor method performance This
test is described in section 8 3 When results of these
spikes indicate atypical method performance for
samples, the samples are diluted to bring method
performance within acceptable limits (section 14 2)
81 5 The laboratory shall, on an on-going basis,
demonstrate through the analysis of the aqueous per-
formance standard (section 6 7 2) that the analysis
system is in control This procedure is described in
sections 11 1 and 11 5
8 1 6 The laboratory shall maintain records to define the
quality of data that is generated Development of ac-
curacy statements is described in sections 8 4 and
115 2
8 2 Initial precision and accuracy—to establish the ability
to generate acceptable precision and accuracy, the
analyst shall perform the following operations
8 2 1 Analyze two sets of four 5-mL aliquots (8 aliquots
total) of the aqueous performance standard (section
6 7 2) according to the method beginning in section
10
8 2 2 Using results of the first set of four analyses in sec-
tion 8 2 1, compute the average recovery (X) in/xg/L
and the standard deviation of the recovery (s) in ug/L
for each compound, by isotope dilution for pollutants
with a labeled analog, and by internal standard for
labeled compounds and pollutants with no labeled
analog
8 2 3 For each compound, compare s and X with the cor-
responding limits for initial precision and accuracy
found in table 5 If s and X for all compounds meet
the acceptance criteria, system performance is ac-
ceptable and analysis of blanks and samples may
begin if, however, any individual s exceeds the
precision limit or any individual X falls outside the
range for accuracy, system performance is unaccep-
table for that compound NOTE The large number of
8
-------
compounds in table 5 present a substantial probabili-
ty that one or more will fail one ot the acceptance
criteria when all compounds are analyzed To deter-
mine if the analytical system is out of control, or if the
failure can be attributed to probability, proceed as
follows
8 2 4 Using the results_of the second set of four analyses,
compute s and X for only those compounds which
failed the test of the first set of four analyses (section
8 2 3) If these compounds now pass, system perfor-
mance is acceptable for all compounds and analysis
of blanks and samples may begin If, however, any of
the same compounds fail again, the analysis system
is not performing properly for the compound (s) in
question In this event, correct the problem and
repeat the entire test (section 8 2 1)
8 3 The laboratory shall spike all samples with labeled
compounds to assess method performance on the
sample matrix
8 3 1 Spike and analyze each sample according to the
method beginning in section 10
8 3 2 Compute the percent recovery (P) of the labeled
compounds using the internal standard method (sec-
tion 7 5)
8 3 3 Compare the percent recovery for each compound
with the corresponding labeled compound recovery
limit in table 5 If the recovery of any compound falls
outside its warning limit, method performance is
unacceptable for that compound in that sample
Therefore, the sample matrix is complex and the
sample is to be diluted and reanalyzed, per section
142
8 4 As part of the QA program for the laboratory, method
accuracy for waste-water samples shall be assessed
and records shall be maintained After the analysis of
five wastewater samples for which the labeled com-
pounds pass the test in section 8 3 3, compute the
average percent recovery (P) and the standard devia-
tion of the percent recovery (sp) for the labeled com-
pounds only Express the accuracy assessment as a
percent recovery interval from P - 2sp to P + 2sp
For example, if P = 90% and sp = 10%, the ac-
curacy interval is expressed as 70-110% Update the
accuracy assessment for each compound on a
regular basis (eg after each 5-10 new accuracy
measurements)
TABLE 5
Acceptance Criteria for Performance Tests
ACCEPTANCE CRITERIA AT 2Q pg/L
INITIAL PRECISION
AND ACCURACY
SECTION 8 2 3
COMPOUND
i (H9A)
% (M9/U
LABELED
COMPOUND
RECOVERY
SECTION 6 3
AND 14 2
P<%>
ON-GOING
ACCURACY
SECTION 11 5
R (HQ/L)
acetone
acrolein
acrylomtrile
note 1 ¦
note 2 ¦
note 2 ¦
benzene
90
13 0 - 28 2
ns-196
4-33
bromodichloromethane
82
6 5-31 5
ns- 199
4 - 34
bromoform
70
7 4- 35 1
ns - 214
6-36
bromomethane
25 0
d - 54 3
ns - 414
d - 61
carbon tetrachloride
69
15 9 - 24 8
42-165
12-30
chlorobenzene
82
14 2 - 29 6
ns - 205
4-35
chloroethane
14 8
2 1 - 46 7
ns - 308
d - 51
2-chloroethylvmyl ether
36 0
d - 69 8
ns - 554
d - 79
chloroform
79
11 6 - 26 3
18-172
8-30
chloromethane
26 0
d - 55 5
ns - 410
d - 64
dibromochloromethane
79
11 2 - 29 1
16 -185
8-32
1,1-dichloroethane
67
11 4-31 4
23-191
9-33
1,2-dichloroethane
7 7
11 6 - 30 1
12 - 192
8-33
1,1-dichloroethene
11 7
d - 49 8
ns-315
d - 52
trans-1,2-dichloroethene
7 4
105-31 5
15-195
8-34
1,2-
-------
8 5 Blanks—reagent water blanks are analyzed to
demonstrate freedom from carry-over (section 3) and
contamination
8 5 1 The level at which the purge and trap system will
carry greater than 5 /ug/L of a pollutant of interest
(table 1) into a succeeding blank shall be determined
by analyzing successively larger concentrations of
these compounds When a sample contains this con-
centration or more, a blank shall be analyzed im-
mediately following this sample to demonstrate no
carry-over at the 5 /ug/L level
8 5 2 With each sample lot (samples analyzed on the same
8 hr shift), a blank shall be analyzed immediately after
analysis of the aqueous performance standard (sec-
tion 11 1) to demonstrate freedom from contamina-
tion If any of the compounds of interest (table 1) or
any potentially interfering compound is found in a
blank at greater than 10 jug/L (assuming a response
factor of 1 relative to the nearest eluted internal stan-
dard for compounds not listed in table 1), analysis of
samples is halted until the source of contamination is
eliminated and a blank shows no evidence of con-
tamination at this level
8 6 The specifications contained in this method can be
met if the apparatus used is calibrated properly, then
maintained in a calibrated state The standards used
for calibration (section 7), calibration verification
(section 11 5) and for initial (section 8 2) and on-
going (section 11 5) precision and accuracy should
be identical, so that the most precise results will be
obtained The GC/MS instrument in particular will
provide the most reproducible results if dedicated to
the settings and conditions required for the analyses
of volatiles by this method
8 7 Depending on specific program requirements, field
replicates may be collected to determine the preci-
sion of the sampling technique, and spiked samples
may be required to determine the accuracy of the
analysis when internal or external standard methods
are used
9 SAMPLE COLLECTION, PRESERVATION, AND
HANDLING
91 Grab samples are collected in glass containers hav-
ing a total volume greater than 20 mL Fill sample
bottles so that no air bubbles pass through the sam-
ple as the bottle is filled Seal each bottle so that no
air bubbles are entrapped Maintain the hermetic seal
on the sample bottle until time of analysis
9 2 Samples are maintained at 0-4 °C from the time of
collection until analysis If the sample contains
residual chlorine, add sodium thiosulfate preser-
vative (10 mg/40 mL) to the empty sample bottles
just prior to shipment to the sample site EPA
Methods 330 4 and 330 5 may be used for measure-
ment of residual chlorine (reference 8) If preser-
vative has been added, shake the bottle vigorously
for one minute immediately after filling
9 3 Experimental evidence indicates that some aromatic
compounds, notably benzene, toluene, and ethyl
benzene are susceptible to rapid biological degrada-
tion under certain environmental conditions
94
Refrigeration alone may not be adequate to preserve
these compounds in wastewaters for more than
seven days For this reason, a separate sample
should be collected, acidified, and analyzed when
these aromatics are to be determined Collect about
500 mL of sample in a clean container Adjust the pH
of the sample to about 2 by adding HC1 (1 +1) while
stirring Check pH with narrow range (1 4 to 2 8) pH
paper Fill a sample container as described in section
91 If residual chlorine is present, add sodium
thiosulfate to a separate sample container and fill as
in section 9 1
All samples shall be analyzed within 14 days of col-
lection
10 PURGE, TRAP, AND GC/MS ANALYSIS
10 1 Remove standards and samples from cold storage
and bring to 20-25 °C
10 2 Adjust the purge gas flow rate to 40 ± 4 mL/min
Attach the trap inlet to the purging device and set the
valve to the purge mode (figure 3) Open the syringe
valve located on the purging device sample introduc-
tion needle (figure 1)
10 3 Remove the plunger from a 5-mL syringe and attach
a closed syringe valve Open the sample bottle and
carefully pour the sample into the syringe barrel until
it overflows Replace the plunger and compress the
sample Open the syringe valve and vent any
residual air while adjusting the sample volume to 5 0
mL Because this process of taking an aliquot
destroys the validity of the sample for future analysis,
fill a second syringe at this time to protect against
possible loss of data Add an appropriate amount of
the labeled compound spiking solution (section 6 6)
through the valve bore, then close the valve
10 4 Attach the syringe valve assembly to the syringe
valve on the purging device Open both syringe
valves and inject the sample into the purging
chamber
10 5 Close both valves and purge the sample for 11 0 ±
0 1 minutes at 20-25°C
10 6 After the 11 minute purge time, attach the trap to the
chromatograph and set the purge and trap apparatus
to the desorb mode (figure 4) Desorb the trapped
compounds into the GC column by heating the trap
to 170-180 °C while backflushing with carrier gas at
20-60 mL/min for four minutes Start MS data acquisi-
tion upon start of the desorb cycle, and start the GC
column temperature program 3 minutes later Table
2 summarizes the recommended operating condi-
tions for the gas chromatograph Included in this
table are retention times and detection limits that
were achieved under these conditions An example
of the separations achieved by the column listed is
shown in figure 8 Other columns may be used pro-
vided the requirements in section 8 can be met If the
priority pollutant gases produce GC peaks so broad
that the precision and recovery specifications (sec-
tion 8 2) cannot be met, the column may be cooled to
ambient or sub-ambient temperature to sharpen
these peaks
lO
-------
10 7 While analysis of the desorbed compounds pro- 11512
ceeds, empty the purging chamber using the sample
introduction syringe Wash the chamber with two
5-mL portions of reagent water After the purging
device has been emptied, allow the purge gas to vent
through the chamber until the frit is dry, so that it is
ready for the next sample
10 8 After desorbing the sample for four minutes, recondi-
tion the trap by returning to the purge mode Wait 15
seconds, then close the syringe valve on the purging
device to begin gas flow through the trap Maintain 115 2
the trap temperature at 170-180 °C After approx-
imately seven minutes, turn off the trap heater and
open the syringe valve to stop the gas flow through
the trap When cool, the trap is ready for the next
sample
11 SYSTEM PERFORMANCE
111 At the beginning of each 8 hr shift during which
analyses are performed, system calibration and per-
formance shall be verified for all pollutants and la-
beled compounds For these tests, analysis of the
aqueous performance standard (section 6 7 2) shall
be used to verify all performance criteria Adjustment
and/or recalibration (per section 7) shall be per-
formed until all performance criteria are met Only
after all performance criteria are met may blanks and
samples be analyzed
11 2 BFB spectrum validity—the criterai in table 3 shall be
met
11 3 Retention times—the absolute retention times of all
compounds shall approximate those given in table 2
114 GC resolution—the valley height between toluene
and toluene-d« (at m/z 91 and 98 plotted on the same
graph) shall be less than 10 percent of the taller of the
two peaks
11 5 Calibration verification and on-going precision and
accuracy—compute the concentration of each pollu-
tant (table 1) by isotope dilution (section 7 4) for
those compounds which have labeled analogs Com-
pute the concentration of each pollutant (table 1)
which has no labeled analog by the internal standard
method (section 7 5) Compute the concentration of
the labeled compounds by the internal standard
method These concentrations are computed based
on the calibration data determined in section 7
115 1 For each pollutant and labeled compound, compare
the concentration with the corresponding limit for on-
going accuracy in table 5 If all compounds meet the
acceptance criteria, system performance is accep-
table and analysis of blanks and samples may con-
tinue If any individual value falls outside the range
given, system performance is unacceptable for that 12 11
compound NOTE The large number of compounds
in table 5 present a substantial probability that one or
more will fail the acceptance criteria when all com-
pounds are analyzed To determilne if the analytical 1212
system is out of control, or if the failure may be at-
tributed to probability, proceed as follows
115 11 Analyze a second aliquot of the aqueous perfor-
mance standard (section 6 7 2)
Compute the concentration for only those com-
pounds which failed the first test (section 1151) If
these compounds now pass, system performance is
acceptable for all compounds and analyses of blanks
and samples may proceed If, however, any of the
compounds fail again, the measurement system is
not performing properly for these compounds In this
event, locate and correct the problem or recalibrate
the system (section 7), and repeat the entire test (sec-
tion 11 1) for all compounds
Add results which pass the specification in 11 5 1 2
to initial (section 8 2) and previous on-going data Up-
date OC charts to form a graphic representation of
laboratory performance (figure 7) Develop a state-
ment of accuracy for each pollutant and labeled com-
pound by calculating the average percent recovery
(R) and the standard deviation of percent recovery
(sr) Express the accuracy as a recovery interval from
R - 2sr to R + 2sr For example, if R = 95% and sr
= 5%, the accuracy is 85-105 percent
3! 120,000
H
<
2 100,000
oc
<
*
}? 80,000
TOLUENE D,
•+3s
3s
8 9 10
£§
in 3
Ui u]
> z
1 10
100
090
ANALYSIS NUMBER
-J I I l_
TOLUENE
1 I I T I 1 I I I
6/1 6/1 6/1 6/1 6f2 6/2 6/3 6/3 6/4 6/5
DATE ANALYZED
+ 39
-3s
12
12 1
FIGURE 7 Quality Control Charts Showing Area
(top graph) and Relative Response of Toluene
to Toluene-d, (lower graph) Plotted as a
Function of Time or Analysis Number.
QUALITATIVE DETERMINATION-accomplished by
comparison of data from analysis of a sample or
blank with data from analysis of the shift standard
(section 111) Identification is confirmed when spec-
tra and retention times agree per the criteria below
Labeled compounds and pollutants having no la-
beled analog
The signals for all characteristic masses stored in the
spectral library (section 7 2 3) shall be present and
shall maximize within the same two consecutive
scans
Either (1) the backgound corrected EICP areas, or (2)
the corrected relative intensities of the mass spectral
peaks at the GC peak maximum shall agree within a
factor of two (0 5 to 2 times) for all masses stored in
the library
11
-------
12 13 The retention time relative to the nearest eluted inter-
nal standard shall be within ± 7 scans or ± 20
seconds, whichever is greater of this difference in the
shift standard (section 111)
12 2 Pollutants having a labeled analog
12 2 1 The signals for all characteristic masses stored in the
spectral library (section 7 2 3) shall be present and
shall maximize within the same two consecutive
scans
12 2 2 Either (1) the backgound corrected EICP areas, or (2)
the corrected relative intensities of the mass spectral
peaks at the GC peak maximum shall agree within a
factor of two for all masses stored in the spectral
library
12 2 3 The retention time difference between the pollutant
and its labeled analog shall agree within ± 2 scans
or ± 6 seconds (whichever is greater) of this dif-
ference in the shift standard (section 11 1)
12 3 Masses present in the experimental mass spectrum
that are not present in the reference mass spectrum
shall be accounted for by contaminant or backgound
ions If the experimental mass spectrum is con-
taminated, an experienced spectrometrist (section
1 4) is to determine the presence or absence of the
compound
13 QUANTITATIVE DETERMINATION
13 1 Istope dilution—by adding a known amount of a
labeled compound to every sample prior to purging,
correction for recovery of the pollutant can be made
because the pollutant and its labeled analog exhibit
the same effects upon purging, desorption, and gas
chromatography Relative response (RR) values for
sample mixtures are used in conjunction with calibra-
tion curves described in section 7 4 to determine
concentrations directly, so long as labeled com-
pound spiking levels are constant For the toluene ex-
ample given in figure 6 (section 7 4 3), RR would be
equal to 1 174 For this RR value, the toluene calibra-
tion curve given in figure 5 indicates a concentration
of 31 8 figIL
13 2 Internal standard—calculate the concentration using
the response factor determined from calibration data
(section 7 5) and the following equation
Concentration = (Asx cis)
(A,s x RF)
where the terms are as defined in section 7 5 1
13 3 If the EICP area at the quantitation mass for any com-
pound exceeds the calibration range of the system,
the sample is diluted by successive factors of 10 and
these dilutions are analyzed until the area is within
the calibration range
13 4 Report results for all pollutants and labeled com-
pounds (table 1) found in all standards, blanks, and
samples, in ^g/L, to three significant figures Results
for samples which have been diluted are reported at
the least dilute level at which the area at the quantita-
tion mass is within the calibration range (section
13 3) and the labeled compound recovery is within
the normal range for the Method (section 14 2)
14 ANALYSIS OF COMPLEX SAMPLES
14 1 Untreated effluents and other samples frequently
contain high levels (>1000 iigll) of the compounds
of interest and of interfering compounds Some
samples will foam excessively when purged, others
will overload the trap and/or GC column
14 2 Dilute 0 5 mL of sample with 4 5 mL of reagent water
and analyze this diluted sample when labeled com-
pound recovery is outside the range given in table 5
If the recovery remains outside of the range for the
diluted sample, the aqueous performance standard
shall be analyzed (section 11) and calibration verified
(section 115) If the recovery for the labeled com-
pound in the aqueous performance standard is out-
side the range given in table 5, the analytical system
is out of control In this case, the instrument shall be
repaired, the performance specifications in section
11 shall be met, and the analysis of the undiluted
sample shall be repeated If the recovery for the
aqueous performance standard is within the range
given in table 5, the method does not work on the
sample being analyzed and the result may not be
reported for regulatory compliance purposes
14 3 Reverse search computer programs can misinterpret
the spectrum of chromatographically unresolved
pollutant and labeled compound pairs with overlapp-
ing spectra when a high level of the pollutant is pre-
sent Examine each chromatogram for peaks greater
then the height of the internal standard peaks These
peaks can obscure the compounds of interest
15 METHOD PERFORMANCE
15 1 The specifications for this method were taken from
the interlaboratory validation of EPA Method 624
(reference 9) Method 1624 has been shown to yield
slightly better performance on treated effluents than
method 624 Additional method performance data
can be found in Reference 10
15 2 A chromatogram of the 20 /xg/L aqueous perfor-
mance standards (sections 6 7 2 and 11 1) is shown
in figure 8
12
-------
MASS CHROHATOGRAH DATA: UOAI01945 «1 SCANS 1 TO 1208
89/81/84 23:95:80 CALI: UOAI01945 II
SAMPLE: UO,S,OPR,08020,68,U,NA:NA,NAJ
CONDS.: 1624B, 3.811,2MM, 3045,45-24808,15S240,20t1L/MINJ
RANGE: C 1,1288 LABEL: N 0, 4.0 QUAN: A 8, 1.8 J 0 BASE: U 20, 3
222976.
46.514
250.575
251
1200 SCAN
800
1088
600
200
6:58 13:48 28:38 27:20 34:10 41:88 TINE
FIGURE 8 Chromatogram of Aqueous Performance Standards
16 REFERENCES
1 "Performance Tests for the Evaluation of Com-
puterized Gas Chromatography/Mass Spectrometry
Equipment and Laboratories," USEPA, EMSUCincin-
nati, OH 45268, EPA-600/4-80-025 (April 1980)
2 Bellar, T A and Lichtenberg, J J, "Journal
American Water Works Association," 66, 739 (1974)
3 Bellar, T A and Lichtenberg, J J , "Semi-automated
Headspace Analysis of Drinking Waters and In-
dustrial Waters for Purgeable Volatile Organic Com-
pounds," in Measurement of Organic Pollutants
Water and Wastewater, C E VanHall, ed , American
Society for Testing Materials, Philadelphia, PA,
Special Technical Publication 686, (1978)
4 "Working with Carcinogens," DHEW, PHS, NIOSH,
Publication 77-206 (1977)
5 "OSHA Safety and Health Standards, General
Industry," 29CFR1910, OSHA 2206, (1976)
6 "Safety in Academic Chemistry Laboratories,"
American Chemical Society Publication, Committee
on Chemical Safety (1979)
7 "Handbook of Analytical Quality Control in Water
and Wastewater Laboratories," USEPA, EMSL/Cin-
cinnati, OH 45268, EPA-4-79-019 (March 1979)
8 "Methods 330 4 and 330 5 for Total Residual
Chlorine," USEPA, EMSL/Cincinnati, OH 45268,
EPA-4-79-020 (March 1979)
9 "Test Method Purgeables—Method 624," USEPA,
EMSL/Cincinnati, OH 45268
10 Colby, B N, Beimer, R G , Rushneck, D R, and
Telliard, W A , "Isotope Dilution Gas
Chromatography-Mass Spectrometry for the Deter-
mination of Priority Pollutants in Industrial Effluents,"
USEPA, Effluent Guidelines Division, Washington,
DC 20460 (1980)
13
-------
Method 1625 Revision B
SEMIVOLATILE ORGANIC COMPOUNDS BY ISOTOPE DILUTION GC/MS
1 SCOPE AND APPLICATION
1 1 This methoc is designed to determine the semivolatile
toxic organic pollutants associated with the 1976
Consent Decree and additional compounds amenable
to extraction and analysis by capillary column gas
chromatography-mass spectrometry (GC/MS)
i 2 The chemical compounds listed in tables 1 and 2 may
be determined in municipal and industrial discharges
by this method The method is designed to meet the
survey requirements of EPA's Industrial Technology
Division (ITD) and the National Pollutants Discharge
Elimination System (NPDES) under 40 CFR 136 1
Any modifications of this method, beyond those ex-
pressly permitted, shall be considered as majcf
modifications subject to application and approval of
alternate test procedures under 40 CFR 136 4 and
136 5
Table 1
Base/Neutral Extractable Compounds
POLLUTANT
LABELED COMPOUND
COMPOUND
STORET
CAS
EGD
NPDES
ANALOG
CAS
EGD
acenaphthene
34205
83-32-9
001 B
001
B
dio
15067-20-2
201 B
acenaphthylene
34200
208-96-8
077 B
002
B
do
93951-97-4
277 B
anthracene
34220
120-1 2-7
078 B
003
B
dio
1719-06-8
278 B
benzidine
39120
92-87-5
005 B
004
B
ds
92890-63-6
205 B
benzo(a)anthracene
34526
56-55-3
072 B
005
B
di2
1718-53-2
272 B
benzo(b)tluoianthene
34230
205-99-2
074 B
007
B
di2
93951-98-5
274 B
benzo(k)fluoianlhene
34242
207-08-9
075 B
009
B
di2
93952-01-3
275 B
benzo(a)pyrene
34247
50-32-B
973 B
006
B
di2
63466-71-7
273 B
benzo(ghi)perylene
34521
191-24-2
079 B
008
B
d,2
93951-66-7
279 B
biphenyl (Appendix C)
81513
92-54-4
512 B
dio
1486-01-7
612 B
bis(2-chloroethyl) ether
34273
111-44-4
018 B
011
B
do
93952-02-4
218 B
bis (2-chloroethoxy) methane
34278
111-91-1
043 B
010
B
do
93966-78-0
243 B
bis(2-chloroisopropyl) ether
34283
108-60-1
042 B
012
B
d,2
93951-67-8
242 B
bis(2-ethylhexyl) phthalate
39100
117-81-7
066 B
013
B
d4
93951-87-2
266 B
4-bromophenyl phenyl ether
34636
101-55-3
041 B
014
B
d5
93951-83-8
241 B
butyl benzyl phthalate
34292
85-68-7
067 B
015
B
d4
93951-88-3
267 B
n-Cio (Appendix C)
77427
124-18-5
517 B
d22
16416-29-8
617 B
n-C12 (Appendix C)
77588
112-40-3
506 B
d2e
16416-30-1
606 B
n-CM (Appendix C)
77691
629-59-4
518 B
n-Ci6 (Appendix C)
77757
544-76-3
519 8
dj4
15716-08-2
619 B
n-C, 8 (Appendix C)
77804
593-45-3
520 B
n-C2o (Appendix C)
77830
112-95-8
521 B
d«2
62369-67-9
621 B
n-C22 (Appendix C)
77859
629-97-9
522 B
n-C24 (Appendix C)
77886
646-31-1
523 B
dso
16416-32-3
623 B
n-C26 (Appendix C)
77901
630-01-3
524 B
n-C28 (Appendix C)
78116
630-02-4
525 B
625 B
n-C3o (Appendix C)
78117
638-68-6
526 B
ds2
93952-07-9
626 B
carbazole (4c)
77571
86-74-8
528 B
da
38537-24-5
628 B
2-chloronaphthalene
34581
81-58-7
020 B
016
B
d,
93951-84-9
220 B
4-chlorophenyl phenyl ether
34641
7005-72-3
040 B
017
B
d5
93951-85-0
240 B
chrysene
34320
218-01-9
076 B
018
B
di2
1719-03-5
276 B
p-cymene (Appendix C)
77356
99-87-6
513 B
du
93952-03-5
613 B
dibenzo(a,h)anthracene
34556
53-70-3
082 B
019
B
du
13250-98-1
282 B
dibenzoluran (Appendix C & 4c)
81302
132-64-9
505 B
da
93952-04-6
605 B
dibenzolhiophene (Synfuel)
77639
132-65-0
504 B
do
33262-29-2
604 B
di-n-butyl ph halate
3911C
84-74-2
068 B
026
B
d,
93952-11-5
268 B
1,2-dichlorobenzene
34536
95-50-1
025 B
020
B
d4
2199-69-1
225 B
1,3-dichlorobenzene
34566
541-73-1
026 B
021
B
d4
2199-70-4
226 B
1,4-dichlorobenzene
34571
106-46-7
027 B
022
B
d4
3855-82-1
227 B
3.3-dichlorobenzidine
34631
91-94-1
028 B
023
B
do
93951-91-8
228 B
diethyl phthalate
34336
84-66-2
070 B
024
B
d4
93952-12-6
270 B
2,4-dimethylphenol
34606
105-67-9
034 B
003
B
ds
93951-75-8
234 B
dimethyl phtnalate
34341
131-11-3
071 B
025
B
d4
93951-89-4
271 B
2,4-dinitrotoluene
34611
121-14-2
035 B
027
B
d,
93951-68-9
235 B
2,6-dimtrotoluene
34626
606-20-2
036 B
028
B
d3
93951-90-7
236 B
di-n-octyl phthalate
34596
117-84-0
069 B
029
B
d4
93952-13-7
269 B
diphenylamine (Appendix C)
77579
1 22-39-4
507 B
dio
37055-51-9
607 B
1
-------
Table 1 (Continued)
Base/Neutral Extractable Compounds
POLLUTANT
LABELED COMPOUND
COMPOUND
STORET
CAS
EGD
NPDES
ANALOG
CAS
EGD
diphenyl ether (Appendix C)
77587
101-84-8
508 B
dio
93952-05-7
608 B
1,2-diphenylhydrazme
34346
122-66-7
037 B
030 B
d,o
93951-92-9
237 B
fluoranthene
34376
206-44-0
039 B
031 B
dio
93951-69-0
231 B
fluorene
34381
86-73-7
080 B
032 B
dio
81103-79-9
080 B
hexachlorobenzene
39700
118-74-1
009 B
033 B
,3C«
93952-14-8
209 B
hexachlorobutadiene
34391
87-68-3
052 B
034 B
,3C4
93951-70-3
252 B
hexachloroethane
34396
67-72-1
012 B
036 B
,3C
93952-15-9
212 B
hexachlorocyclopentadiene
34386
77-47-4
053 B
035 B
,3C.
93951-71-4
253 B
ideno(1,2,3-cd)pyrene
34403
193-39-5
083 B
037 B
isophorone
34408
78-59-1
054 B
038 B
do
93952-16-0
254 B
naphthalene
34696
91-20-3
055 B
039 B
da
1146-65-2
255 B
beta-naphthylamine (Appendix C)
82553
91-59-8
056 B
040 B
d7
93951-94-1
602 B
nitrobenzene
34447
98-95-3
056 B
040 B
d5
4165-60-0
256 B
N-nitrosodimethylamine
34438
62-75-9
061 B
041 B
da
17829-05-9
261 B
N-nitrosodi-n-proplylamine
34428
621-64-7
063 B
042 B
d,.
93951-96-3
263 B
N-nitrosodiphenylamine
34433
86-30-6
062 B
043 B
do
93951-95-2
262 B
phenanthrene
34461
85-01-8
081 B
044 B
dio
1517-22-2
281 B
phenol
34694
108-95-2
065 B
010 B
d5
4165-62-2
265 B
alpha-picolme (Synfuel)
77088
109-06-8
503 B
d,
93951-93-0
503 B
pyrene
34469
129-00-0
084 B
045 B
dio
1718-52-1
284 B
styrene (Appendix C)
77128
100-42-5
510 B
ds
5161-29-5
610 B
alpha-terpmeol (Appendix C)
77493
98-55-5
509 B
d3
93952-06-8
609 B
1,2,3-trichlorobenzene (4c)
77613
87-61-6
529 B
d3
3907-98-0
629 B
1,2.4-trichlorobenzene
34551
120-82-1
008 B
046 B
ds
93952-16-0
208 B
TABLE 2
Acid Extractable Compounds
POLLUTANT
LABELED COMPOUND
COMPOUND
STORET
CAS
EGD
NPDES
ANALOG
CAS
EGD
4-chloro-3-methylphenol
34452
59-50-7
022
A
008
A
d2
93951-72-5
222 A
2-chlorophenol
34586
95-57-8
024
A
001
A
d«
93951-73-6
224 A
2,4-dichlorophenol
34601
120-83-2
031
A
002
A
d3
93951-74-7
231 A
2.4-dinilro phenol
34616
51-28-5
059
A
005
A
d3
93951-77-0
259 A
2-methyl-4,6-dinilrophenol
34657
534-52-1
060
A
004
A
d2
93951-76-9
260 A
2-nitrophenol
34591
88-75-5
057
A
006
A
d<
93951-75-1
257 A
4-mtrophenol
34646
100-02-7
058
A
007
A
di
93951-79-2
258 A
pentachlorophenol
39032
87-86-5
064
A
009
A
,3Ca
85380-74-1
264 A
2,3.6-trichlorophenol (4c)
77688
933-75-5
530
A
d2
93951-81-6
630 A
2,4,5-trichlorophenol (4c)
95-95-4
531
A
dz
93951-82-7
631 A
2,4,6-tnchlorophenol
34621
88-06-2
021
A
011
A
d2
93951-80-5
221 A
1 3 The detection limit of this method is usually depen-
dent on the level of interferences rather than in-
strumental limitations The limits listed in tables 3 and
4 represent the minimum quantity that can be
detected with no interferences present
1 4 The GC/MS portions of this method are for use only
by analysts experienced with GC/MS or under the
close supervision of such qualified persons
Laboratories unfamiliar with the analyses of en-
vironmental samples by GC/MS should run the per-
formance tests in reference 1 before beginning
2 SUMMARY OF METHOD
2 1 Stable isotopically labeled analogs of the com-
pounds of interest are added to a one liter
wastewater sample The sample is extracted at pH
12-13, then at pH <2 with methylene chloride using
continuous extraction techniques The extract is
dried over sodium sulfate and concentrated to a
volume of one mL An internal standard is added to
the extract, and the extract is injected into the gas
chromatograph (GC) The compounds are separated
by the GC and detected by a mass spectrometer
(MS) The labeled compounds serve to correct the
variability of the analytical technique
2 2 Identification of a compound (qualitative analysis) is
performed by comparing the GC retention time and
the background corrected characteristic spectral
masses with those of authentic standards
2 3 Quantitative analysis is performed by GC/MS using
extracted ion current profile (EICP) areas Isotope
dilution is used when labeled compounds are
available, otherwise, an internal or external standard
method is used
2 4 Quality is assured through reproducible calibration
and testing of the extraction and GC/MS systems
2
-------
3 CONTAMINATION AND INTERFERENCES
3 1 Solvents, reagents, glassware, and other sample
processing hardware may yield artifacts and/or
elevated baselines jcausing misinterpretation of
chromatograms and spectra All materials shall be
demonstrated to be free from interferences under the
conditions of the analysis by running method blanks
initially and with each sample lot (samples started
through the extraction process on a given 8 hr shift,
32
to a maximum of 20) Specific selection of reagents
and purification of solvents by distillation in all-glass
systems may be required Glassware and, where
possible, reagents are cleaned by solvent rinse and
baking at 450 °C for one hour minimum
Interferences coextracted from samples will vary
considerably from source to source, depending ori
the diversity of the industrial complex or municipality
being sampled
TABLE 3
Gas Chromatography of Base/Neutral Extractable Compounds
EGD
RETENTION TIME
DETECTION
NO
MEAN
EGD
LIMIT (2)
<1)
COMPOUND
(SEC)
REF
RELATIVE
(MO/L)
164
2,2-'difluorobiphenyl (internal standard)
1163
164
1 000-1 000
10
061
N-nitrosodimethylamme'
385
164
0 264-0 398
50
603
aloha picoline-d?
417
164
0 326-0 393
50
703
alpha picolme
426
603
1 006-1 028
50
610
st/rene-d5
546
164
0 450-0 488
10
710
styrene
549
610
1 002-1 009
10
613
p-cymene-dn
742
164
0 624-0 652
10
7I3
p-cymene
755
613
1 008-1 023
10
265
phenol-ds
696
164
0 584-0 613
10
365
phenol
700
265
0 995-1 010
10
218
bis(2-chloroethyl) ether-d8
696
164
0 584-0 607
10
318
bis(2-chloroethyl) ether
704
218
1 007-1 016
10
6-7
n-decane-d22
698
164
0 585-0 615
10
7" 7
n-decane
720
617
1 022-1 038
10
266
1,3-dichlorobenzene-d4
722
164
0 605-0 636
10
326
1,3-dichlorobenzene
724
226
0 998-1 008
10
227
1,4-dichlorobenzene-d4
737
164
0 601-0 666
10
327
1,4-dichlorobenzene
740
227
0 997-1 009
10
225
1,2-dichlorobenzene-d4
758
164
0 632-0 667
10
325
1,2-dichlorobenzene
760
225
0 995-1 008
10
242
bis(2-chloroisopropyl) ether-d12
788
164
0 664-0 691
10
342
bis(2-chloroisopropyl) ether
799
242
1 010-1 016
10
212
hexachloroethane-,3C
819
164
0 690-0 717
10
312
hexachloroethane
823
212
0 999-1 001
10
063
N-nitrosodi-n-propylamine *
830
164
0 701-0 721
2Cf
256
nitrobenzene-d5
845
164
0 706-0 727
10
356
nitiobenzene
849
256
1 002-1 007
10
254
isophorone-da
881
164
0 747-0 767
10
354
isophorone
889
254
0 999-1 017
10
234
2,4-dimelhylphenol-d3
921
164
0 781-0 803
10
334
2,4-dimelhylphenol
924
234
0 999-1 003
10
043
bis(2-chloroethoxy) methane"
939
164
0 799-0 815
10
208
1,2,4-trichlorobenzene-d3
955
164
0 813-0 830
10
308
1,2,4-tnchlorobenzene
958
208
1 000-1 005
10
255
naphthalene-dn
963
164
0 819-0 836
10
355
naphthalene
967
255
1 001-1 006
10
609
alpia-terpineol-dj
973
164
0 829-0 844
10
709
alpia-terpineol
975
609
0 998-1 008
10
606
n-dodecane-d26
953
164
0 730-0 908
10
706
n-dodecane
981
606
0 986-1 051
10
529
1,2,3-tnchlorobenzene*
1003
164
0 855-0 870
10
252
he>achlorobutadiene-,3C4
1005
164
0 856-0 871
10
352
hexachlorobutadiene
1006
252
0 999-1 002
10
253
hexachlorocyclopentadiene-,3C»
1147
164
0 976-0 986
10
353
hexachlorocyclopentadiene
1142
253
0 999-1 001
10
220
2-chloronaphthalene-d7
1185
164
1 014-1 024
10
320
2-chloronaphthalene
1200
220
0 997-1 007
10
518
n-tetradecane*
1203
164
1 015-1 026
10
612
biphenyl-d10
1205
164
1 016-1 027
10
712
biphenyl
1195
612
1 001-1 006
10
608
diphenyl ether-d,0
1211
164
1 036-1 047
10
708
diphenyl ether
1216
608
0 997-1 009
10
277
acenaphthylene-de
1265
164
1 080-1 095
10
3
-------
EGD
NO
(1)
377
271
371
236
336
201
301
605
705
602
702
280
360
240
340
270
370
619
719
235
335
237
337
607
707
262
362
041
209
309
281
520
381
278
378
604
704
528
621
721
268
368
239
339
284
384
205
305
522
623
723
067
276
376
272
372
228
328
266
366
524
269
369
525
4
10
10
10
10
10
10
10
10
10
50
50
10
10
10
10
10
10
10
10
10
10
20
20
20
20
20
20
10
10
10
10
10
10
10
10
10
10
20
10
10
10
10
10
10
10
10
50
50
10
10
10
10
10
10
10
10
50
50
10
10
10
10
10
10
TABLE 3 (Continued)
Gas Chromatography of Base/Neutral Extractable Compounds
RETENTION TIME
MEAN
EGD
COMPOUND
(SEC)
REF
RELATIVE
acenaphthylene
1247
277
1 000-1 004
dimethyl phthalate-d4
1269
164
1 083-1 102
dimethyl phthalate
1273
271
0 998-1 005
2.6-dinitrotoluene-
-------
TABLE 3 (Continued)
Gas Chromatography of Base/Neutral Extractable Compounds
EGD
RETENTION TIME
DETECTION
NO
MEAN
EGO
LIMIT (2)
(1)
COMPOUND
(SEC)
REF
RELATIVE
(MQ/U
274
benzo(b)fluoranthene-d,2
2281
164
1 902-2 025
10
354
benzo(b)fluoranthene
2293
274
1 000-1 005
10
275
benzo(k)fluoranthene-d, 2
2287
164
1 906-2 033
10
375
benzo{k)fluoranthene
2293
275
1 000-1 005
10
273
benzofajpyrene-d)!
2351
164
1 954-2 088
10
373
benzo(a)pyrene
2350
273
1 000-1 004
10
626
r-triacontane-ds!
2384
164
1 972-2 127
10
.'26
n-triacontane
2429
626
1 011-1 028
10
083
mdeno(i .2 3-cd)pyrene'
2650
164
2 119-2 356
20
082
dibenzo(a,h)anthracene *
2660
164
2 121-2 358
20
279
benzo(ghi)perylene-dij
2741
164
2 187-2 524
20
379
benzo(ghi)perylene
2750
279
1 001-1 006
20
(1) Reference numbers beginning with 0 1 01 5 indicate a pollutant quantified by the internal standard method, reference numbers beginning with 2 or 6
indicate a labeied compound quantified by the internal standard method reference numbers beginning with 3 or 7 indicate a pollutant quantified by
isotope dilution
(2) This is a minimum level at which the entire GC/MS system must give lecogmzable mass spectra (background corrected) and acceptable calibration
po nts
(3) detected as azobenzene
(4) detected as ciphenylamine
' specification derived from related compound
Column 30 ± 2 m x 0 25 ± 0 02 mm i d 94% methyl, 4% phenyl, 1 % vinyl bonded phase fused silica capillary
Temperature program 5 min at 30 °C 30 - 280 °C at 8°C per mm isothermal at 280 °C until benzo(ghi)perylene elutes
Gas velocity 30 ± 5 cm/sec
TABLE 4
Gas Chromatography of Acid Extractable Compounds
EGD
RETENTION TIME
DETECTION
NO
MEAN
EGD
LIMIT (2)
(1)
COMPOUND
(SEC)
REF
RELATIVE
(pg/L)
164
2,2'-difluorobiphenyl (internal standard)
1163
164
1 000-1 000
10
224
2-chlorophenol-d«
701
164
0 587-0 618
10
324
2-chlorophenol
705
224
0 997-1 010
10
257
2-nitrophenol-d.
898
164
0 761-0 783
20
357
2-nitrophenol
900
257
0 994-1 009
20
231
2 4-dichlorophenol-da
944
164
0 802-0 822
10
331
2 4-dichlorophenol
947
231
0 997-1 006
10
222
4-chloro-3-methylphenol-d2
1086
164
0 930-0 943
10
322
4-chloro-3-methylphenol
1091
222
0 998-1 003
10
221
2,4 6-trichlorophenol-dj
1162
164
0 994-1 005
10
321
2,4,6-trichlorophenol
1165
221
0 998-1 004
10
531
2,4,5-trichlorophenol"
1170
164
0 996-1 016
10
530
2,3.6-tnchlorophenol*
1195
164
1 016-1 140
10
259
2,4-dimtrophenol-dj
1323
164
1 127-1 149
50
359
2,4-dimtrophenol
1325
259
1 000-1 005
50
258
4-nitrophenol-d4
1349
164
1 147-1 175
50
358
4-nitrophenol
1354
258
0 997-1 006
50
260
2-methyl-4,6-dimtrophenol-d2
1433
164
1 216-1 249
20
360
2-methyl-4,6-dinitrophenol
1435
260
1 000-1 002
20
264
pentachlorophenol-,3CB
1559
164
1 320-1 363
50
364
pentachlorophenol
1561
264
0 998-1 002
50
(1) Reference numbers beginning with 0 1 or 5 indicate a pollutant quantified by the internal standard method, reference numbers beginning with 2 or 6
indicate a labeled compound quantified by the internal standard method, reference numbers beginning with 3 or 7 indicate a pollutant quantified by
isotope dilution
(2) This is a minimum level at which the entire GC/MS system must give recognizable mass spectra (background corrected) and acceptable calibration
points
' specification denved from related compound
Column 30 ± 2 m x 0 25 ± 0 02 mm id 94% methyl 4% phenyl, t % vinyl bonded phase (used silica capillary
Temperature prog am 5 mm at 30°C 30 - 250°C or until pentachlorophenol elutes
Gas velocity 30 ± cm/sec
5
-------
4 SAFETY
4 1 The toxicity or carcinogenicity of each compound or
reagent used in this method has not been precisely
determined, however, each chemical compound
should be treated as a potential health hazard
Exposure to these compounds should be reduced to
the lowest possible level The laboratory is responsi-
ble for maintaining a current awareness file of OSHA
regulations regarding the safe handling of the
chemicals specified in this method A reference file
of data handling sheets should also be made
available to all personnel involved in these analyses
Additional information on laboratory safety can be
found in references 2-4
4 2 The following compounds covered by this method
have been tentatively classified as known or
suspected human or mammalian carcinogens ben-
zo(a)anthracene, 3,3'-dichlorobenzidine, benzo(a)py-
rene, dibenzo(a,h)anthracene, N-nitrosodimethyla-
mine, and beta-naphthylamine Primary standards of
these compounds shall be prepared in a hood, and a
NIOSH/MESA approved toxic gas respirator should
be worn when high concentrations are handled
5 APPARATUS AND MATERIALS
51 Sampling equipment for discrete or composite
sampling
5 1 1 Sample bottle, amber glass, 1 1 liters minimum If
amber bottles are not available, samples shall be pro-
tected from light Bottles are detergent water
washed, then solvent rinsed or baked at 450 °C for
one hour minumum before use
5 1 2 Bottle caps—threaded to fit sample bottles Caps are
lined with Teflon Aluminum foil may be substituted if
the sample is not corrosive Liners are detergent
water washed, then reagent water (section 6 5) and
solvent rinsed, and baked at approximately 200°C
for one hour minumum before use
5 1 3 Compositing equipment—automatic or manual com-
positing system incorporating glass containers for
collection of a minimum 1 1 liters Sample containers
are kept at 0 to 4 "C during sampling Glass or Teflon
tubing only shall be used If the sampler uses a
peristaltic pump, a minimum length of compressible
silicone rubber tubing may be used in the pump only
Before use, the tubing is thoroughly rinsed with
methanol, followed by repeated rinsings with reagent
water (section 6 5) to minimize sample contamina-
tion An integrating flow meter is used to collect pro-
portional composite samples
5 2 Continuous liquid-liquid extractor—Teflon or glass
connecting joints and stopcocks without lubrication
(Hershberg-Wolf Extractor) one liter capacity, Ace
Glass 6841-10, or equivalent
5 3 Drying column—15 to 20 mm i d Pyrex chromato-
graphic column equipped with coarse glass frit or
glass wool plug
5 4 Kuderna-Danish (K-D) apparatus
54 1 Concentrator tube— 10mL, graduated (Kontes
K-570050-1025, or equivalent) with calibration
verified Ground glass stopper (size 19/22 joint) is
used to prevent evaporation of extracts
5 4 2 Evaporation flask—500 mL (Kontes K-570001 -0500,
or equivalent), attached to concentrator tube with
springs (Kontes K-662750-0012)
5 43 Snyder column—three ball macro (Kontes
K-503000-0232, or equivalent)
5 4 4 Snyder column —two ball micro (Kontes
K-469002-0219, or equivalent)
5 4 5 Boiling chips—approx 10/40 mesh, extracted with
methylene chloride and baked at 450°C for one hr
minimum
5 5 Water bath—heated, with concentric ring cover,
capable of temperature control (± 2 °C), installed in a
fume hood
5 6 Sample vials—amber glass, 2-5 mL with Teflon-lined
screw cap
5 7 Analytical balance—capable of weighing 0 1 mg
5 8 Gas chromatograph—shall have splitless or on-
column injection port for capillary column,
temperature program with 30 °C hold, and shall meet
all the performance specifications in section 12
581 Column—30 ±5 m x 0 25 ±0 02 mm i d 5% phenyl,
94% methyl, 1 % vinyl silicone bonded phase fused
silica capillary column (J & W DB-5, or equivalent)
5 9 Mass spectrometer—70 eV electron impact ioniza-
tion, shall repetitively scan from 35 to 450 amu in
0 95 to 1 00 second and shall produce a unit resolu-
tion (valleys between m/z 441-442 less than 10 per-
cent of the height of the 441 peak), background cor-
rected mass spectrum from 50 ng decafluoro-
triphenylphosphine (DFTPP) introduced through the
GC inlet The spectrum shall meet the mass-intensity
criteria in table 5 (reference 5) The mass spec-
trometer shall be interfaced to the GC such that the
end of the capillary column terminates within one
centimeter of the ion source but does not intercept
the electron or ion beams All portions of the column
which connect the GC to the ion source shall remain
at or above the column temperature during analysis
to preclude condensation of less volatile com-
P0""dS TABLE 5
DFTPP Mass-intensity Specifications
MASS INTENSITY REQUIRED
51
8-82 percent of mass 198
68
< 2 percent of mass 69
69
11-91 percent of mass 198
70
<2 percent of mass 69
127
32-59 percent of mass 198
198
base peak, 100 percent abundance
199
4-9 percent of mass 198
275
11 -30 percent of mass 198
441
44-110 percent of mass 443
442
30-86 percent of mass 198
443
14-24 percent of mass 442
5 10
Data system—shall collect and record MS data, store
mass intensity data in spectral libraries, process
GC/MS data, generate reports, and shall compute
and record response factors
5 10 1 Data acquisition—mass spectra shall be collected
continuously throughout the analysis and stored on a
mass storage device
6
-------
0 2
03
04
6
6 1
62
63
64
6 5
66
6 7
Mass spectral libraries—user created libraries con-
taining mass spectra obtained from analysis of
authentic standards shall be employed to reverse
search GC/MS runs for the compounds of interest
(section 7 2)
Data processing—the data system shall be used to
search, locate, identify, and quantify the compounds
of interest in each GC/MS analysis Software routines
shall be employed to compute retention times and
peak areas Displays of spectra, mass chromato-
grams, and library comparisons are required to verify
results
Response factors and multipoint calibrations—the
data system shall be used to record and maintain
lists ot response factors (response ratios for isotope
dilution) and multipoint calibration curves (section 7)
Computations of relative standard deviation (coeffi-
cient of variation) are useful for testing calibration
linearity Statistics on initial (section 8 4) and on-
going (section 12 7) performance shall be computed
and maintained
REAGENTS AND STANDARDS
Sodium hydroxide—reagent grade, 6N in reagent
water
Sulfuric acid—reagent grade, 6N in reagent water
Sodium sulfa'e—reagent grade, granular anhydrous,
rinsed with methylene chloride (20 mUg) and condi-
tioned at 450°C for one hour minimum
Methylene chloride—distilled in glass (Burdick and
Jackson, or equivalent)
Reagent water—water in which the compounds of in-
te'est and interfering compounds are not detected by
th's method
Standard solutions—purchased as solutions or mix-
tures with certification to their purity, concentration,
and authenticity, or prepared from materials of
known purity and composition If compound purity is
96 percent or greater, the weight may be used
without correction to compute the concentration of
the standard When not being used, standards are
stored in the dark at -20 to -10°C in screw-
capped vials with Teflon-lined lids A mark is placed
on the vial at the level of the solution so that solvent
evaporation loss can be detected The vials are
brought to room temperature prior to use Any
precipitate is redissolved and solvent is added if sol-
vent loss has occurred
Preparation of stock solutions—prepare in
methylene chloride, benzene, p-dioxane, or a mixture
of these solvents per the steps below Observe the
sa'ety precautions given in section 4 The large
number of labeled and unlabeled acid, base/neutral,
and Appendix C compounds used for combined
ca ibration (section 7) and calibration verification
(12 5) require high concentrations (approx 40
mg/mL) when individual stock solutions are
prepared, so that dilutions of mixtures will permit
calibration with all compounds in a single set of solu-
tions The working range for most compounds is
10-200 MQ/mL Compounds with a reduced MS
response may be prepared at higher concentrations
6 7 1 Dissolve an appropriate amount of assayed
reference material in a suitable solvent For example,
weigh 400 mg naphthalene in a 10 mL ground glass
stoppered volumetric flask and fill to the mark with
benzene After the naphthalene is completely
dissolved, transfer the solution to a 15 mL vial with
Teflon-lined cap
6 7 2 Stock standard solutions should be checked foi
signs of degradation prior to the preparation of
calibration or performance test standards Quality
control check samples that can be used to determine
the accuracy of calibration standards are available
from the US Environmental Protection Agency,
Environmental Monitoring and Support Laboratory,
Cincinnati, Ohio 45268
6 7 3 Stock standard solutions shall be replaced after six
months, or sooner if comparison with quality control
check samples indicates a change in concentration
6 8 Labeled compound spiking solution—from stock
standard solutions prepared as above, or from mix-
tures, prepare the spiking solution at a concentration
of 200 Mg/mL, or at a concentration appropriate to
the MS response of each compound
6 9 Secondary standards—using stock solutions (sec-
tion 6 7), prepare a secondary standard containing all
of the compounds in tables 1 and 2 at a concentra-
tion of 400 Mg/mL, or higher concentration ap-
propriate to the MS response of the compound
6 10 Internal standard solution—prepare 2,2'-difluoro-
biphenyl (DFB) at a concentration of 10 mg/mL in
benzene
6 11 DFTPP solution—prepare at 50 Mg/mL in acetone
6 12 Solutions for obtaining authentic mass spectra (sec-
tion 7 2)—prepare mixtures of compounds at con-
centrations which will assure authentic spectra are
obtained for storage in libraries
6 13 Calibration solutions—combine 0 5 mL of the solu-
tion in section 6 8 with 25, 50, 125, 250, and 500 mL
of the solution in section 6 9 and bring to 1 00 mL
total volume each This will produce calibration solu-
tions of nominal 10, 20, 50, 100 and 200 Mg/mL of
the pollutants and a constant nominal 100M9/mL of
the labeled compounds Spike each solution with 10
mL of the internal standard solution (section 6 10)
These solutions permit the relative response (labeled
to unlabeled) to be measured as a function of con-
centration (section 7 4)
6 14 Precision and recovery standard—used for deter-
mination ot initial (section 8 2) and on-going (section
12 7) precision and recovery This solution shall con-
tain the pollutants and labeled compounds at a
nominal concentration of 100 Mg/mL
6 15 Stability of solutions—all standard solutions (sections
6 8-6 14) shall be analyzed within 48 hours of
preparation and on a monthly basis thereafter for
signs of degradation Standards will remain accep-
table if the peak area at the quantitation mass relative
to the DFB internal standard remains within ± 15 per-
cent of the area obtained in the initial analysis of the
standard
7
-------
7 CALIBRATION
7 1 Assemble the GC/MS and establish operating condi-
tions in table 3 Analyze standards per the procedure
in section 11 to demonstrate that the analytical
system meets the detection limits in tables 3 and 4,
and the mass-intensity criteria in table 5 for 50 ng
DFTPP
7 2 Mass spectral libraries—detection and identification
of compounds of interest are dependent upon spec-
tra stored in user created libraries
7 2 1 Obtain a mass spectrum of each pollutant, labeled
compound, and the internal standard by analyzing an
authentic standard either singly or as part of a mix-
ture in which there is no interference between closely
eluted components That only a single compound is
present is determined by examination of the spec-
trum Fragments not attributable to the compound
under study indicate the presence of an interfering
compound
7 2 2 Adjust the analytical conditions and scan rate (for this
test only) to produce an undistorted spectrum at the
GC peak maximum An undistorted spectrum will
usually be obtained if five complete spectra are col-
lected across the upper half of the GC peak Soft-
ware algorithms designed to "enhance" the spec-
trum may eliminate distortion, but may also eliminate
authentic masses or introduce other distortion
7 2 3 The authentic reference spectrum is obtained under
DFTPP tuning conditions (section 7 1 and table 5) to
normalize it to spectra from other instruments
7 2 4 The spectrum is edited by saving the 5 most intense
mass spectral peaks and all other mass spectral
peaks greater than 10 percent of the base peak This
edited spectrum is stored for reverse search and for
compound confirmation
7 3 Analytical range—demonstrate that 20 ng anthra-
cene or phenanthrene produces an area at m/z 178
approx one-tenth that required to exceed the linear
range of the system The exact value must be deter-
mined by experience for each instrument It is used
to match the calibration range of the instrument to the
analytical range and detection limits required, and to
diagnose instrument sensitivity problems (section
15 4) The 20 uglmL calibration standard (section
6 13) can be used to demonstrate this performance
7 31 Polar compound detection—demonstrate that
unlabeled pentachlorophenol and benzidine are
detectable at the 50 jug/mL level (per all criteria in
section 13) The 50 M9/mL calibration standard (sec-
tion 6 13) can be used to demonstrate this perfor-
mance
7 4 Calibration with isotope dilution—isotope dilution is
used when 1) labeled compounds are available, 2) in-
terferences do not preclude its use, and 3) the quan-
titation m/z (tables 6 and 7) extracted ion current pro-
file (EICP) area for the compound is in the calibration
range If any of these conditions preclude isotope
dilution, the internal standard method (section 7 5) is
used
TABLE 6
Base/Neutral Extractable Compound
Characteristic Masses
LABELED
PRIMARY
COMPOUND
ANALOG
M/Z'S
acenaphthene
dio
154/164
acenaphthylene
da
1 52/160
anthracene
dio
178/188
benzidine
d«
184/192
benzo(a)anlhracene
di2
228/240
benzo(b)tluoranthene
di2
252/264
benzo(k)fluoranthene
di2
252/264
benzo(a)pyrene
di2
252/264
benzo(ghi)perylene
di2
276/288
biphenyl
dio
154/164
bis(2-chloroethyl) ether
da
93/101
bis(2-chloroethoxy) methane
93
bis(2-chloroisopropyl) ether
d,2
121/131
bis(2-ethylhexyl) phthalale
d«
149/153
4-bromophenyl phenyl ether
248
butyl benzyl phthaiate
149
n-Cio
d22
55/66
n-Ci2
d26
55/66
n-C t4
55
n-C ia
dj<
55/66
n-Cia
55
n-C2D
d«2
55/66
n-C22
55
n-C24
dso
55/66
n-C2s
55
n-C2B
55
n-Cso
d{2
55/66
carbazole
de
167/175
2-chloronaphthalene
d7
162/169
4-chlorophenyl phenyl ether
d5
204/209
chrysene
d 12
228/240
p-cymene
di4
119/1 30
dibenzo(a,h)anthracene
278
dibenzofuran
da
168/1 76
dibenzothiophene
da
184/192
di-n-butyl phthaiate
d<
1 49/1 53
1,2-dichlorobenzene
d«
146/152
1,3-dichlorobenzene
d.
1 46/1 52
1,4-dichlorobenzene
d.
1 46/1 52
3,3'-dichlorobenzidine
da
252/258
diethyl phthaiate
d<
149/153
2,4-dimethylphenol
di
122/125
dimethyl phthaiate
d<
163/167
2,4-dinitrotoluene
d3
165/168
2.6-dinitrotoluene
ds
165/167
di-n-octyl phthaiate
d4
149/153
diphenylamine
dio
169/179
diphenyl ether
dio
1 70/180
1,2-diphenylhydrazine'
dio
77/82
tluoranlhene
dio
202/212
fluorene
dio
166/176
hexachlorobenzene
,3Ca
284/292
hexachlorobutadiene
,3C<
225/231
hexachloroethane
,3C
201/204
hexachlorocyclopentadiene
,3C,
237/241
ideno(1,2,3-cd)pyrene
276
isophorone
da
82/88
naphthalene
da
128/136
beta-naphthylamine
dj
143/150
nitrobenzene
d5
123/128
N-nitrosodimethylamme
74
N-nitrosodi-n-propylamine
70
N-nitrosodiphenylamme''
ds
169/175
phenanthrene
dio
178/188
8
-------
TABLE 6 (Continued)
Base/Neutral Extractable Compound
Characteristic Masses
LABELED
PRIMARY
COMPOUND
ANALOG
M/Z'S
phenol
d5
94/71
alpha-picoline
d7
93/100
pyiene
dio
202/212
styrene
d5
104/109
alpha-lerpineol
d3
59/62
1,2,3-trichlorobenzene
d3
180/183
1,2,4-trichlorobenzene
d3
180/183
"detected as azobenzene
' 'delected as diphenylamme
TABLE 7
Acid Extractable Compound
Characteristic Masses
LABELED
PRIMARY
COMPOUND
ANALOG
M/Z'S
4-chloro-3-methvlphenol
d2
107/109
2-chlorophenol
d4
128/132
2,4-dichlorophenol
d3
162/167
2,4-dmitrophenol
d3
184/187
2-methyl-4,6-din tropheaol
d2
198/200
2-nitrophenol
d.
139/143
4-nitrophenol
d»
139/143
pentachlorophenol
,3Ca
266/272
2,3,6-trichlorophenol
d2
196/200
2,4,5-trichlorophenol
d2
196/200
2,4,6-trichloroph9nol
d2
196/200
7 4 1 A calibration curve encompassing the concentration
range is prepa'ed tor each compound determined
The relative response (pollutant to labeled) vs con-
centration in standard solutions is plotted or com-
puted using a linear regression The example in
figure 1 shows a calibration curve for phenol using
i i i i i i
T 1 1 1 1 r~
2 10 20 50 100 200
CONCENTRATION (gg/mL)
FIGURE 1 Relative Response Calibration Curve
for Phenol. The Dotted Lines Enclose a ± lO Per-
cent Error Window
phenol-ds as the isotopic diluent Also shown are the
±10 percent error limits (dotted lines) Relative
Response (RR) is determined according to the pro-
cedures described below A minumum of five data
points are employed for calibration
7 4 2 The relative response of a pollutant to its labeled
analog is determined from isotope ratio values com-
puted from acquired data Three isotope ratios are
used in this process
Rx= the isotope ratio measured for the pure
pollutant
Ry= the isotope ratio measured for the labeled
compound
Rm= the isotope ratio of an analytical mixture of
pollutant and labeled compounds
The mlz's are selected such that Rx > Ry If Rm is not
between 2Ry and 0 5RX, the method does not apply
and the sample is analyzed by the internal standard
method (section 7 5)
7 4 3 Capillary columns usually separate the pollutant-
labeled pair, with the labeled compound eluted first
(figure 2) For this case,
D _ [area m,/z]
"x •
1
at the retention time of the pollutant (RT2)
Ry = ^
[area m2/z]
at the retention time of the labeled compound (RT,)
p _ [area m,/z (at RT2)]
nm — .
[area m2/z (at RT,)]
as measured in the mixture of the pollutant and la-
beled compounds (figure 2), and RR = Rm
AREA AT
MJZ
AREA AT
M,/Z
RT,
FIGURE 2 Extracted Ion Current Profiles for
Chromatographically Resolved Labeled (m,/z)
and Unlabeled (m,/z) Pairs.
7 4 4 Special precautions are taken when the pollutant-
labeled pair is not separated, or when another la-
beled compound with interfering spectral masses
overlaps the pollutant (a case which can occur with
isomeric compounds) In this case, it is necessary to
determine the respective contributions of the pollu-
tant and labeled compounds to the respective EICP
areas If the peaks are separated well enough to per-
mit the data system or operator to remove the con-
tributions of the compounds to each other, the equa-
tions in section 7 4 3 apply This usually occurs
when the height of the valley between the two GC
peaks at the same m/z is less than 10 percent of the
height of the shorter of the two peaks If significant
9
-------
GC and spectral overlap occur, RR is computed us-
ing the following equation
pp _ (Ry~ RmX^x"*" 1 )
(Rm— RxKRy+1)
where Rx is measured as shown in figure 3A, Ry is
measured as shown in figure 3B, and Rm is
measured as shown in figure 3C For the example,
R _ 46100 _ 9 644
Ry =
4780
_ 2650
43600
49200
. = 0 0608
= 1 019
745
48300
RR =1 114
To calibrate the analytical system by isotope dilution,
analyze a 1 OfiL aliquot of each of the calibration
standards (section 6 13) using the procedure in sec-
tion 11 Compute the RR at each concentration
AREA = 4780
AREA = 46100
(3B)
AREA = 2650
AREA = 43600
AREA = 48300
AREA = 49200
7 4 6
75
FIGURE 3 Extracted Ion Current Profiles lor (3A)
Unlabeled Compound, (3B) Labeled Com-
pound, and (3C) Equal Mixture of Unlabeled
and Labeled Compounds.
Linearity—if the ratio of relative response to concen-
tration for any compound is constant (less than 20
percent coefficient of variation) over the 5 point
calibration range, an averaged relative response/
concentration ratio may be used for that compound,
otherwise, the complete calibration curve for that
compound shall be used over the 5 point calibration
range
Calibration by internal standard—used when criteria
for isotope dilution (section 7 4) cannot be met The
internal standard to be used for both acid and
base/neutral analyses is 2,2'-difluorobiphenyl The
internal standard method is also applied to deter-
mination of compounds having no labeled analog,
and to measurement of labeled compounds for intra-
laboratory statistics (sections 8 4 and 12 7 4)
7 5 1 Response factors—calibration requires the deter-
mination of response factors (RF) which are defined
by the following equation
RF = (As x C|s) , where
(A|S X Cs),
As is the area at the characteristic mass for the com-
pound in the daily standard
A,s is the area of the characteristic mass for the inter-
nal standard
CIS is the concentration of the internal standard
(ftg/mL)
Cs is the concentration of the compound in the daily
standard (ug/mL)
7 5 11 The response factor is determined for at least five
concentrations appropriate to the response of each
compound (section 6 13), nominally, 10, 20, 50,100,
and 200 /ug/mL The amount of internal standard
added to each extract is the same (100 /ug/mL) so
that CIS remains constant The RF is plotted vs con-
centration for each compound in the standard (Cg) to
produce a calibration curve
7 5 12 Linearity—if the response factor (RF) for any com-
pound is constant (less than 35 percent coefficient of
variation) over the 5 point calibration range, an
averaged response factor may be used for that com-
pound, otherwise, the complete calibration curve for
that compound shall be used over the 5 point range
7 6 Combined calibration—by using calibration solutions
(section 6 13) containing the pollutants, labeled com-
pounds, and the internal standard, a single set of
analyses can be used to produce calibration curves
for the isotope dilution and internal standard
methods These curves are verified each shift (sec-
tion 12 5) by analyzing the 100/ug/mL calibration
standard (section 6 13) Recalibration is required
only if calibration verification (section 12 5) criteria
cannot be met
8 QUALITY ASSURANCE/QUALITY CONTROL
8 1 Each laboratory that uses this method is required to
operate a formal quality assurance program The
minimum requirements of this program consist of an
initial demonstration of laboratory capability, analysis
of samples spiked with labeled compounds to
evaluate and document data quality, and analysis of
standards and blanks as tests of continued perfor-
mance Laboratory performance is compared to
established performance criteria to determine if the
results of analyses meet the performance character-
istics of the method
8 1 1 The analyst shall make an initial demonstration of the
ability to generate acceptable accuracy and preci-
sion with this method This ability is established as
described in section 8 2
8 1 2 The analyst is permitted to modify this method to im-
prove separations or lower the costs of
measurements, provided all performance specifica-
tions are met Each time a modification is made to the
method, the analyst is required to repeat the pro-
cedure in section 8 2 to demonstrate method perfor-
mance
lO
-------
8 1 3 Analyses ol blanks are required to demonstrate
freedom from contamination The procedures and
criteria for analysis of a blank are described in sec-
tions 8 5
8 1 4 The laboratory shall spike all samples with labeled
compounds to monitor method performance This
test is described in section 8 3 When results of these
spikes indicate atypical method performance for
samples, the samples are diluted to bring method
performance within acceptable limits (section 15)
815 Tne laboratory shall, on an on-going basis,
demonstrate through calibration verification and the
analysis of the precision and recovery standard (sec-
tion 6 14) that the analysis system is in control
These procedures are described in sections 12 1,
12 5, and 12 7
8 1 6 The laboratory shall maintain records to define the
quality of data that is generated Development of ac-
curacy statements is described in section 8 4
8 2 Initial precision and accuracy—to establish the ability
to generate acceptable precision and accuracy, the
analyst shall perform the following operations
8 2 1 Extract, concentrate, and analyze two sets of four
one-liter aliquots (8 aliquots total) of the precision and
recovery standard (section 6 14) according to the
procedure in section 10
8 2 2 Using results of the first seJ_of four analyses, com-
pute the average recovery (X) in /*g/mL and the stan-
dard deviation of the recovery (s) in /tg/mL for each
compound, by isotope dilution for pollutants with a
labeled analog, and by internal standard for labeled
compounds and pollutants with no labeled analog
8 2 3 For each compound, compare s and X with the cor-
responding limits for initial precision and accuracy in
table 8 If s and X for all compounds meet the accep-
tance criteria, system performance is acceptable and
analysis of blanks and samples may begin If,
however, any individual s exceeds the precision limit
or any individual X falls outside the range for ac-
curacy, system performance is unacceptable for that
compound NOTE The large number of compounds
in table 8 present a substantial probability that one or
more will fail one of the acceptance criteria when all
compounds are analyzed To determine if the
analytical system is out of control, or if the failure can
be attributed to probability, proceed as follows
8 2 4 Using the results of the second set of four analyses,
compute s and ^ for only those compounds which
failed the test of the first set of four analyses (section
TABLE 8
Acceptance Criteria for Performance Tests
ACCEPTANCE CRITERIA
INITIAL
LABELED
CALIBRA-
PRECISION
COMPOUND
TION
AND ACCURACY
RECOVERY
VERIFI-
ON-GOING
EGD
SECTION 8 2 3
SECTION 8 3
CATION
ACCURACY
NO
(UU/L)
AND 14 2
SECTION 12 5 SECTION 12 7
(V
COMPOUND
s
X
P<%)
(UO/mL)
R (mq/L)
30"
acenaphlhene
21
79-134
80 - 125
72 - 144
20
acenaphthene-dto
38
38-147
20 - 270
71-141
30-180
377
acenaphthylene
38
69 -186
60 - 166
61 - 207
277
acenaphthyiene-da
31
39-146
23 - 239
66 -152
33-168
378
anthracene
41
58-174
60 -168
50- 199
278
anthracene-d,0
49
31 - 194
14-419
58-171
23 - 242
305
benzidine
119
16-518
34 - 296
11-672
205
benzidine-da
269
ns - ns
ns - ns
ns - ns
ns - ns
372
benzo(a)anthracene
20
65 -168
70 -142
62-176
272
benzo(a)anth racene-d 12
41
25 - 298
12 - 605
28 - 357
22 - 329
374
benzo(b)fluoranihene
183
32 -545
61-164
20 - ns
274
benzo(b)fluoranthene-d,j
168
11-577
ns - ns
14 - ns
ns - ns
375
benzo(k)fluoranthene
26
59-143
13 - ns
53-155
275
benzo(k)fluoranthene-d 12
114
15-514
ns - ns
13 - ns
ns - 685
373
benzo(a)pyrene
26
62-195
78 -129
59 - 206
273
benzo(a)pyrene-d,2
24
35-181
21 -290
12 - ns
32-194
379
benzo(ghi)perylene
21
72-160
69 -145
58-168
279
benzo(ghi)perylene-d, 2
45
29 - 268
14 - 529
13 - ns
25 - 303
712
biphenyl (Appendix C)
41
75-148
58-171
62-176
612
biphenyl-d,0
43
28-165
ns - ns
52-192
17-267
318
bis(2-chloroethyl) ether
34
55-196
61-164
50-213
218
bis(2-chloroethyl) ether-d9
33
29-196
15-372
52 -194
25 - 222
043
bis(2-chlorceihyoxy) methane'
27
43-153
44 - 228
39-166
342
bis(2-chloroisopropyl) ether
17
81-138
67-148
77-145
242
bis(2-chloroisopropyl) ether-d12
27
35 - 149
20 - 260
44 - 229
30-169
366
bis(2-ethylhexyl) phthalate
31
69 - 220
76-131
64 - 232
266
bis(2-ethylhexyl) phthalate-d<
29
32 - 205
18 - 364
43 - 232
28 - 224
041
4-bromophenyl phenyl ether*
44
44-140
52 - 193
35-172
067
butyl benzyl phthalate*
31
37-183
22 - 450
35-195
11
-------
TABLE 8 (Continued)
Acceptance Criteria for Performance Tests
ACCEPTANCE CRITERIA
EGD
NO
INITIAL
PRECISION
AND ACCURACY
SECTION 8 2 3
(PQ/L)
LABELED
COMPOUND
RECOVERY
SECTION 8 3
AND 14 2
CALIBRA-
TION
VERIFI- ON-GOING
CATION ACCURACY
SECTION 12 5 SECTION 12 7
(1)
COMPOUND
s
X
P<%)
(UO/mL)
R (UO/L)
717
n-Cio (Appendix C)
51
24-195
42 - 235
19-237
617
n-Cio-d22
70
ns - 298
ns - ns
44 - 227
ns - 404
706
n-Ci2 (Appendix C)
74
35 - 369
60 - 166
29-424
606
n-C 12-028
53
ns - 331
ns - ns
41 - 242
ns - 408
518
n-Cn (Appendix C)'
109
ns - 985
37 - 268
ns - ns
719
n-C,6 (Appendix C)*
33
80- 162
72-138
71-181
619
rv-Ci8-d3<
46
37-162
18-308
54 -186
28 - 202
520
n-Cis (Appendix C)"
39
42-131
40 - 249
35-167
721
n-C2o (Appendix C)
59
53 - 263
54 - 184
46-301
621
n-Cpo-C. ?
34
34-172
19-306
62 -162
29 -198
522
n-C22 (Appendix C)"
31
41 - 184
40 - 249
39-195
723
n-C21 (Appendix C)
11
80-139
65-154
78-142
623
n-C2»-d5o
28
27-211
15-376
50- 199
25 - 229
524
n-C26 (Appendix C)*
35
35-193
26 - 392
31-212
525
n-C2» (Appendix C)*
35
35-193
26 - 392
31 -212
726
n-C30 (Appendix C)
32
61 - 200
66 -152
56-215
626
n-C3o-de2
41
27- 242
13-479
24 -423
23-274
528
carbazole (4c)*
38
36-165
44 -227
31-188
320
2-chloronaphthalene
100
46-357
58-171
35-442
220
2-chloronaphthalene-dr
41
30-168
15-324
72-139
24 - 204
322
4-chloro-3-methylphenol
37
76-131
85 -115
62 -159
222
4-chloro-3-methytphenol-d2
111
30-174
ns - 613
68-147
14-314
324
2-chlorophenol
13
79- 135
78-129
76-138
224
2-chlorophenol-dj
24
36- 162
23 - 255
55-180
33-176
340
4-chlorophenyl phenyl ether
42
75-166
71-142
63-194
240
4-chlorophenyl phenyl ether-d5
52
40-161
19-325
57-175
29-212
376
chrysene
51
59-186
70-142
48- 221
276
chrysene-di2
69
33-219
13-512
24 -411
23 - 290
713
p-cymene (Appendix C)
18
76-140
79-127
72-147
613
p-cymene-du
67
ns - 359
ns - ns
66 - 152
ns - 468
082
dibenzo(a,h)anthracene'
55
23 - 299
13-761
19-340
705
dibenzofuran (Appendix C)
20
85-136
73-136
79 - 1 46
605
dibenzofuran-ds
31
47-136
28 - 220
66 - 150
39 -160
704
dibenzothiophene (Synluel)
31
79-150
72-140
70 - 168
604
dibenzothiophene-d6
31
48-130
29-215
69-145
40-156
368
di-n-butyl phthalate
15
76-165
71 - 142
74 -169
268
di-n-butyl phthalate-da
23
23-195
1 3 - 346
52-192
22 - 209
325
1,2-dichlorobenzene
17
73-146
74-135
70-152
225
1,2-dichlorobenzene-d)
35
14-212
ns - 494
61-164
11-247
326
1,3-dichlorobenzene
43
63 - 201
65 - 1 54
55 - 225
226
1.3-dichlorobenzejie-d4
48
13-203
ns - 550
52-192
ns - 260
327
1,4-dichlorobenzene
42
61 - 194
62-161
53-219
227
1,4-dichlorobenzene-d»
48
15-193
ns - 474
65 -153
11 - 245
328
3,3-dichlorobenzidine
26
68 - 1 74
77-130
64 - 185
228
3,3'-dichlorobenzidine-da
80
ns - 562
ns - ns
18 - 558
ns - ns
331
2,4-dichlorophenol
12
85-131
67 -149
83-135
231
2,4-dichlorophenol-d3
28
38-164
24 - 260
64-157
34 - 182
370
diethyl phthalate
44
75 - 196
74-135
65-222
270
diethyl phthalate-d4
78
ns - 260
ns - ns
47-211
ns - ns
334
2,4-dimethylphenol
13
62-153
67-150
60 - 156
234
2,4-dimethylphenol-d3
22
15-228
ns - 449
58-172
14 - 242
3/1
dimethyl phthalate
36
74-188
73-137
67 - 207
271
dimethyl phthalale-d«
108
ns - 640
ns - ns
50 - 201
ns - ns
359
2,4-dinitrophenol
18
72 - 134
75-133
68-141
259
2,4-dinitrophenol-
-------
TABLE 8 (Continued)
Acceptance Criteria lor Performance Tests
ACCEPTANCE CRITERIA
EGD
NO
INITIAL
PRECISION
AND ACCURACY
SECTION 8 2 3
(UO/D
LABELED
COMPOUND
RECOVERY
SECTION 0 3
AND 14 2
CALIBRA-
TION
VERIFI- ON-GOING
CATION ACCURACY
SECTION 12 5 SECTION 12 7
(1)
COMPOUND
s
X
P(%)
(ug/mL)
R (MQ/L)
269
di-n-octy phthalate-d<
46
12 - 383
ns - ns
21 -467
10-433
707
diphenylamine (Appendix C)
45
58 - 205
57 -1 76
51 -231
607
diphenylamine-dio
42
27 - 206
11 - 488
59 -169
21 - 249
708 diphenyl ether (Appendix C)
19
82 -136
83 -120
77-144
608
diphenyl elher-dio
37
36-155
19-281
77-129
29 - 186
337
1,2-diphenylhydrazine
73
49 - 308
75 -134
40 - 360
237
1,2-diphenylhydrazine-dio
35
31-173
17-316
58-174
26 - 200
339
fluoranthene
33
71 -177
67 -149
64 - 194
239
fluoranthene-dio
35
36-161
20-278
47-215
30-187
380
fluorene
29
81 -132
74 -135
70-151
280
lluorene-dio
43
51 -131
27 - 238
61 -164
38-172
309
hexachlorobenzene
16
90-124
78 -128
85-132
209
hexachlorobenzene-13C6
81
36 - 228
13-595
38 - 265
23 - 321
352
hexachlorobutadiene
56
51 - 251
74-135
43-287
252
hexachlorobutadiene-13C«
63
ns - 316
ns - ns
68 -1 48
ns - 413
312
hexachloi oethane
227
21 - ns
71-141
13 - ns
212
hexachloi oethane-'3C,
77
ns - 400
ns - ns
47-212
ns - 563
353
hexachloi ocyclopentadiene
15
69-144
77-129
67-148
2E3
hexachloi ocyclopentadiene-,3C<
60
ns - ns
ns - ns
47-211
ns - ns
083
ideno(1,2,3-cd)pryene*
55
23 - 299
13-761
19 - 340
354
isophorone
25
76- 156
70-142
70 - 168
254
isophorone-da
23
49-133
33 -193
52 - 194
44-147
360
2-methyl-4,6-dinitrophenol
19
77-133
69 -1 45
72-142
260
2-methyl-4,6-dinitrophenol-d2
64
36- 247
16-527
56 -1 77
28 - 307
355
naphthalene
20
80-139
73-137
75-149
255
naphthalene-do
39
28-157
14 - 305
71-141
22 - 192
702
beta-naphthylamine (Appendix C)
49
10 - ns
39 - 256
ns - ns
602
beta-naphthylamine-d7
33
ns - ns
ns - ns
44 -230
ns - ns
356
nitrobenzene
25
69-161
85 -115
65-169
256
mtrobenzene-d5
28
18-265
ns - ns
46-219
15-314
357
2-nitrophenol
15
78-140
77-129
75-145
257
2-nitrophenol-d4
23
41-145
27-217
61-163
37-158
358
4-nitropherol
42
62-146
55-183
51-175
258
4-nitrophenol-d,
188
14 - 398
ns - ns
35 - 287
ns - ns
061
N-nitrosodimethylamine*
198
21 -472
40 - 249
12 - ns
063
N-nitrosodi-n-propylamine'
198
21 - 472
40 - 249
12 - ns
362
N-nitrosodiphenylamine
45
65-142
68 -148
53-173
262
N-nitrosodiphenylamme-d6
37
54 - 126
26 - 256
59-170
40-166
364
pentachloiophenol
21
76-140
77-130
71-150
264
pentachloiophenol-'3C6
49
37-212
18-412
42 -237
29 - 254
381
phenanthrene
13
93 - 119
75-133
87-126
281
phenanthrene-dio
40
45-130
24 -241
67-149
34 - 168
365
phenol
36
77-127
65-155
62-154
26b
phenol-d5
161
21 -210
ns - ns
48 - 208
ns - ns
703
alpha-pico.me (Synfuel)
36
59-149
60-165
50 - 1 74
603
alpha-pico ine-dr
138
11 - 380
ns - ns
31 -324
ns - 608
384
pyrene
19
76-152
76-132
72-159
284
pyrene-dio
29
32-176
18 - 303
48-210
28 - 196
710
styrene (Aopendix C)
42
53-221
65-153
48 - 244
610
styrene-d5
49
ns - 281
ns - ns
44 - 228
ns - 348
709
alpha-terpneol (Appendix C)
44
42- 234
54 -186
38 - 258
609
alpha-terpneol-d3
48
22-292
ns - 672
20 - 502
18-339
529
1,2,3-trichlorobenzene (4c)"
69
15-229
60-167
11 - 297
308
1,2.4-trichlorobenzene
19
82 - 136
78-128
77-144
208
1,2,4-trichlorobenzene-d3
57
15-212
ns - 592
61-163
10-282
53C
2,3,6-trichlorophenol (4c)*
30
58-137
56 -180
51-153
531
2 4,5-trichlorophenol (4c)*
30
58-137
56-180
51-153
321
2,4,6-trichlorophenol
57
59 - 205
81-123
48 - 244
221
2,4,6-trichlorophenol-d2
47
43-183
21 - 363
69 -144
34 - 226
(1) Reference numbers beginning with 0 1 or 5 indicate a polutant quantified by the internal standard method, reference numbers beginning with 2 or 6
indicate a labeled compound quantified by the internal standard method, reference numbers beginning with 3 or 7 indicate a pollutant quantified by
isotope dilution
* measured by internal standard specification derived from related compound
ns - no specification limit is outside the range that can be measured reliably 1
-------
8 2 3) If these compounds now pass, system perfor-
mance is acceptable for all compounds and analysis
of blanks and samples may begin If, however, any of
the same compounds fail again, the analysis system
is not performing properly for the compounds In this
event, correct the problem and repeat the entire test
(section 8 21)
8 3 The laboratory shall spike all samples with labeled
compounds to assess method performance on the
sample matrix
8 3 1 Analyze each sample according to the method
beginning in section 10
8 3 2 Compute the percent recovery (P) of the labeled
compounds using the internal standard method (sec-
tion 7 5)
8 3 3 Compare the labeled compound recovery for each
compound with the corresponding limits in table 8 If
the recovery of any compound falls outside its warn-
ing limit, method performance is unacceptable for
that compound in that sample Therefore, the sample
matrix is complex and is to be diluted and reanalyzed
per section 15 4
8 4 As part of the OA program for the laboratory, method
accuracy for wastewater samples shall be assessed
and records shall be maintained After the analysis of
five wastewater samples for which the labeled com-
pounds pass the tests in section 8 3, compute the
average percent recovery (P) and the standard devia-
tion of the percent recovery (sp) for the labeled com-
pounds only Express the accuracy assessment as a
percent recovery interval from P - 2sp to P + 2sp
For example, if P = 90% and sp = 10%, the ac-
curacy interval is expressed as 70-110% Update the
accuracy assessment for each compound on a
regular basis (e g after each 5-10 new accuracy
measurements)
8 5 Blanks—reagent water blanks are analyzed to
demonstrate freedom from contamination
8 5 1 Extract and concentrate a blank with each sample lot
(samples started through the extraction process on
the same 8 hr shift, to a maximum of 20 samples)
Analyze the blank immediately after analysis of the
precision and recovery standard (section 614) to
demonstrate freedom from contamination
8 5 2 If any of the compounds of interest (tables 1 and 2) or
any potentially interfering compound is found in a
blank at greater than 10 uglL (assuming a response
factor of 1 relative to the internal standard for com-
pounds not listed in tables 1 and 2), analysis of
samples is halted until the source of contamination is
eliminated and a blank shows no evidence of con-
tamination at this level
8 6 The specifications contained in this method can be
met if the apparatus used is calibrated properly, then
maintained in a calibrated state The standards used
for calibration (section 7), calibration verification
(section 12 5), and for initial (section 8 2) and on-
going (section 12 7) precision and recovery should
be identical, so that the most precise results will be
obtained The GC/MS instrument in particular will
provide the most reproducible results if dedicated to
the settings and conditions required for the analyses
of semivolatiles by this method
8 7 Depending on specific program requirements, field
replicates may be collected to determine the preci-
sion of the sampling technique, and spiked samples
may be required to determine the accuracy of the
analysis when internal or external standard methods
are used
9 SAMPLE COLLECTION, PRESERVATION, AND
HANDLING
9 1 Collect samples in glass containers following con-
ventional sampling practices (reference 7) Com-
posite samples are collected in refrigerated glass
containers (section 5 1 3) in accordance with the re-
quirements of the sampling program
9 2 Maintain samples at 0-4 °C from the time of collection
until extraction If residual chlorine is present, add 80
mg sodium thiosulfate per liter of water EPA
Methods 330 4 and 330 5 may be used to measure
residual chlorine (reference 8)
9 3 Begin sample extraction within seven days of collec-
tion, and analyze all extracts within 40 days of extrac-
tion
10 SAMPLE EXTRACTION AND CONCENTRATION
(See figure 4)
10 1 Labeled compound spiking—measure 1 00 + 0 01
liter of sample into a glass container For untreated
effluents, and samples which are expected to be dif-
ficult to extract and/or concentrate, measure an addi-
tional 10 0 ± 0 1 mL and dilute to a final volume of
1 00 ± 0 1 liter with reagent water in a glass con-
tainer
10 11 For each sample or sample lot (to a maximum of 20)
to be extracted at the same time, place three 1 00 ±
0 01 liter aliquots of reagent water in glass con-
tainers
10 12 Spike 0 5 mL of the labeled compound spiking solu-
tion (section 6 8) into all samples and one reagent
water aliquot
10 13 Spike 1 0 mL of the precision and recovery standard
(section 6 14) into the two remaining reagent water
aliquots
10 14 Stir and equilibrate all solutions for 1-2 hr
10 2 Base/neutral extraction—place 100-150 mL
methylene chloride in each continuous extractor and
200-300 mL in each distilling flask
10 2 1 Pour the sample(s), blank, and standard aliquots into
the extractors Rinse the glass containers with
50-100 mL methylene chloride and add to the
respective extractor
10 2 2 Adjust the pH of the waters in the extractors to 12-13
with 6N NaOH while monitoring with a pH meter
Begin the extraction by heating the flask until the
methylene chloride is boiling When properly ad-
justed, 1-2 drops of methylene chloride per second
will fall from the condenser tip into the water After
1-2 hours of extraction, test the pH and readjust to
12-13 if required Extract (or 18-24 hours
10 2 3 Remove the distilling flask, estimate and record the
14
-------
STANDARD
[10.1.11
[10.1.2]
110.1.3]
[10.1.4]
[10.2|
[10.31
[10.4 2]
[10.4,10.51
[11.31
[11-41
1 L REAGENT
WATER
SPIKE
1 0 mL
OF STANDARDS
STIR AND
EQUILIBRATE
STANDARD OR BLANK
EXTRACT BASE/
NEUTRAL
ORGANIC
AQUEOUS
CONCENTRATE
TO 1 0 mL
ADD INTERNAL
STANDARD
INJECT
BLANK
1 L REAGENT
WATER
SAMPLE
STIR AND
EQUILIBRATE
J,
EXTRACT ACID
N
f
N
CONCENTRATE
CONCENTRATE
TO 2-4 mL
TO 2-4 mL
N
SPIKE
OF 200
ISOT
500 pL
pg/mL
3PES
1 L ALIQUOT
>
f
SPIKE
OF 200
ISOT
500 pL
pg/mL
DPES
STIR AND
EQUILIBRATE
EXTRACT BASE/
NEUTRAL
ORGANIC T AQUEOUS
^
EXTRACT ACID
CONCENTRATE
TO 1 0 mL
CONCE
TO 1
SITRATE
0 mL
V
f
>
f
ADD INTERNAL
STANDARD
ADD INTERNAL
STANDARD
N
>
f
INJECT
INJECT
FIGURE 4 Flow Chart for Extraction/Concentration of Precision and Recovery Standard, Blank, and Sample by
Method 1625. Numbers in Brackets [ ] Refer to Section Numbers in the Method
15
-------
volume of extract (to the nearest 100 mL), and pour 11
the contents through a drying column containing 7 to 1 -| -|
10 cm anhydrous sodium sulfate Rinse the distilling
flask with 30-50 mL of methylene chloride and pour
through the drying column Collect the solution in a
500 mL K-D evaporator flask equipped with a 10 mL
concentrator tube Seal, label as the base/neutral 11 2
fraction, and concentrate per sections 10 4 to 10 5
10 3 Acid extraction—adjust the pH of the waters in the
extractors to 2 or less using 6N sulfuric acid Charge
clean distilling flasks with 300-400 mL of methylene .. 3
chloride Test and adjust the pH of the waters after
the first 1-2 hr of extraction Extract for 18-24 hours
10 3 1 Repeat section 10 2 3, except label as the acid frac-
tion
10 4 Concentration—concentrate the extracts in separate 11 4
500 mL K-D flasks equipped with 10 mL concentrator
tubes
10 4 1 Add 1 to 2 clean boiling chips to the flask and attach
a three-ball macro Snyder column Prewet the col-
umn by adding approximately one mL of methylene
chloride through the top Place the K-D apparatus in a
hot water bath so that the entire lower rounded sur-
face of the flask is bathed with steam Adjust the ver-
tical position of the apparatus and the water
temperature as required to complete the concentra-
tion in 15 to 20 minutes At the proper rate of distilla- 12
tion, the balls of the column will actively chatter but j 2 1
the chambers will not flood When the liquid has
reached an apparent volume of 1 mL, remove the
K-D apparatus from the bath and allow the solvent to
drain and cool for at least 10 minutes Remove the
Snyder column and rinse the flask and its lower joint
into the concentrator tube with 1-2 mL of methylene
chloride A 5-mL syringe is recommended for this
operation
10 4 2 For performance standards (section 8 2 and 12 7)
and for blanks (section 8 5), combine the acid and
base/neutral extracts for each at this point Do not 12 2
combine the acid and base/neutral extracts for
samples
10 5 Add a clean boiling chip and attach a two ball micro
Snyder column to the concentrator tube Prewet the
column by adding approx 0 5 mL methylene chloride 12 3
through the top Place the apparatus in the hot water
bath Adjust the vertical position and the water
temperature as required to complete the concentra-
tion in 5-10 minutes At the proper rate of distillation,
the balls of the column will actively chatter but the 124
chambers will not flood When the liquid reaches an
apparent volume of approx 0 5 mL, remove the ap-
paratus from the water bath and allow to drain and
cool for at least 10 minutes Remove the micro 125
Snyder column and rinse its lower joint into the con-
centrator tube with approx 0 2 mL of methylene
chloride Adjust the final volume to 1 0 mL
10 6 Transfer the concentrated extract to a clean screw-
cap vial Seal the vial with a Teflon-lined lid, and mark
the level on the vial Label with the sample number
and fraction, and store in the dark at - 20 to - 10°C
until ready for analysis
GC/MS ANALYSIS
Establish the operating conditions given in tables 3 or
4 for analysis of the base/neutral or acid extracts,
respectively For analysis of combined extracts (sec-
tion 10 4 2), use the operating conditions in table 3
Bring the concentrated extract (section 10 6) or stan-
dard (sections 6 13-6 14) to room temperature and
verify that any precipitate has redissolved Verify the
level on the extract (sections 6 6 and 10 6) and bring
to the mark with solvent if required
Add the internal standard solution (section 6 10) to
the extract (use 1 0 nL of solution per 0 1 mL of
extract) immediately prior to injection to minimize the
possibility of loss by evaporation, adsorption, or
reaction Mix thoroughly
Inject a volume of the standard solution or extract
such that 100 ng of the internal standard will be in-
jected, using on-column or splitless injection For 1
mL extracts, this volume will be 1 0 nl Start the GC
column initial isothermal hold upon injection Start
MS data collection after the solvent peak elutes Stop
data collection after the benzo (ghi) perylene or pen-
tachlorophenol peak elutes for the base/neutral or
acid fraction, respectively Return the column to the
initial temperature for analysis of the next sample
SYSTEM AND LABORATORY PERFORMANCE
At the beginning of each 8 hr shift during which
analyses are performed, GC/MS system perfor-
mance and calibration are verified for all pollutants
and labeled compounds For these tests, analysis of
the 100 /ig/mL calibration standard (section 6 13)
shall be used to verify all performance criteria Ad-
justment and/or recalibration (per section 7) shall be
performed until all performance criteria are met Only
after all performance criteria are met may samples,
blanks, and precision and recovery standards be
analyzed
DFTPP spectrum validity—inject 1 fit of the DFTPP
solution (section 6 11) either separately or within a
few seconds of injection of the standard (section
12 1) analyzed at the beginning of each shift The
criteria in table 5 shall be met
Retention times—the absolute retention time of
2,2 -difluorobiphenyl shall be within the range of
1078 to 1248 seconds and the relative retention
times of all pollutants and labeled compounds shall
fall within the limits given in tables 3 and 4
GC resolution—the valley height between an-
thracene and phenanthrene at m/z 178 (or the
analogs at m/z 188) shall not exceed 10 percent of
the taller of the two peaks
Calibration verification—compute the concentration
of each pollutant (tables 1 and 2) by isotope dilution
(section 7 4) for those compounds which have la-
beled analogs Compute the concentration of each
pollutant which has no labeled analog by the internal
standard method (section 7 5) Compute the concen-
tration of the labeled compounds by the internal stan-
dard method These concentrations are computed
based on the calibration data determined in section 7
16
-------
12 5 1 For each pollutant and labeled compound being
tested, compare the concentration with the calibra-
tion verification limit in table 8 If all compounds meet
the acceptance criteria, calibration has been verified
and analysis of blanks, samples, and precision and
recovery standards may proceed If, however, any
compound fails, the measurement system is not per-
forming properly for that compound In this event,
prepare a fresh calibration standard or correct the
problem causing the failure and repeat the test (sec-
tion 12 1), or recalibrate (section 7)
12 6 Multiple peaks—each compound injected shall give
a single, distinct GC peak
12 7 On-going precision and accuracy
12 7 1 Analyze the extract of one of the pair of precision and
recovery standards (section 1 o 1 3) prior to analysis
of samples from the same lot
12 7 2 Compute the concentration of each pollutant (tables
1 and 2) by isotope dilution (section 7 4) for those
compounds which have labeled analogs Compute
the concentration of each pollutant which has no
labeled analog by the internal standard method (sec-
tion 7 5) Compute the concentration of the labeled
compounds by the internal standard method
12 7 3 For each pollutant and labeled compound, compare
the concentration with the limits for on-going ac-
curacy in table 8 If all compounds meet the accep-
tance criteria, system performance is acceptable and
analysis of blanks and samples may proceed If,
however, any individual concentration falls outside of
the range given, system performance is unaccep-
table for that compound NOTE The large number of
compounds in table 8 present a substantial probabil-
ity that one or more will fail when all compounds are
analyzed To determine if the extraction/concentra-
tion system is out of control or if the failure is caused
by probability, proceed as follows
12 7 3 1 Analyze a second aliquot of the pair of precision and
recovery standards (section 1013)
12 7 3 2 Compute the concentration for only those pollutants
or labeled compounds that failed the previous test
(section 12 7 3) If these compounds now pass, the
extraction/concentration processes are in control
and analyses of blanks and samples may proceed If,
however, any of the same compounds fail again, the
extraction/concentration processes are not being
performed properly for these compounds In this
event, correct the problem, re-extract the sample lot
(section 10) and repeat the on-going precision and
recovery test (section 12 7)
12 7 4 Add results which pass the specifications in 12 7 3 to
initial and previous on-going data Update QC charts
to form a graphic representation of continued
laboratory performance (figure 5) Develop a state-
ment of laboratory accuracy for each pollutant and
labeled compound by calculating the average per-
cent recovery (R) and the standard deviation of per-
cent recovery (sr) Express the accuracy as a
recovery interval from R - 2sr to R + 2sr For exam-
ple, if R = 95% and sr = 5%, the accuracy is
85-105%
5
*
55
o
ui
is
H
lu %
u]
£ z
45,000
35.000
25,000
_1_
_l l_
ANTHRACENE D„
• + 3*>
-35
3 4 5 6 7 8 9
ANALYSIS NUMBER
1 00
> i
UJ <
H
Z
<
ANTHRACENE
. — - #
0 90 i j 1 1 1 1 1 i r~
6/1 6/1 6/1 6/1 6/2 6/2 6/3 6/3 6/4 6/5
DATE ANALYZED
• + 3'>
-3s
FIGURE 5 Quality Control Charts Showing Area
(top graph) and Relative Response of
Anthracene to Anthracene-d10 (lower graph)
Plotted as a Function of Time or Analysis
Number
13 QUALITATIVE DETERMINATION
13 1 Qualitative determination is accomplished by com-
parison of data from analysis of a sample or blank
with data from analysis of the shift standard (section
12 1) and with data stored in the spectral libraries
(section 7 2 4) Identification is confirmed when
spectra and retention times agree per the criteria
below
13 2 Labeled compounds and pollutants having no la-
beled analog
13 2 1 The signals for all characteristic masses stored in the
spectral library (section 7 2 4) shall be present and
shall maximize within the same two consecutive
scans
13 2 2 Either (1) the backgound corrected EICP areas, or (2)
the corrected relative intensities of the mass spectral
peaks at the GC peak maximum shall agree within a
factor of two (0 5 to 2 times) for all masses stored in
the library
13 2 3 The retention time relative to the nearest eluted inter-
nal standard shall be within ± 15 scans or ± 15
seconds, whichever is greater of this difference in the
shift standard (section 12 1)
13 3 Pollutants having a labeled analog
13 31 The signals for all characteristic masses stored in the
spectral library (section 7 2 4) shall be present and
shall maximize within the same two consecutive
scans
13 3 2 Either (1) the backgound corrected EICP areas, or (2)
the corrected relative intensities of the mass spectral
peaks at the GC peak maximum shall agree within a
factor of two for all masses stored in the spectral
library
13 3 3 The retention time difference between the pollutant
and its labeled analog shall agree within ± 6 scans
or ± 6 seconds (whichever is greater) of this dif-
ference in the shift standard (section 12 1)
17
-------
13 4 Masses present in the experimental mass spectrum
that are not present in the reference mass spectrum
shall be accounted for by contaminant or backgound
ions If the experimental mass spectrum is con-
taminated, an experienced spectrometrist (section
1 4) is to determine the presence or absence of the
compound
14 QUANTITATIVE DETERMINATION
14 1 Istope dilution—by adding a known amount of a
labeled compound to every sample prior to extrac-
tion, correction for recovery of the pollutant can be
made because the pollutant and its labeled analog
exhibit the same effects upon extraction, concentra-
tion, and gas chromatography Relative response
(RR) values for sample mixtures are used in conjunc-
tion with calibration curves described in section 7 4
to determine concentrations directly, so long as
labeled compound spiking levels are constant For
the phenol example given in figure 1 (section 7 4 1),
RR would be equal to 1 114 For this RR value, the
phenol calibration curve given in figure 1 indicates a
concentration of 27 /*g/ml_ in the sample extract
(^ex)
14 2 Internal standard—compute the concentration in the
extract using the response factor determined from
calibration data (section 7 5) and the following equa-
tion
Cex (^g/mL) = (As X C|s)
(AIS x RF)
where Cex is the concentration of the compound in
the extract, and the other terms are as defined in sec-
tion 7 5 1
143
14 4
14 5
The concentration of the pollutant in water is com-
puted using the volumes of the original water sample
(section 10 1) and the final extract volume (section
10 5), as follows
_ (Cex x Vex)
Concentration in water (hqIL)
Vs
where Vex is the extract volume in mL, and Vs is the
sample volume in liters
If the EICP area at the quantitation mass for any com-
pound exceeds the calibration range of the system,
the extract of the dilute aliquot (section 101) is
analyzed by isotope dilution, otherwise, the extract is
diluted by a factor of 10, 9 ftL of internal standard
solution (section 6 10) are added to a 1 0 mL aliquot,
and this diluted extract is analyzed by the internal
standard method (section 14 2) Quantify each com-
pound at the highest concentration level within the
calibration range
Report results for all pollutants and labeled com-
pounds (tables 1 and 2) found in all standards,
blanks, and samples, in figlL, to three significant
figures Results for samples which have been diluted
are reported at the least dilute level at which the area
at the quantitation mass is within the calibration
range (section 14 4) and the labeled compound
recovery is within the normal range for the method
(section 15 4)
15 ANALYSIS OF COMPLEX SAMPLES
15 1 Untreated effluents and other samples frequently
contain high levels (>1000 ftgll) of the compounds
of interest, interfering compounds, and/or polymeric
materials Some samples will not concentrate to one
mL (section 10 5), others will overload the GC col-
umn and/or mass spectrometer
15 2 Analyze the dilute aliquot (section 10 1) when the
sample will not concentrate to 1 0 mL If a dilute ali-
quot was not extracted, and the sample holding time
(section 9 3) has not been exceeded, dilute an aliquot
of the sample with reagent water and re-extract (sec-
tion 10 1), otherwise, dilute the extract (section 14 4)
and analyze by the internal standard method (section
14 2)
15 3 Recovery of internal standard—the EICP area of the
internal standard should be within a factor of two of
the area in the shift standard (section 12 1) If the ab-
solute areas of the labeled compounds are within a
factor of two of the respective areas in the shift stan-
dard, and the internal standard area is less than one-
half of its respective area, then internal standard loss
in the extract has occurred In this case, use one of
the labeled compounds (preferably a polynuclear
aromatic hydrocarbon) to compute the concentration
of a pollutant with no labeled analog
15 4 Recovery of labeled compounds—in most samples,
labeled compound recoveries will be similar to those
from reagent water (section 12 7) If the labeled com-
pound recovery is outside the limits given in table 8,
the dilute extract (section 10 1) is analyzed as in sec-
tion 14 4 If the recoveries of all labeled compounds
and the internal standard are low (per the criteria
above), then a loss in instrument sensitivity is the
most likely cause In this case, the 100/
-------
RIC DATA: ABNID1166 #1
03/13/84 5:24:00 CALI: ABN1D1166 ttl
SAMPLE: AB,G,VER,00100,00,C,NA:NA,NA$
CONDS.: 1625fl,30l1,0.25m, 5@30,30-28868,15B280,30CIVSI
RANGE: G 1,3200 LABEL: N 2, 3.0 QUAN: A 2, 2.0 J
SCANS 1 TO 3200
0 BASE: U 20, 3
100.0'
JJ
J
I
715776.
1080
15:50
1500
23:45
r
2888
31:40
2500
39:35
i
3800
47:30
SCAN
TIPIE
FIGURE 6 Chromatogram of Combined Acid/Base/Neutral Standard.
17 REFERENCES
1 "Performance Tests for the Evaluation of Com-
puterized Gas Chromatography/Mass Spectrometry
Equipment and Laboratories," USEPA, EMSL/Cincin-
nati, OH 45268, EPA-600/4-80-025 (April 1980)
2 "Working with Carcinogens," DHEW, PHS, CDC,
NIOSH, Publication 77-206, (Aug 1977)
3 "OSHA Safety and Health Standards, General In-
dustry," OSHA 2206, 29 CFR 1910 (Jan 1976)
4 "Safety in Academic Chemistry Laboratories," ACS
Committee on Chemical Safety (1979)
5 "Inter-laboratory Validation of US Environmental
P'otection Agency Method 1625," USEPA, Effluent
Guidelines Division, Washington, DC 20460 (June
15, 1984)
6 "Handbook of Analytical Quality Control in Water
and Wastewater Laboratories," USEPA, EMSL/Cin-
cinnati, OH 45268, EPA-600/4-79-019 (March 1979)
7 "Standard Practice for Sampling Water," ASTM
Annual Book of Standards, ASTM, Philadelphia, PA,
76 (1980)
8 "Methods 330 4 and 330 5 for Total Residual
Chlorine," USEPA, EMSL/Cincinnati, OH 45268,
EPA 600/4-70-020 (March 1979)
9 Colby, B N, Beimer, R G , Rushneck, D R , and
Telliard, W A, "Isotope Dilution Gas Chromatog-
raphy-Mass Spectrometry for the Determination of
Priority Pollutants in Industrial Effluents," USEPA, Ef-
fluent Guidelines Division, Washington, DC 20460
(1980)
19
------- |