EPA 902-B-93-001
United States Environmental Protection Agency May 1993
Region II
RCRA Outreach Program
«^°sr^
TECHNICAL ASSISTANCE DOCUMENT
FOR COMPLYING WITH THE TC RULE
AND IMPLEMENTING THE TOXICITY
CHARACTERISTIC LEACHING
PROCEDURE (TCLP)
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TECHNICAL ASSISTANCE DOCUMENT FOR
COMPLYING WITH THE TC RULE AND
IMPLEMENTING THE TOXICITY
CHARACTERISTIC LEACHING PROCEDURE (TCLP)
The following individuals prepared Chapter 1
John Hansen
Hazardous Waste Compliance Branch
Air and Waste Management Division
USEPA Region II
26 Federal Plaza
New York, New York 10278
Claudette Reed
Hazardous Waste Compliance Branch
Air and Waste Management Division
USEPA Region II
26 Federal Plaza
New York, New York 10278
Michael Scudese
TRC Environmental Corporation
18 World's Fair Drive
Somerset, New Jersey 08873
Edited by: Frank Langone, IBM Corporation
The following individuals prepared Chapters 2 to 6:
Leon Lazarus Mitzi Miller
Monitoring Management Branch Environmental Quality Management
Environmental Services Division 10801 Fox Park
USEPA Region II Knoxville, Tennessee 37931
2890 Woodbridge Avenue
Edison, New Jersey 08837
Edited by: Frank Langone, IBM Corporation
May 1993
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References herein to any specific commercial product, process or service by
trade name, manufacturer, or otherwise does not imply its endorsement or
recommendation by EPA, TRC or EQM.
in
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IV
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Acknowledgements
The authors would like to thank the following individuals
for peer reviewing this document:
Kate Anderson, USEPA Office of Waste Programs Enforcement
Phil Flax, USEPA Region II
Oliver Fordham, USEPA Office of Solid Waste
Kathleen Grimes, NJDEPE Bureau of Environmental Measurements
and Quality Assurance
Dr. Larry Jackson, Environmental Quality Managment
Kevin Kubik, USEPA Region II
Davis Jones, USEPA Office of Waste Programs Enforcement
Rose Lew, USEPA Office of Waste Programs Enforcement
Ken Peist, USEPA Region II
Gale Sutton, Galson Laboratories
Rock Vitale, Environmental Standards
Appreciation is also expressed for techncial contributions from:
Jennifer Bramlett, SAIC Corporation
Melissa Girard, CDM Federal Programs Corporation
Dr. Mike Maskarinec, Oak Ridge National Laboratory
Carla Stout, TRC Environmental Corporation
Ted Varouxis, Associated Design and Manufacturing
the supplier of equipment and training tapes for the course
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VI
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Course Introduction and Goals
The goals of this course are to assist the regulated community in cost effective compliance
when utilizing the Toxicity Characteristic Leaching Procedure (TCLP) to demonstrate
compliance with the Toxicity Characteristic and Land Ban Regulations. The following
issues will be discussed:
What is TCLP?
• When must TCLP be performed?
• Which analyte lists should be used to demonstrate compliance with TC and Land
Ban regulations?
. How should a sampling strategy be developed?
• How much QA/QC and analytical deliverables are appropriate?
• How should one use the USEPA Region II TCLP data validation criteria?
• How should sampling plans be developed for multi-phase and oily materials?
VII
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VIII
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TABLE OF CONTENTS
Chapter Page
1.0 TECHNICAL ASSISTANCE DOCUMENT FOR COMPLYING WITH THE TC RULE 1-1
1.1 Preface 1-1
1.1 Introduction 1-2
1.2 RCRA OVERVIEW 1-3
1.2.1 Growth of Hazardous Waste in America: The Case of Love Canal .... 1-3
1.2.2 RCRA Cradle to Grave Concept 1-5
1.2.3 Definitions of Hazardous Waste 1-8
1.2.4 Making a Hazardous Waste Determination 1-10
1.3 THE TOXICITY CHARACTERISTIC RULE 1-11
1.3.1 EPToxTest 1-11
1.3.2 TCLPTest 1-12
1.3.3 TC Rule's Effect Upon Generators and TSDFs 1-15
1.4 TC RULE'S EFFECT ON INDIVIDUAL RCRA REGULATIONS 1-20
1.4.1 General . . . 1-20
1.4.2 Corrective Action and Closure 1-21
1.4.3 Land Disposal Restrictions (LDR) 1-22
1.4.4 Minimum Technology Requirements for Landfills and Surface
Impoundments 1-23
1.4.5 Exemption for Tanks (Minimum Technology Requirements) 1-24
1.4.6 Mixture Rule Exemption 1-25
1.4.7 Previously Delisted Wastes 1-26
1.4.8 Special Waste Exemptions 1-27
1.4.9 Hazardous Waste Listings 1-28
1.4.10 "Mixture" and "Derived From" Rules 1-29
1.4.11 Excluded Wastes 1-30
1.5 IMPACT OF TC RULE ON OTHER EPA PROGRAMS 1-31
1.5.1 Underground Storage Tanks (USTs) 1-31
1.5.2 Comprehensive Environmental Response and Liability Act (CERCLA) . 1-33
1.5.3 Clean Water Act (CWA) 1-34
1.5.4 Safe Drinking Water Act (SDWA) 1-36
1.5.5 Federal Insecticide, Fungicide, and Rodenticide Act (FIFRA) 1-39
1.5.6 Used Oil Recycling Act 1 -40
1.5.7 Toxic Substances Control Act (TSCA) 1-41
1.6 POLLUTION PREVENTION 1-42
1.7 CONCLUSIONS 1-45
IX
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TABLE OF CONTENTS (Continued)
Chapter Page
2.0 APPLICATIONS OF THE TCLP METHOD 2-1
2.1 What is TCLP? 2-2
2.2 When is the Use of TCLP Applicable? 2-3
2.3 Analytical Method Selection 2-9
3.0 TC AND TCLP PROJECT PLANNING 3-1
3.1 Data Quality Objectives 3-2
3.2 Case Study 3-10
3.3 Sampling and Analysis Design 3-19
4.0 OVERVIEW OF THE TCLP METHOD 4-1
4.1 Preliminary Sample Preparation for Leaching 4-2
4.2 Leaching Procedure for Nonvolatiles 4-5
4.3 Leaching Procedure for Volatiles 4-10
4.4 TCLP Method Quality Control 4-14
5.0 DATA VALIDATION AND DELIVERABLES 5-1
5.1 Data Validation 5-2
5.2 Data Deliverables 5-6
6.0 ANALYZING AND ASSESSING MULTI-PHASIC AND OILY WASTES 6-1
6.1 Definition of Oily Waste 6-2
6.2 Problems/Issues 6-3
6.3 Suggestions 6-5
6.4 Most Commonly Asked TCLP Question 6-7
6.5 Analytical Options 6-15
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TABLE OF CONTENTS (Continued)
TABLES
Table Page
1-1 TC Rule Constituents 1-13
1-2 TC Rule Reporting Requirements (Due Dates) 1-14
1-3 Permit Modifications 1-18
1-4 Compliance Scenarios 1-19
2-1 Toxicity Characteristic Constituents - Alphabetical 2-10
2-2 Metals Analysis Method By ICP 2-12
2-3 Metals Analysis Methods by GFAA and Mercury by CVAA 2-12
2-4 Pesticide and Herbicide Quantitation Limits by SW 846 and CLP 2-13
2-5 Quantitation Limits for Volatile TC Constituents 2-14
2-6 Quantitation Limits for Semivolatile TC Constituents 2-15
3-1 TCLP Holding Times 3-27
4-1 Volume of Extract Required for One Nonvolatile Analysis 4-7
XI
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TABLE OF CONTENTS (Continued)
FIGURES
Figure Page
3-1 Overview of the Data Quality Objectives Planning Process 3-6
3-2 Decision Performance Curve for Cadmium Fly-Ash Waste Example 3-19
4-1 TCLP Preliminary Determinations 4-4
4-2 Nonvolatile Extraction 4-6
4-3 Volitile by ZHE 4-11
4-4 Volitiles by ZHE Continued 4-12
4-5 Standard Addition Plot 4-16
XII
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TABLE OF CONTENTS (Continued)
APPENDICES
Appendix
I TCLP Methods From 40 CFR 261 Appendix II; SW 846 Method 1311 (Method
Without Typographical Errors); November 24, 1992 Update
II CCWE List from LDR Technology-Based Standards by RCRA Waste Code; CCW List
and August 18, 1992 Updates to Tables
III Associated Design and Larry Jackson's TCLP Bench Sheets and Calculations
IV USEPA Region II Organic, Inorganic and TCLP Data Validation Methods
V References for Multi-phasic and Oily Waste
VI Office of Solid Waste Management Methods Section Memoranda #35, #36
VII Recommendations and Rationale for Analysis of Contaminant Release by the
Environmental Engineering Committee, Science Advisory Board, October 1991
VIII USEPA Region II Special Analytical Services Request
IX Office of Solid Waste, Methods Section Required Uses of SW 846
XIII
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XIV
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List of Abbreviations and Acronyms
AC Alternating Current
ARARs Applicable or Relevant and Appropriate Requirements
ASTM American Society of Testing and Materials
BOAT Best Demonstrated Available Technology
BNA Base, Neutral and Acid Extractable Organics
CBEC Concentration Based Exemption Criteria
CCWE Constituent Concentrations in Waste Extracts
CERCLA Comprehensive Environmental Response Compensation and Liability Act of 1980
CESQG Conditionally Exempt Small Quantity Generator
CFR Code of Federal Regulations
CLP Contract Laboratory Program
COC Chain of Custody
CTRL Chronic Toxicity Reference Levels
CWA Clean Water Act
DAF Dilution Attenuation Factor
DC Direct Current
NPDES National Pollutant Discharge Elimination System
DQO Data Quality Objectives
DQOPP Data Quality Objectives Planning Process
ECHO Expanded Characteristics Option
EP Tox Extraction Procedure Toxicity
GFAA Graphite Furnace Atomic Absorption
HSWA Hazardous Solid Waste Amendments
HWN Hazardous Waste Numbers
P designates Acute Toxicity
U designates Toxic Waste
K designates Process Waste
F designates Generic Source Waste
D designates Characteristic Waste
ICP Inductively Coupled Plasma
LDR Land Disposal Restrictions
HAZWRAP Hazardous Waste Remedial Action Program
LOG Large Quantity Generator
MCLs Maximum Contaminant Levels
MS Matrix Spike
MSD Matrix Spike Duplicate
NIPDWS National Interim Primary Drinking Water Standards
POTWs Publically Owned Treatment Works
RCRA Resource Conservation and Recovery Act
RSD Risk Specific Doses
RfD Referenced Doses
SDWA Safe Drinking Water Act
SQG Small Quantity Generator
SW-846 Solid Waste Procedures
TC Toxicity Characteristic
TCLP Toxicity Characteristic Leaching Procedure
TSCA Toxic Substances Control Act
QA Quality Assurance
QC Quality Control
TSDF Treatment Storage and Disposal Facility
UST Underground Storage Tank
VOA Volatile Organic Analysis
ZHE Zero Headspace Extraction
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XVI
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TJ
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Chapter 1
TECHNICAL ASSISTANCE DOCUMENT FOR
COMPLYING WITH THE TC RULE
Introduction
RCRA Overview
The Toxicity Characteristic Rule
TC Rule's Effect on Individual RCRA Regulations
Impact on Other RCRA Programs
Pollution Prevention
Conclusions
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1.0 TECHNICAL ASSISTANCE DOCUMENT FOR COMPLYING WITH THE TC RULE
1.1 Preface
The purpose of this chapter is to provide an understanding of the Toxicity
Characteristic (TC) Rule, as it relates to hazardous waste management under
the Resource Conservation and Recovery Act (RCRA). The development of
hazardous waste issues in the United States is discussed first, giving the
example of Love Canal, which is a case study of an uncontrolled hazardous
waste site. Then an overview of RCRA is presented, with a comparison of the
Extraction Procedure Toxicity (EP Tox) Test and the TC Rule, including the
Toxicity Characteristic Leaching Procedure (TCLP) is presented. Finally, the
impact of the TC Rule on RCRA and non-RCRA regulations is discussed.
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1.2 Introduction
Hazardous waste growth in America.
RCRA system to control hazardous waste disposal.
Determination of hazardous waste by testing.
Changes to the testing procedure for hazardous waste. TC Rule replaces
the EP Tox Test.
Purpose of the manual.
In America, about 500,000 companies generate approximately 170,000 metric tons
of hazardous waste annually.
In 1976, the Resource Conservation and Recovery Act (RCRA) was passed to
properly manage of hazardous waste to protect human health and the environment.
One way a waste was defined to be hazardous or not was by a laboratory testing
procedure called the Extraction Procedure Toxicity (EP Tox) Test.
The Toxicity Characteristic Leaching Procedure (TCLP) recently replaced the EP Tox
test as the test used for identifying hazardous wastes.
The purpose of this manual to explain how the change from the EP Toxicity
Characteristic to the Toxicity Characteristic Rule affects generators of hazardous
waste.
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1.2 RCRA OVERVIEW
1.2.1 Growth of Hazardous Waste in America: The Case of Love Canal
. America in the 1890's.
• The invention of electricity.
• New chemicals.
• Clustering of industries around power sources.
• Building of Love Canal to connect the lower and upper parts of Niagara
Falls.
• DC power versus AC power.
America in the 1890's was undergoing industrialization. With the invention of
electric power, chemicals could be created which never existed before. A widely
used chemical process was the electrolysis of sodium chloride (salt) to yield sodium
hydroxide (lye) and chlorine, a byproduct. Lye was mixed with animal fat (tallow),
left over from animal slaughter houses, to produce modern soap (Ivory soap,
incidently, is still made this way. Chlorine, originally a useless byproduct,
eventually found various uses, including as a raw material in the production of
chlorinated solvents and pesticides. These chemicals had toxic effects which were
not well understood at the time.
The type of electricity used for this electrolysis process was direct current (DC). DC
power did not travel far over voltage lines, hence industries of the day had to
cluster around their DC power sources.
In Niagara Falls, a hydroelectric dam generated low cost electrical energy, which
industries used to produce various chemicals. Industries were clustered in the area
to obtain inexpensive DC power. Construction commenced on the Love Canal
industrial transportation network to connect the lower and upper parts of the
Niagara Falls area.
However, when alternating current (AC) electricity was invented, electricity
travelled much further over power lines. Thus, it was no longer necessary to
cluster industries around the Niagara Falls area. Therefore, the Love Canal project
was abandoned, and it was subsequently used by industry to dump their hazardous
waste. Love Canal continually leached toxic contaminants into the surrounding
groundwater and soil. Even after it was capped and closed, toxic chemicals
continued to leach out.
Most of the dumped hazardous chemicals were contained in the clay-lined Love
Canal until school and highway construction breached the walls, causing chemicals
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to contaminate local homes. The Love Canal area later became a residential area,
with a school built directly on the dump site. People living in the area started to
experience health problems, including miscarriages, stillbirths, and chromosome
damage.
In 1980, President Jimmy Carter ordered the evacuation of approximately 700
families out of the Love Canal area to protect their health.
The purpose of RCRA is to prevent this type of poor hazardous waste management.
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1.2.2 RCRA Cradle to Grave Concept
RCRA tracks hazardous waste from cradle to grave:
The manifest system.
Components:
generator/transporter/treatment storage and disposal facility
(TSDF).
Anyone generating hazardous waste must notify EPA:
generator definition.
RCRA is considered a "cradle to grave" system because it tracks hazardous waste
from creation to disposal. This ensures that waste is handled properly to avoid the
environmental contamination that occurred at sites such as Love Canal.
There are three handlers of hazardous waste: the generator, who creates the
hazardous waste; the transporter, who transports the hazardous waste to the
ultimate disposal site; and the disposal site called the TSDF or treatment, storage
and disposal facility. The final disposal may take place after interim
storage/treatment/recycling operations at various sites.
Facilities that generate solid wastes must determine if their solid waste is a
hazardous waste.
If the facility generates hazardous waste, the facility must notify EPA or the
authorized State agency, using the EPA Notification of Hazardous Waste Activities
form, and obtain an EPA facility identification number (EPA ID number).
The EPA or authorized State agency issues an EPA ID number to uniquely identify
each facility which handles hazardous waste.
The generator must manage the hazardous waste according to RCRA regulations.
The generator must dispose of the waste properly, and must complete a uniform
hazardous waste manifest detailing the contents of the waste.
The generator is responsible for using an authorized (permitted) transporter and
disposal facility, both of which must also have an EPA ID number.
The generator can usually store hazardous waste onsite for up to 90 days,
otherwise a storage permit is required (i.e., the facility must apply for a permit to
become a permitted TSDF).
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Generator responsibilities:
Determination of hazardous waste
Notify EPA
Obtain EPA ID number
Prepare manifest
Dispose of waste using an authorized transporter and an
authorized TSDF
Accumulation time
Annual reports
Contingency plans/Training requirements
Generator categories - CESQG/SQG/LQG
RCRA enforcement:
State versus Federal
The generator must file bi-annual reports detailing the amount of waste disposed of
during the year.
Generator categories
LOG - Large quantity generators (LOG) are generators which generate more
than 1000 kilograms (kg) of hazardous waste per calendar month or
> 1 kg acutely hazardous waste per calendar month. LQGs are fully
regulated and must comply with all generator requirements indicated
above.
SQG - Small quantity generators (SQG) are generators which:
Generate between 100 and 1,000 kg per month of hazardous
waste per calendar month.
Accumulate no more than 6,000 kg of hazardous waste on
site at any one time.
Accumulate hazardous waste on site for up to 180 days (or
270 days if the disposal site for the waste is over 200 miles
away).
Must provide notification of hazardous waste activities, use
manifests to dispose of hazardous waste, and dispose of
hazardous waste at TSDFs, but do not need to file an annual
report.
CESQG - Conditionally exempt small quantity generators (CESQG) are
generators which:
Generate less than 100 kg/month non-acute hazardous
waste per calendar month or;
Generate less than 1 kg/month acute hazardous waste
(P-waste code). There are also several acutely
hazardous F-listed wastes.
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May never accumulate more than 1000 kg of hazardous
waste or greater than 1 kg of acute hazardous waste at
any time. If they do, they will be regulated as a SQG.
They are subject to reduced requirements: they do not
need to notify EPA or State agencies, use manifests, or
dispose of their hazardous waste in a TSDF (they may
use a municipal or industrial landfill).
RCRA enforcement
EPA has delegated RCRA enforcement authority to many states. In those
states, the hazardous waste regulations may be more strict than RCRA, but
may not be less strict than EPA's regulations.
EPA, however, retains overall jurisdiction over state RCRA programs.
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1.2.3 Definitions of Hazardous Waste
. Only wastes classified as "solid wastes" may be characterized as
"hazardous wastes".
The definition of hazardous waste has four parts:
"Statutory definition"
"Listed waste" - Four lists: F, K, U, P
"Mixture rule" - Defines hazardous waste as being a mixture of a
hazardous waste and a non-hazardous waste.
"Characteristic waste"
Ignitable
Corrosive
Reactive
Toxic - (TC Rule)
Only wastes classified as "solid wastes" may be characterized as "hazardous
wastes." The definition of a solid waste is
"The term solid waste means any garbage, refuse, sludge, from a waste
treatment plant, water supply treatment plant, or air pollution control facility
and other discarded material, including solid, liquid, semisolid, or contained
gaseous material resulting from industrial, commercial, mining, and
agricultural operations, and from community activities, but does not include
solid or dissolved materials in irrigation return flows or industrial discharges
which are point sources subject to permits under Section 402 of the Federal
Water Pollution Control Act, as amended Statute 880, or source, special
nuclear, or byproduct material as defined by the Atomic Energy Act of 1954,
as amended (68 Statute 923).n1 (For additional information on this see 40
CFR 261.2 for the regulatory definitions.)
The definition of hazardous waste is
"The term "hazardous waste" means a solid waste, or combination of solid
wastes, which because of its quantity, concentration, or physical, chemical
or infectious characteristics may:
(A) cause, or significantly contribute to an increase in mortality or an
increase in serious irreversible, or incapacitating reversible, illness; or
(B) pose a substantial present or potential hazard to human health or the
environment when improperly treated, stored, transported, or
disposed of, or otherwise managed. "*
1 42 United States Code (USC) 6903, Section 1004(27)
2 - Ibid, (5)
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Regulatory Definition:
• Listed waste - Some wastes are considered hazardous. There are four lists of
hazardous waste: F, K, U, and P.
Four types of listed waste:
F Waste - List of waste from non-specific sources
K Waste - List of waste from specific sources
U Waste - List of discarded chemical products
P Waste - List of acutely toxic discarded chemical products
• Mixture rule - Any mixture of a listed hazardous waste and a non-hazardous waste
is considered hazardous.
• Derived from rule - see 261.3c
• Characteristic waste - There are four characteristics utilized to determine if a solid
waste is considered a hazardous waste.
• Characteristic of ignitability
A flashpoint of < 140°F.
For non-liquids - if the waste, when ignited, can burn spontaneously.
An ignitable compressed gas.
An oxidizer.
• Characteristic of corrosivity
The waste is aqueous and pH < = 2 or > = 12.5.
The waste corrodes steel at a rate of > = 6.35 millimeters/year.
• Characteristic of reactivity
The waste is unstable and undergoes violent reaction.
The waste reacts violently with water.
The waste, when heated, is explosive.
The waste, when mixed with water, releases toxic gases.
If the waste is a cyanide or a sulfide, and releases toxic gases when exposed
to pH conditions between 2 and 12.5.
The waste can explode if shocked or heated.
The waste is defined as an explosive by U.S. Department of Transportation
regulations.
Characteristic of toxicity
A waste exhibits the characteristic of toxicity if the concentration of one or
more of the 39 toxicity characteristic analytes in the TCLP aqueous extract
exceeds regulatory action levels. This is known as the TC Rule. This
replaces the EP Tox Test, which contained 8 inorganic and 6 organic
constituents.
Note: If wastes are listed solely because they exhibit a characteristic, and the
resulting mixture no longer exhibits a characteristic, the material is no longer a
hazardous waste.
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1.2.4 Making a Hazardous Waste Determination
Does the waste meet the definition of solid and hazardous waste?
Is the waste excluded?
Is the waste listed?
Does the waste exhibit a characteristic of hazardous waste?
Hazardous Waste Determination
• Is the waste a solid waste?
• If it meets the definition of solid waste, is the waste excluded from regulation?
• If the solid waste is not excluded from regulation as a solid waste, is it a listed
waste? If so, it is a hazardous waste.
• If neither excluded nor listed, does this solid waste exhibit any of the characteristics
of hazardous waste? If so, it is a hazardous waste.
Note: Solid waste is determined to be hazardous waste by:
The generator's reasonable knowledge of the characteristics of the waste, or
The generator's testing of the waste.
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1.3 THE TOXICITY CHARACTERISTIC RULE
1.3.1 EPToxTest
What is the Extraction Procedure Toxicity (EP Tox) Test?
What is the EP Tox Test based on?
Landfill leaching
14 metals and organics form the basis of the EP Tox Test
Contaminant levels of the EP Tox Test
Relationship to drinking water standards
Dilution attenuation factor (DAF)
EP Tox Test is the previous analytical method utilized to determine if a waste
exhibited the characteristic of toxicity by analyzing a waste extract for 14 specified
chemical constituents.
EP Tox Test is based on:
The assumption that chemicals placed into a landfill will leach at a certain
rate into the groundwater.
The 14 metals and organic chemicals regulated by the drinking water
program have EP Tox regulatory levels.
8 metals
4 insecticides
2 herbicides
Arsenic
Barium
Cadmium
Chromium
Lead
Mercury
Selenium
Silver
Endrin
Lindane
Methoxychlor 2
Toxaphene
2,4- D
2,4,5 - TP (silvex)
EP Tox regulatory action levels are based upon drinking water standards
(allowable drinking water level) X 100 = EP Tox regulatory level (assumes
that as toxic chemical leaches out of landfill, the chemical will be diluted by
a factor of 100;
The factor of 100 is termed a dilution attenuation factor (DAF).
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1.3.2 TCLPTest
Why replace the EP Tox Test with the TC Rule?
How is TC different than EP Tox?
How regulatory limits are determined for the TC Rule.
Regulatory level = CTRL X DAF
Improvements over the EP Tox.
The EP Tox Test was replaced by the TC Rule because of a Congressional mandate
to aggressively regulate additional toxic constituents.
The original EP Tox Test was not capable of leaching certain types of organic
compounds.
Changes:
14 original EP Tox chemicals adopted
25 additional organic chemicals added
The regulatory limit for the TCLP constituents was determined by multiplying the
Chronic Toxicity Reference Level (CTRL) times the Dilution Attenuation Factor
(DAF)
Regulatory level = CTRL X DAF
The CTRL is a level below which health effects constituent are not expected to
occur. The CTRL is based on: drinking water standards maximum contaminant
level (MCL); or for carcinogens, the risk specific dose (RSD); or for non-carcinogens
the reference dose (RFD).
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TABLE 1-1 - TC RULE CONSTITUENTS
EPA WASTE
NUMBER
D004
0005
0006
0007
0008
0009
0010
D011
D012
0013
0014
D015
0016
0017
HAZARDOUS
CONSTITUENT'
Arsenic
Barium
Cadmium
Chromium
Lead
Mercury
Selenium
Silver
Endrin
Lindane
Methoxychlor
Toxaphene
2.4-D
2,4.5-TP (Silvex)
Level
(mg/l)
6.0
100.0
1.0
5.0
5.0
0.2
1.0
5.0
0.02
0.4
10.0
0.5
10.0
1.0
EPA WASTE
NUMBER
D018
D019
D02O
D021
D022
0023
D024
0025
D026
D027
0028
D029
D030
HAZARDOUS
CONSTITUENT2
Benzene
Carbon tetrachloride
Ch lord one
Chlorobenzene
Chloroform
o-Cresol
m-Cresol
p-Cresol
Cresol
1 ,4-Dichlorobenzene
1.2-Dichloroethene
1 , 1 -Dichloroethvlene
2, 4-Dintro toluene
Level
(mg/l)
0.5
0.5
0.03
100.0
6.0
200.0
200.0
200.0
200.O
7.5
0.6
0.7
0.13
EPA WASTE
NUMBER
D031
D032
D033
D034
D035
D036
D037
D038
D039
D040
D041
D042
D043
HAZARDOUS
CONSTITUENT1
Heptachtor (&
epoxide)
Hexachlorobenzene
Hexacholoro-1,3-
butadiene
Hexachloroethane
Methyl ethyl ketone
Nitrobenzene
PentBcholorphenol
Pyridine
Tatrachloroethylene
Trichloroethano
2.3.6-Trichlorophenol
2,4.6-Trichlorophenol
Vinyl chloride
Level
(mg/l)
0.008
0.13
0.5
3.0
200.0
2.0
100.0
5.0
0.7
0.5
400.0
2.0
0.2
' Original EP Tox constituents.
' Chemical constituent added by TC Rule (shaded areas).
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TABLE 1-2 - TC RULE REPORTING REQUIREMENTS (DUE DATES)
Handler Category
Report Type
Deadline
Generators
3010
(Notification of hazardous
waste activity)
SQGs - November 2,
19901
LQGs - October 29,
19902
TSDFs
• New
Disposal Units
Storage Units
Interim Status
Permitted (with new
units)
Surface
Impoundments
Part A (Revised Permit
Application)
3010 (Notification of
Revised Permit)
Part B (Revised Permit
Application)
Certifications3
Part B (Revised Permit
Application)
Amended Part A
Class 1 - Permit Mods
Class 2 or 3 - Permit Mods
Certification* - Minimum
technology requirements
September 25, 1990
October 20, 1990
September 25, 1991
September 25, 1991
When Requested
September 25, 1990
September 25, 1990
March 24, 1991
March 29, 1994
SQGs began to comply with all applicable RCRA regulations for TC wastes on
March 29, 1991.
LQGs began to comply with all applicable RCRA regulations on September 25,
1990.
Ground water monitoring and financial assessments.
Retrofitting surface impoundments to meet minimum technology requirements and
assurance requirements.
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1.3.3 TC Rule's Effect Upon Generators and TSDFs
Generators
Notification
Manifests
Annual report
LDR
In addition to the above requirements, TSDFs must
Obtain a new permit
Modify an existing permit
Close prior to obtaining a permit
Close prior to the notification deadline
Obtain interim status
Make changes to interim status
Meet minimum technology requirements for pretreatment
Generators
Generators which generate hazardous waste not previously regulated must
submit notification, use manifests, etc. as required by their generator status
(CESQG/SQG/LQG - see Section 1.3.1 for generator responsibilities). If the
waste was previously regulated under EP Tox, no additional requirements are
necessary.
Options for TSDFs
Obtain new permit
Land disposal facilities newly regulated by the TC Rule will have to
meet minimum technology requirements when new units are added,
existing units are replaced, or existing units are laterally expanded.
New permit requirements found in 40 CFR 270.
Modify an existing permit
The three classes of permit modifications are based on the
significance of the modification. This three-tiered process, which
replaces the two-tiered major/minor process, is used by the permittee
to initiate a permit change. In contrast, EPA uses the old major/minor
process if it initiates a permit change.
Class 1 - modifications for routine changes;
Class 2 - modifications for changes of moderate complexity that
allow the facility to respond to changing conditions; and
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Class 3 - modifications for substantial facility alterations.
If waste at a permitted Subtitle C facility exhibits the TC for constituents
that were previously identified as EP toxic, the facility continues to comply
with its permit. No permit modification is needed.
Permitted Subtitle C facilities/units handling newly regulated TC wastes must
submit permit modifications to incorporate:
new TC Rule wastes
new regulated units managing TC Rule wastes
Because EPA implemented the TC Rule under HSWA, permit modifications
must be managed under new permit modification regulations (53 FR 37912,
September 28, 1988). See 40 CFR 270.42 for more information.
TSD Options
Close the facility prior to obtaining a permit.
Close prior to the notification deadline
Close the facility prior to the notification deadline for notifying EPA
that hazardous waste is generated at the facility.
Obtain interim status
Submit a Part A application permit as an interim permitted TSDF.
Make changes to interim status
Change the conditions of the Part A interim status permit application
to reflect the new hazardous waste.
EPA's new procedures for interim status are listed in
40 CFR 270.72 (a)(1)
No prior approval is required for adding newly regulated units to Part
A permit application, if:
Units were managing new wastes (e.g., TC wastes) on or
before effective date.
Amended Part A was submitted by effective date.
Prior to March 7, 1989, any new unit had to receive approval
from EPA.
These new units are not subject to the reconstruction limit,
which restricts cumulative interim status facility changes to no
more than 50% of the capital costs of a comparable new
facility.
Make changes to interim status - Facilities with Surface Impoundments
Implementation of the TC Rule may cause some facilities to alter their
management practices to avoid regulation of certain units under
Subtitle C of RCRA.
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EPA expects many facilities will convert their on-site surface
impoundments that treat TC Rule wastewaters to tanks to avoid
Subtitle C regulation (40 CFR 265.1{c)(9) & (10) or 40 CFR 264.1
(g)(5) & (6)).
The owner/operator of a newly regulated surface impoundment is
required to retrofit that impoundment no later than four years from
the promulgation of the additional listing or characteristic that made it
subject to regulation (1994 for TC Rule [HSWA 3005(j)(6)]).
The four-year retrofitting requirement applies only to those
impoundments that contain solely the new TC Rule wastes. Surface
impoundments that already contained regulated wastes were
previously subject to this requirement.
Retrofitting entails adding liners and leachate collection systems not
installed when the impoundment was constructed.
Surface impoundments with active hazardous waste management
may convert to non-hazardous waste management before September
25, 1990. They may be considered not subject to Subtitle C if they
do not manage hazardous waste on-site after that date.
Make changes to interim status - Land Disposal Units
New land disposal units should have submitted certification of
compliance with ground water monitoring and financial responsibility
requirements by September 25, 1991. Note that this is a new
requirement in §270.73(e) that was published March 7, 1989 (54 FR
9596).
Land Ban Requirements
Land disposal restrictions refer to restrictions on the land
disposal of hazardous wastes. Restricted wastes must be
treated as specified in the LDR regulations, otherwise they are
banned from disposal on land.
Any TC Rule wastes regulated by the LDR regulations would
be prohibited from land disposal.
Minimum Technology Requirements - Surface Impoundments
Surface impoundments which are newly regulated as a result of the
TC Rule will be required to meet minimum technology standards by
March 29, 1994.
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TABLE 1-3 - PERMIT MODIFICATIONS
Type of Unit
Involved
Permit Change Needed
Modification
Class
Tank or container
Surface
Impoundment,
Landfill, Waste
Pile, Land
Treatment
Incinerator
Addition of waste codes or units that will not
require additional or different management
practices than specified in the permit.
Addition of waste codes or units that will
require additional or different management
practices than specified in the permit.
Addition of waste codes or units that will not
require additional or different management
practices than specified in the permit.
Addition of waste codes or units that will
require additional or different management
practices than specified in the permit.
Addition of units.
If waste does not contain a principal organic
hazardous constituent (POHC) that is more
difficult to incinerate and no additional
performance standards are needed.
If waste contains POHC that is more difficult
to incinerate.
If different performance standards are
needed in the permit.
3
2
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TABLE 1-4 - COMPLIANCE SCENARIOS
FACILITY/
STATUS
TSDF
Interim Status
Permitted
Interim Status
Permitted
Interim Status
Permitted
Interim Status
Permitted
Operating on
9/25/90
Newly Permitted
GENERATOR
LOG
LOG
LOG
COMPLIANCE SCENARIOS
Constituent Status
Previously
EP Toxic
Y
Y
Y
Y
N
N
N
N
N
Y
Y
N
TC
Toxic
N
N
Y
Y
Y
Y
Y
Y
Y
N
Y
Y
Type of Unit
Regulated
N
N
Y
Y
Y
Y
N
N
NA
NA
NA
NA
Newly
Regulated
N
N
N
N
N
N
Y
Y
NA
NA
NA
NA
REQUIREMENTS
No notification requirements; change in
management status.
No notification requirements; no change in
management status.
Submit revised Part A permit application
with new waste codes by 9/25/90.
Submit Class 1 permit modification by
9/25/90.
Submit revised Part A permit application to
identify new waste codes by 9/25/90;
comply with interim status regulations.
Submit Class 1 permit modification by
9/25/90; continue to comply with permit
requirements.
Submit revised Part A permit application by
9/25/90; comply with interim status
regulations and ground water monitoring and
financial requirements by 9/25/90; retrofit
surface impoundments to meet minimum
technology requirements.
Submit Class 1 permit modification by
9/25/90; comply with interim status
requirements; retrofit surface
impoundments.
Submit 3010 notification of hazardous
waste activity by 1 0/29/90; submit Part B
permit application for all land disposal units
by 9/25/90; comply with ground water
monitoring and financial certification
requirements; retrofit surface
impoundments.
No notification required. Waste no longer
hazardous.
No notification required; change waste code
assigned to the waste.
Submit a 3010 notification of hazardous
waste activity by 10/9/90 (1 1/2/90 for
SQGs); comply with generator requirements
by 9/25/90 (3/29/91 for SQGs).
Key: Y = Yes
N = No
NA = Not Applicable
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1.4 TC RULE'S EFFECT ON INDIVIDUAL RCRA REGULATIONS
1.4.1 General
The TC Rule has potential impact on other parts of the RCRA program.
Regulations not impacted
Regulations which are impacted
The implementation of the TC Rule affects some RCRA regulations because it
expands the types of solid waste classified as hazardous waste. The expanded
definition will cause waste not previously considered to be hazardous considered
hazardous. The following RCRA regulations are affected by the TC Rule (they will
be explained more fully in the following sections):
Corrective action and closure
Land disposal restriction (LDR) regulations
Minimum technology requirements for surface impoundments and landfills
Mixture rule exemptions
Previously delisted wastes
Special waste exclusions
The TC Rule will not affect wastes already considered hazardous. The following
RCRA regulations are not affected by the TC Rule:
The hazardous waste lists (i.e., the F, K, P, and U lists)
Wastes that are hazardous by the "Mixture" and "Derived From" rules (i.e.,
these wastes are still considered hazardous wastes)
Wastes already excluded from regulation (they are still excluded from
regulation)
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1.4.2 Corrective Action and Closure
TC increased the universe of regulated facilities.
Number of Subtitle C permitted and interim status facilities subject to
corrective action increased.
Number of regulated units within permitted or interim status
facilities undergoing closure increased.
Excavated material from corrective action and closure that exhibits the
TC must be managed as hazardous waste.
TC levels are not used to set clean-up levels for corrective actions or
clean closures.
The TC Rule added more wastes of concern and brought more facilities under the
RCRA program as hazardous waste management facilities. Therefore, additional
facilities are newly subject to the Subtitle C corrective action and closure
requirements.
Previously unregulated TSDFs managing TC Rule wastes are subject to
RCRA requirements if they did not close or change management practices
(e.g. exempt tanks) before the TC Rule became effective.
Existing RCRA facilities may have to amend their closure plans to reflect
newly regulated units as the TC Rule expands the number of regulated units.
Excavated materials, which did not previously exhibit the toxicity characteristic,
may now have to be managed as hazardous waste.
The Subtitle C corrective action program addresses remediation hazardous waste
releases from facilities subject to RCRA permitting. The TC Rule levels are neither
action levels nor cleanup standards, both of which are developed from site-specific
information gathered during the investigatory and evaluation phases of the process.
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1.4.3 Land Disposal Restrictions (LDR)
• LDR standards will continue to affect the 14 wastes previously
regulated under the EP Tox Test.
• No LDR standards are currently promulgated for the 25 new TC
constituents.
• LDR treatment standards are based on the best demonstrated available
technology (BOAT) standards. The characteristic (regulatory) levels
were developed using a risk-based approach.
• For some constituents, LDR treatment standards are set at the
regulatory level.
HSWA requires EPA to make an LDR determination for all newly listed wastes
within six months of publication in the Federal Register, or by the effective date of
the TC Rule ruling. Newly listed or identified wastes were not automatically
prohibited from land disposal under LDRs if EPA failed to make this determination
within six months (i.e., no "hammer11 provisions).
EPA set LDR standards for the 14 original EP characteristic constituents,
which EPA does not consider newly identified. These 14 constituents had to
meet LDR treatment standards before land disposal on the effective date of
the TC Rule.
The 25 new organics identified by the TC Rule are considered newly
identified, and as such have not yet been affected by LDR regulations.
EPA is reviewing the treatability of each TC Rule constituent independently to
determine LDR treatment standards for TC Rule wastes. These standards may
differ from standards set for spent solvent wastes (F001-F005) based on
differences in treatability.
LDR treatment standards are based entirely on technology-based standards
expressed as BOAT. While TC Rule levels are based upon health-based allowable
concentration levels and dilution/attenuation factors, they are not the same as LDR
treatment standards. However, for many TC wastes, EPA has set the LDR
treatment standards at the regulatory level.
This issue is being litigated. Therefore, the LDR treatment standards for TC Rule
wastes may change.
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1.4.4 Minimum Technology Requirements for Landfills and Surface Impoundments
Landfills and surface impoundments newly regulated under RCRA
because of the TC need to comply with minimum technology
requirements
HSWA requires that:
Interim status waste piles, landfills, and surface impoundments
meet certain minimum technology requirements
Surface impoundments be retrofitted to meet minimum
technology requirements
Existing land disposal units (except surface impoundments) that already contained
TC Rule wastes will not require retrofitting unless they are expanding or are
replacing units or continuing to place TC Rule wastes in these units after the TC
Rule effective date.
The minimum technology requirements (liners and leachate collection systems) for
interim status surface impoundments are found in 40 CFR 265.221.
Surface impoundments that become regulated under Subtitle C because of the TC
Rule must meet the minimum technology requirements by March 29, 1994. This
extension applies to those impoundments that contain the newly identified or
characteristic wastes.
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1.4.5 Exemption for Tanks (Minimum Technology Requirements)
TC wastes treated in wastewater treatment tanks are exempt from
hazardous waste management standards under 40 CFR 264. Kg) and
265.1(c).
Generators that manage TC waste waters in on-site surface
impoundments may switch to exempt tanks in order to avoid Subtitle C
requirements.
However, generators and handlers should have converted their surface
impoundments to tanks prior to effective date of the final rule to
maintain the exemption.
Facilities managing TC wastes after the effective date, even
unintentionally, are subject to interim status requirements.
40 CFR 264.Kg) and 265.1{c) exempt wastewater treatment units containing
hazardous waste from Subtitle C regulation.
Generators that continue managing wastewaters in an on-site surface impoundment
or non-wastewaters on-site, will require either interim status (and eventually a
RCRA permit) or a RCRA permit modification/change during interim status,
depending on whether or not the facility is currently a Subtitle C TSDF.
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1.4.6 Mixture Rule Exemption
The mixture rule exemption was not modified by the TC rule; mixtures
of wastewaters and certain listed spent solvents are exempt from
Subtitle C regulations unless the wastewaters:
Exhibit hazardous waste characteristic; or
Contain listed hazardous wastes not specified in the exemption.
TC Rule may regulate currently exempted wastewaters under Subtitle C.
The mixture rule under 40 CFR 261.3(a)(2)(iv) provides an exemption from RCRA
Subtitle C requirements for mixtures of wastewaters and certain listed spent
solvents in low concentrations.
The mixture rule exemption only addresses hazardous waste listings. Therefore, the
mixture rule exemption does not affect the TC Rule.
The mixture rule exemption ensures that mixtures of wastewaters and certain listed
spent solvents will not be considered hazardous unless they exhibit a characteristic
of hazardous waste.
EPA proposed modifying the mixture rule exemption to make it more consistent
with current risk information.
The TC Rule regulatory levels are based on state-of-the-art toxicological data and
risk assessment methodologies. In contrast, the mixture rule exemption levels are
based upon less current risk information.
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1.4.7 Previously Delisted Wastes
A waste previously "excluded" under Subtitle C regulation may no
longer be delisted if it exhibits a hazardous characteristic (e.g., the
characteristic of toxicity).
TC rule applies to already delisted wastes that now exhibit TC
characteristics.
These wastes are no longer considered "not hazardous"
These wastes must now be managed under Subtitle C
Because delisting levels are generally more stringent than the final TC
levels, the impact of TC rule on previously delisted wastes is expected
to be minimal.
Wastes "excluded" from Subtitle C regulation under the delisting program may
nevertheless be hazardous if they exhibit a hazardous characteristic (see 40 CFR
260.22). Hazardous waste characteristic levels are those above which a waste is
hazardous due to a particular property; delisting levels are those below which a
waste is not hazardous for any reason. Thus, it is reasonable that these two levels
do not coincide.
Although the TC Rule applies to delisted wastes, EPA does not, in general, expect
that such wastes will become hazardous because of application of the revised TC
Rule. However, if a previously delisted waste exhibits the TC Rule, it will again be
subject to Subtitle C requirements, and the facility will have to notify EPA of its
activity.
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1.4.8 Special Waste Exemptions
RCRA defines four special waste categories exempted from Subtitle C
regulation:
Mining wastes
Mineral processing wastes
Oil and gas wastes
Domestic sewage
Subtitle C regulations may apply to these special wastes on a case-by-
case basis.
Special waste exclusions are being reevaluated as mandated by
Congress.
• If EPA makes a determination that any special wastes should be regulated under
RCRA Subtitle C, the Agency will make a separate determination concerning the
applicability of the TC Rule to such wastes.
• After completing the studies required by RCRA Section 8002, EPA may determine
that one or more special wastes should be regulated under RCRA Subtitle C. Such
wastes would then be listed or the generators required to determine whether the
wastes exhibit a hazardous characteristic, including those specified in the TC Rule.
Other Special Waste Exemptions
• The TC Rule will have no direct effect on the following types of wastes:
Hazardous waste listings
Wastes classified as hazardous by the "mixture" and "derived from" rules
Wastes already excluded from regulation under 40 CFR 261.4
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1.4.9 Hazardous Waste Listings
TC rule has no effect on listings of hazardous waste
Waste already listed as hazardous are always considered
hazardous, unless they are delisted.
Hazardous waste listings will continue to complement the revised TC Rule, as they
did the EP Tox Test. The TC Rule revisions do not justify elimination of any
hazardous waste listings.
Listed wastes continue to be hazardous even if they contain TC Rule constituents in
concentrations below the regulatory levels.
TC Rule regulatory levels are not designed to identify the full range of wastes that
may be toxic to human beings. Instead, the characteristic levels were established
to protect human health.
Listed wastes that do not exhibit the toxicity characteristic may nevertheless be
hazardous because:
They contain listed hazardous waste constituents; or
They contain hazardous constituents that are not covered by the TC Rule.
Listed wastes frequently contain hazardous constituents other than the ones cited
in Appendix VII of 40 CFR Part 261. These additional hazardous constituents
present in a waste may not be TC Rule constituents. Removing wastes from a
hazardous waste listing without evaluating additional constituents would be
inconsistent with the intent of RCRA §3001 (f).
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1.4.10 "Mixture" and "Derived From" Rules
TC has no effect on the regulatory status of waste "mixtures" or
"derived from" wastes:
Mixtures of listed wastes and solid wastes, and residues derived
from listed wastes, are still hazardous until delisted.
TC alone is not adequate to regulate mixtures and treatment residues.
Problems may result by applying "mixture" and "derived from" rules.
The "mixture" rule (40 CFR 261.2(a)(2)(iv)) states that any mixture of a listed
hazardous waste and a solid waste is a RCRA hazardous waste.
The "derived from" rule (40 CFR 261.3(c)) states that any waste derived from the
treatment, storage, or disposal of a listed hazardous waste is hazardous.
The "mixture" and "derived from" rules may create inequities in the treatment of
certain dilute wastes. For example, very low constituent concentrations in listed
wastes may still be considered hazardous even after treatment.
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1.4.11 Excluded Wastes
TC Rule does not apply to wastes that are already excluded from
Subtitle C regulations under 40 CFR 261.4:
For example, household hazardous waste is excluded from
Subtitle C; it remains excluded after the TC effective date.
TC Rule does not add any exclusions to the applicability of previously
promulgated hazardous waste characteristics.
Wastes described in 40 CFR 261.4(b) that are already excluded from Subtitle C
regulations will continue to be exempt from regulation as hazardous wastes, even if
they exhibit the TC Rule.
EPA does not at this time intend to expand the list of exemptions under 40 CFR
261.4(b) to include creosote- and pentachlorophenol-treated wood.
Other wastes that are excluded from Subtitle C in 40 CFR 261.4(b) include:
Household hazardous wastes
Certain mining wastes
Certain solid wastes generated from farming or raising animals
Certain wastes generated from the combustion of coal or other fossil fuels
Wastes associated with the production of crude oil and natural gas
Some chromium containing wastes
Solid waste from extraction and processing of ores and minerals
Cement kiln dust wastes
Certain wood products
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1.5 IMPACT OF TC RULE ON OTHER EPA PROGRAMS
1.5.1 Underground Storage Tanks (USTs)
Two programs currently regulate underground storage tanks (USTs).
Subtitle C (tanks containing hazardous wastes) or Subtitle D
(tanks containing non-hazardous solid wastes),
Subtitle I (tanks containing petroleum product or hazardous
substance products).
The TC Rule may increase the number of tanks regulated under Subtitle
C.
Product (petroleum, hazardous substance) that leaks may become a
hazardous waste and may also exhibit TC.
Petroleum contains several TC constituents. Therefore, it is likely that some
petroleum-contaminated media will exhibit the Toxicity Characteristic.
The management of any petroleum-contaminated media exhibiting Toxicity
Characteristic would normally be subject to Subtitle C requirements for hazardous
waste management. However, EPA believes further study of these impacts is
necessary before imposing TC requirements on media and debris contaminated
solely by petroleum from USTs.
EPA has insufficient information on the impact of the TC Rule on UST cleanups;
therefore, EPA has deferred a final decision on the application of the TC Rule to
media and debris contaminated with petroleum from USTs exhibiting the D018-
D043 waste characteristics that are subject to the 40 CFR Part 280 requirements.
EPA believes deferral of a final decision concerning the application of the TC Rule to
UST cleanups is necessary. Imposition of the Subtitle C requirements is likely to
significantly delay cleanups and severely discourage the self-monitoring and
voluntary reporting essential to implementing the UST program.
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Subtitle I and Subtitle C potentially overlap if a substance exhibits the
TC characteristic and the origin of substance is not known.
The contents of a tank determines which regulatory program (i.e..
Subtitle C or Subtitle I) applies:
Subtitle C regulates hazardous wastes;
Subtitle I regulates hazardous products and petroleum.
Hazardous product that leaks may become hazardous waste.
Petroleum and hazardous product may exhibit the TC but may not be regulated
under Subtitle C.
Corrective action under Subtitle I addresses releases of product.
Old releases of product not subject to Subtitle I may have occurred:
Via inactive tanks;
In areas considered as RCRA solid waste management units.
If wastes exhibit the TC for D004-D017, RCRA standards may apply to these old
releases.
TC Rule excludes D018-D043 wastes from RCRA regulation if they are covered
under Subtitle I Corrective Action:
Petroleum-contaminated soil and ground water; and
Petroleum-contaminated debris (tanks).
EPA is studying impacts of Subtitle C regulation on petroleum-contaminated areas.
Note: Petroleum contaminated media from aboveground storage tanks are also
excluded from TCLP testing requirements where a state has an adequate treatment
mechanism in place.
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1.5.2 Comprehensive Environmental Response and Liability Act (CERCLA)
CERCLA response actions must comply with all applicable, or relevant
and appropriate requirements (ARARs), including RCRA regulations.
TC will cause more Superfund wastes to be classified as RCRA
hazardous wastes.
Thus, more Superfund cleanups will be subject to RCRA
regulations.
TC will not, however, affect CERCLA clean-up levels.
Comprehensive Environmental Response, Compensation, and Liability Act (CERCLA
or Superfund) addresses remediation of inactive waste sites.
ARARs are "applicable or relevant and appropriate requirements." CERCLA must
meet other Federal or State environmental requirements whenever they are
applicable or relevant and appropriate to CERCLA actions.
The primary effect of TC Rule on Superfund will be to regulate many organic
constituents found at Superfund sites as RCRA hazardous wastes.
A current problem at many Superfund sites is determining if an organic
constituent is from a listed RCRA hazardous waste.
There is often little evidence about the source of contamination that exists at
Superfund sites to prove a waste is a listed waste. Therefore, a waste may
not be managed under RCRA (but it will be handled in a protective manner
according to risk assessment).
Under the TC regulation, if tetrachloroethylene is found above the TC
regulatory level, the waste is hazardous regardless of its origin.
As in RCRA corrective actions, Superfund response personnel will not use the TC to
determine whether to undertake a clean-up action. The TC will affect decisions
concerning the management of wastes generated during cleanup activities (i.e.,
hazardous wastes generated during cleanup must be managed in accordance with
Subtitle C).
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1.5.3 Clean Water Act (CWA)
The CWA regulates discharges of pollutants to surface waters and to
publicly owned treatment works (POTWs).
Regulatory levels of TC are consistent with those of the CWA:
NPDES effluent guidelines; and
Pretreatment standards.
Treated wastewaters that exhibit the TC Rule.
Clean Water Act regulates discharges of hazardous substances to surface waters
(through the National Pollutant Discharge Elimination System (NPDES) permit
program), and pretreatment standards for POTWs.
EPA believes TC levels and CWA standards are consistent.
Thus, CWA discharges are exempt from RCRA regulation under 40 CFR Part 261.
Treated wastewaters exhibiting TC are regulated under RCRA unless:
discharged under NPDES unit
treated in POTW
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Objectives of the Clean Water Act
Impact of the Clean Water Act
^•^^••••1
Objectives of the CWA are:
to restore and maintain the chemical, physical, and biological integrity of the
nation's waters;
to eliminate the discharge of pollutants into surface waters;
to attain water quality that provides for the protection and propagation of
fish, shellfish, and wildlife, and provides for recreation in and on the water.
Impact of the Clean Water Act:
In lieu of retrofitting and obtaining permits for existing surface
impoundments to meet RCRA requirements, hazardous waste management
facilities may utilize tank treatment and storage of hazardous wastewater,
which is exempt from RCRA permitting requirements.
Wastewater treatment facilities using surface impoundments to treat TC
waste may be subject to RCRA regulations.
The Agency expects many owner/operators to replace surface
impoundments with wastewater treatment tanks.
Wastewater treatment tanks are exempt from Subtitle C regulation
under 40 CFR 264.1(g)(6) and 265.1(c).
If a POTW sludge (from wastewater treatment) exhibits TC, however, the
owner/operator must treat the sludge to remove the characteristic.
Treatment may be through a pre-treatment program (i.e., before
POTW receives discharge); or
After sludge is produced.
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1.5.4 Safe Drinking Water Act (SDWA)
Safe Drinking Water Act (SDWA) establishes maximum levels of
contaminants acceptable in public drinking water supplies.
Maximum Contaminant Levels (MCLs)
Maximum Contaminant Level Goals (MCLGs)
TC fate and transport models assume ingesting contaminated drinking
water, and uses MCLs as the basis for setting regulatory levels for many
TC constituents.
SDWA mandates regulations to protect human health from contaminants in drinking
water.
The specific objectives are:
to assure that all people served by public water systems be provided with a
high quality water;
to remove contaminants found in water supplies to protect human health;
and
to establish programs to protect underground sources of drinking water from
contamination.
SDWA primary drinking water regulations include MCLs for specific contaminants.
Many TC levels are based on SDWA MCLs.
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Underground injection control (UIC) program regulates injection of fluids
to protect underground sources of drinking water (USDWs).
Five classes of wells are regulated under the UIC program:
Class I - municipal or industrial waste discharged beneath
USDWs
Class II - oil and gas production
Class III - mineral recovery
Class IV - hazardous or radioactive waste into or above
USDWs
Class V - all other wells used for injection of fluids,
including septic tanks and sumps.
Class I wells are often used by generators of hazardous waste or owner/operators
of hazardous waste management facilities to inject hazardous waste below USDWs.
The largest user of hazardous waste Class I wells is the chemical industry. Class I
is the smallest class of wells with 554 reported in 1989.
Class IV wells are banned with the exception of wells used for remediation of
aquifers contaminated with hazardous wastes (40 CFR 144.13).
The largest group of injection wells is Class V, with approximately 180,000 wells.
The second largest group of wells is the Class II group which contains
approximately 150,000 wells, followed by Class III wells with 20,000 wells.
The Agency is enforcing the ban on shallow injection of hazardous wastes. The
Agency is also developing guidance on best management practices to reduce the
amount and toxicity of wastes injected into Class V wells (40 CFR 144.24).
The TC Rule may increase the number of Class I wells accepting TC waste, and
bring newly identified hazardous Class I wells into the Subtitle C program.
Some Class V wells may be illegally accepting hazardous wastes; the number may
increase as a result of the TC Rule.
Class V wells that may receive TC wastes:
Agricultural drainage wells;
Industrial drainage wells;
Experimental technology wells;
Industrial process water and waste disposal wells;
Automobile service station wells; and
Aquifer remediation-related wells.
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Wastes injected into some Class V wells are exempted from regulation as a
hazardous waste. For example: geothermal electric and direct heat re-injection
wells, several of the domestic wastewater disposal wells, most of the mineral and
fossil fuel recovery-related wells, and certain experimental technology wells.
Many of the facilities that operate Class V wells (e.g., auto service stations) also
generate listed hazardous waste, such as solvents. It is possible that some
facilities are not managing their listed wastes properly, and that hazardous wastes
are entering Class V wells. Of course, when hazardous wastes are injected into
Class V wells, they become Class IV wells.
It is unclear at this time what effects TC will have on UIC program because the
Class V program is very new.
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1.5.5 Federal Insecticide, Fungicide, and Rodenticide Act (FIFRA)
FIFRA regulates the sale, distribution, and use of all pesticide products.
RCRA regulates listed wastes, including pesticide product wastes.
TC Rule:
adds one pesticide to the list of TC constituents; and
regulates more "multiple active ingredient" formulations.
Other TC constituents may be ingredients in pesticides.
If pesticide wastes exhibit TC, they are subject to Subtitle C regulation
unless they are exempt.
Current RCRA exemptions limit the extent pesticide users are subject to RCRA:
Household waste (e.g., household pesticide wastes) exemption.
Farmers exemption (i.e., farmers who triple rinse their containers and
dispose of the containers on their own farm in accordance with 40 CFR
262.51 and the pesticide manufacturer's label instruction on disposal are
exempted).
Small quantity generators follow reduced requirements. Many pesticide
users are small quantity generators.
Properly emptied containers may be exempted from further RCRA
requirements under 40 CFR 261.7. Many pesticide containers, therefore,
may not be subject to regulation as hazardous waste.
No change in listed pesticide wastes that are either pure, technical grade, or sole
active ingredient product wastes; they will continue to be regulated under Subtitle
C (P and U listings).
The exemption for arsenic-treated wood was not expanded in the TC Rule.
This exemption may be reevaluated in the future.
Multiple active ingredient products are usually not regulated as RCRA Subtitle C
wastes, but are instead regulated under RCRA Subtitle D or FIFRA.
TC increases the potential for multiple active ingredient product wastes to be
hazardous.
The principal effects of adding new pesticide constituents to the TC Rule will be felt
by commercial applicators, such as aerial applicators and pest control operators. If
they use large quantities of multiple active ingredient pesticide products that have
not previously been regulated, such applicators may be newly subject to RCRA
Subtitle C requirements.
Wastes from multiple active ingredient products that do not exhibit a characteristic
will still be regulated under applicable FIFRA and RCRA Subtitle D requirements.
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1.5.6 Used Oil Recycling Act
• Some used oil exhibits TC or ignitability characteristic.
• TC will affect used oil that is
used for road oiling;
that is dumped;
disposed in solid waste landfills and incinerators.
• TC will not affect used oil that is:
Managed by do-it-yourselfers (exempt as household hazardous
waste);
Recycled through energy recovery (40 CFR Part 279 regulates
this activity);
Recycled in any other manner (regulated under 40 CFR 279).
Used oil may exhibit the TC or ignitability characteristics.
Used oil exhibiting the TC characteristic that is disposed of is subject to full RCRA
Subtitle C regulation (40 CFR 279.80).
However, oil that is burned for energy recovery is not regulated as a hazardous
waste.
Used oil generated by household do-it-yourselfers is exempt form RCRA
under 40 CFR 279.20(a)(1).
Used oil that exhibits one or more of the characteristics of hazardous wastes
but is recycled in some other manner than being burned for energy recovery
is exempt under 261.6(a)(43).
Significant quantities of used oil may exhibit EP toxicity for metals, but little used
oil is currently recognized as EP toxic.
Shifts in used oil management practices may result from the TC Rule. Management
practices may shift away from road oiling, dumping, and disposal in solid waste
facilities to burning as fuel, recycling, and disposal in Subtitle C facilities.
Standards for regulating used oil that is recycled were promulgated in the Federal
Register on September 10, 1992 (FR 41566).
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1.5.7 Toxic Substances Control Act (TSCA)
TSCA addresses manufacturing, processing, and distributing hazardous
substances such as PCBs.
If TSCA-regulated products become wastes and contain D004-D017,
they become RCRA regulated.
If Polychlorinated Biphenyls (PCBs) are fully regulated under TSCA, TC
rule exempts those PCB-wastes containing D018-D043 from RCRA
regulations; not all PCB wastes are fully regulated under TSCA (D004-
D017).
Exempt wastes include PCB-containing dielectric fluids removed from:
Electrical transformers; and
Capacitors.
Toxic Substances Control Act (TSCA) regulates toxic substances and specifically
addresses PCB management and disposal.
Dielectric fluids from electrical transformers, capacitors and associated PCB-
contaminated electrical equipment could exhibit the TC because they may contain
chlorinated benzenes.
These wastes exhibiting TC characteristics are exempted from Subtitle C
management standards if they exhibit waste codes D018-D043.
The exemption applies only to certain wastes noted above that are fully
regulated under TSCA, not to all PCB wastes.
PCB wastes exhibiting D004-D017 characteristics (i.e., those hazardous under EP
toxicity) remain regulated under RCRA if they are a D004-D017 waste under TC
(i.e., contain other constituents).
1-41
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1.6 POLLUTION PREVENTION
Defining pollution prevention.
Pollution prevention as a national priority for managing hazardous waste.
Priorities of pollution prevention:
Source Reduction;
Source Reduction exclusions.
Implementation.
The Pollution Prevention Act of 1990 encourages waste reduction at the source
rather than the management of waste already produced.
An integral component of EPA's RCRA program is pollution prevention through
waste minimization.
Therefore, EPA's priority is hazardous waste source reduction rather than "end-of-
pipe" controls.
EPA has produced industry-specific outreach materials to assist industry in their
waste minimization efforts (source reduction, process modifications, recycling, and
the use of less toxic materials).
There are significant benefits to industry from pollution prevention:
can reduce the costs of raw materials, and hazardous waste treatment and
disposal;
can minimize regulatory burdens of compliance;
can minimize liability for environmental problems and occupational safety
problems;
can improve public image in community and among employees; and
may enhance efficiency and product quality.
EPA encourages industries affected by this ruling to consider achieving compliance
through pollution prevention.
Steps taken by EPA to create Pollution Prevention incentives:
incorporate its philosophy into internal EPA planning and decision-making;
makes technical information available to firms.
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Source reduction is:
(i) a practice that reduces the amount of any hazardous waste entering a waste
stream or the environment that occurs prior to recycling, treatment, or disposal;
(ii) a practice that reduces hazards to public health and the environment due to
release of hazardous substances, pollutants, or contaminants.
Source reduction includes:
equipment/technology modifications;
process/procedure modifications;
reformulations/redesign of products;
substitution of raw materials;
improvements in housekeeping, maintenance, training.
Source Reduction Exclusions include:
"Source reduction" does not include practices that alter the physical,
chemical, biological characteristics or volume of a hazardous substance,
pollutant, or contaminant through process or activity that, itself, is not
integral to and necessary for the production of the product or service.
EPA is implementing the strategy by:
creating incentives for industry;
building pollution prevention into their decision-making processes;
making technical information available to help firms reduce waste generation
through the use of:
The Pollution Prevention Information Clearinghouse (PPIC), a
nationwide network of people and resources with direct experience in
waste reduction strategies in many industries (202-260-1023);
The Pollution Prevention Information Exchange System (PPIES), a
computer electronic bulletin board (703-506-1025) which contains a
database of bulletins, programs, contacts, and reports related to
pollution prevention.
supporting the development of state programs to assist generators in their
waste reduction efforts;
initiating specific new regulatory requirements for generators to:
certify on their hazardous waste manifests and annual permit reports
that they have in place a program to reduce the volume or toxicity of
their hazardous wastes as much as possible;
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describe on their RCRA biennial reports the efforts undertaken during
the year to reduce the volume and toxicity of their hazardous waste
and compare the efforts to those in previous years;
to require waste minimization/pollution prevention in RCRA permits
for TSDFs that generate hazardous waste.
communicating the strategy by targeting, specifically, small businesses, and
industry in general.
EPA recommendations for owners/operators implementing waste minimization
programs at the plant level:
conduct a waste minimization assessment by selecting a few processes or
waste streams for source reduction or recycling and keeping accurate
records on the rate of generation and the cost of management;
identify waste minimization techniques;
inventory management (substitute less toxic source materials);
modification of equipment (upgrading the performance of process
equipment, reducing leaks and malfunctions, installing conditioning or
recovery systems);
production process changes; and
recycling and reuse.
Contact the Pollution Prevention Office, U.S. EPA, 401 M Street, SW, Washington,
D.C. 20460 to obtain information or to offer suggestions on how the Agency
might facilitate waste reduction efforts.
Role of the TC Rule in the Pollution Prevention strategy:
By subjecting a larger number of toxic compounds to the RCRA regulations,
it increases the costs to generators of managing solid wastes.
In effect, the TC forces waste managers to rethink their solid waste
management practices due to the high cost of compliance with RCRA
Subtitle C requirements.
The TC will alter the past management of wastes that might leach toxic
contaminants by restricting their management in land-based units (surface
impoundments, waste piles, lagoons, etc.).
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1.7 CONCLUSIONS
The TC Rule expands the definition of hazardous waste.
The TC Rule adds 25 additional organic analytes.
The TC Rule should encourage facilities to utilize less hazardous
chemicals, to avoid the increased disposal costs associated with the TC
Rule.
By expanding the number of toxicity characteristic constituents from 14 to 39, EPA
has expanded the definition of hazardous waste, and brought more wastes under
the RCRA jurisdiction. This will have the overall effect of keeping wastes within
the RCRA "cradle to grave" system and preventing them from harming human
health or the environment by being placed in municipal landfills which are not
designed to handle hazardous wastes.
By addressing organics in addition to the EP Tox inorganics, the TC Rule addresses
the potential harm these organic substances could cause in the environment.
By increasing the costs of disposal for facilities which are now handling hazardous
wastes which were formerly not regulated, facilities are encouraged to find
substitutes or otherwise avoid chemicals which are hazardous.
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o
m
73
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Chapter 2
APPLICATIONS OF THE TCLP METHOD
What is TCLP?
When is the Use of TCLP Applicable?
Analytical Method Selection
-------
2.0 APPLICATIONS OF THE TCLP METHOD
Discussions in this chapter include:
What is TCLP?
• When is the use of TCLP applicable?
• Analytical method selection.
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2.1 What is TCLP?
An analytical method to simulate leaching through a landfill. The
leachate is analyzed for appropriate analytes.
TCLP is comprised of four fundamental procedures:
- sample preparation for leaching
- sample leaching
- preparation of leachate for analysis
- leachate analysis
The Toxicity Characteristic does NOT equal TCLP.
The leaching procedure can be found in either of the following references:
• Test Methods for Evaluating Solid Wastes (Physical/Chemical Methods, EPA
Method Number 1311), July 1992. (Forthcoming update)
• Code of Federal Regulations (40 CFR Part 261, Appendix II).
Both procedures were amended by a November 24, 1992 Federal Register Notice.
The SW 846 method 1311 will be updated to correct typographical errors in section 7.3.4
and section 7.2.11. Appendix I of this document includes the updated method 1311,
which is forthcoming. When regulations specify the use of TCLP, approval to deviate from
the method must be obtained from the State or EPA Region.
The Toxicity Characteristic (TO is one of four criteria in 40 CFR Part 261 to determine
whether a solid waste is classified as a hazardous waste. The other three are corrosivity,
reactivity, and ignitability. The Toxicity Characteristic of a waste material is established
by determining the levels of 8 metals and 31 organic chemicals in the aqueous leachate of
the waste. The TC utilizes the TCLP method to generate the leachate under controlled
conditions. The regulatory levels of the TC constituents in the TCLP leachate are listed in
Table 2-1.
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2.2 When is the Use of TCLP Applicable?
The most common reasons for performing the TCLP are:
• Determining if an unknown waste is hazardous according to 40 CFR
261.24.
• Determining what type of disposal (hazardous waste or solid waste) is
appropriate. Solid wastes ARE NOT NECESSARILY Hazardous.
• Demonstrating the effectiveness of treatment processes to comply with
Land Disposal Restrictions (LDR) or "Land Ban" requirements.
• Fulfilling shipping or transportation requirements.
When is the use of TCLP NOT applicable?
The most common misuse of TCLP is to:
• Perform Risk Assessments.
Determining if a Waste is Hazardous
The toxicity characteristic regulations require that generators be responsible for
determining whether a solid waste is a regulated hazardous waste. Generators of
potentially hazardous waste can determine if a waste is hazardous by any one of the
following methods:
• If a waste is excluded from regulation (40 CFR 261.4), no further determination is
necessary.
• If the waste is listed per 40 CFR 261.30-261.35. Listings may be industry and
process-specific (K-wastes) or may encompass all wastes from non-specific
processes (F-wastes). Listings also include commercial chemical and off-
specification products (P and U wastes).
• If a waste is not excluded or not listed as a hazardous waste, the generator must
ascertain whether the waste exhibits any hazardous waste characteristic: toxicity,
ignitability, corrosivity, or reactivity.
• A solid waste is classified as a hazardous waste because of characteristics,
knowledge, or testing.
• If the waste is not listed, and there is not enough information to determine whether
the Toxic Characteristic constituents are present above regulatory action levels, the
TCLP test must be performed.
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• The waste generator must certify in writing that the waste is not hazardous and
must maintain records to demonstrate exclusion from RCRA requirements by
knowledge or testing results.
Characterizing Waste for Disposal
• The RCRA regulations specify how listed and characteristic hazardous waste must
be treated or disposed.
• Hazardous waste disposal facilities are permitted to accept specific categories of
hazardous waste. Hazardous waste disposal facilities cannot accept hazardous
waste without a manifest which lists the characteristics of the hazardous waste.
TCLP waste characterization may be required by some disposal facilities.
• Disposal facilities may require initial waste testing. After analytical data are
collected from a waste, process knowledge may be used instead of testing.
The Land Disposal Restrictions (LDR) regulate hazardous waste treatment and subsequent
disposal. The following is a synopsis of the LDR regulations and their CFR citations:
• 40 CFR Part 268 Subpart A
The highlights are:
Definitions of "Waste water" (40 CFR 268.2).
Material otherwise prohibited from land disposal may be treated in a surface
impoundment if the residues from that treatment comply with applicable
standards.
Petitions to allow land disposal of 40 CFR Part 268 Subpart C prohibited
wastes must include comprehensive waste and simulation model sampling
and analysis. This typically includes TCLP and other analysis.
Generators of restricted waste must either analyze their waste or its TCLP
extract or use process knowledge to ascertain if the waste complies with 40
CFR Part 268 Subpart D treatment standards for land disposal. The
generators must submit copies of the restricted waste's chemical analysis to
the hazardous waste storage or disposal facility.
Restricted wastes are subject to the treatment standards of 40 CFR Part
268 Subpart D. The generator must notify the disposal company of the
restriction and must supply test data if available.
• 40 CFR Part 268 Subpart B
This section outlines a timetable for waste disposal prohibitions and establishment
of treatment standards.
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40 CFR Part 268 Subpart C
This section outlines waste disposal prohibitions. The following are examples of
hazardous wastes that must meet LDR requirements:
Solvent waste codes F001-F005, including waste from Comprehensive
Environmental Response, Compensation and Liability Act of 1980 (CERCLA)
actions.
Dioxin containing waste codes F020-F023 and F026-F028, including
CERCLA waste.
California List wastes, including hazardous waste that contain 1,000 mg/L
(liquid) or 1,000 mg/kg (non-liquid) of certain halogenated organic
compounds, liquid hazardous wastes that contain >_ 50 ppm PCBs, and
liquid hazardous wastes that contain >_ 134 mg/L nickel or _>. 130 mg/L
thallium.
SW-846 Method 9095 must be used to determine if a waste is liquid.
The initial generator of a California List hazardous waste must test
the waste (not an extract), or use knowledge of the waste, to
determine if the concentration levels in the waste meet the regulatory
levels for California listed waste.
Prohibitions for wastes with D, K, P, and U hazardous waste codes
are also listed with effective dates of prohibition.
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40 CFR Part 268 Subpart D
This section outlines LDR treatment standards. 40 CFR Subpart D 268.41 lists
treatment standards expressed as concentrations in the waste extract.
A restricted waste may be land disposed only if an extract of the waste or of
the treatment residue of the waste, using the TCLP, does not exceed the
values shown in CCWE of 268.41 for any TC constituent (See Appendix II).
The August 18, 1992 Federal Register (see Appendix II) requires total
analysis instead of TCLP leachate testing for some hazardous wastes.
The regulation specifies concentrations which may not be exceeded by the
extract of a waste or waste treatment residual using the TCLP method. The
following Hazardous Waste Codes are exceptions: D004, D008 (lead),
D031, K084, P010, P011, P012, P036, and U136 (all arsenic), K101 (o-
nitroaniline, arsenic, cadmium, lead, and mercury), and K102 (o-nitrophenol,
arsenic, cadmium, lead, and mercury).
The maximum concentrations which may not be exceeded for arsenic and
lead containing wastes listed were based on EP Toxicity Tests, not TCLP. If
the waste does not pass the concentration requirements by TCLP, the EP
Toxicity Test found in Appendix IX of 40 CFR Part 268 or SW 846 Method
1310A may be used for these contaminants.
LDR treatment standards are based entirely on technology-based standards
expressed as Best Demonstrated Available Technology (BOAT). TC levels
are based upon health-based allowable concentration levels and Dilution
Attenuation Factors (DAFs). Therefore the TC regulatory action levels are
NOT the same as the LDR treatment standards in all cases. For many
characteristic wastes, EPA has set the LDR treatment standards at the
characteristic level. Note that EPA has not yet established LDR standards
for D018 through D043 TC wastes.
LDR Records
40 CFR Part 268.7 requires hazardous waste generators and receivers to maintain
the following records of process knowledge or data regarding:
A determination that a restricted waste does NOT meet treatment standards.
A determination that a restricted waste can be land disposed without further
treatment.
A determination that waste is exempt under 40 CFR Part 268.5, 268.6 or a
nationwide capacity variance under Subpart C of 40 CFR Part 268.
A determination to manage a prohibited waste in tanks or containers during
waste treatment.
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• The generator must certify that the waste is not hazardous either by knowledge of
testing or by knowledge of process generation. While records are only required for
hazardous waste, it is prudent to maintain records of non-hazardous waste
classification.
• The generator must keep records on-site for five years from the date that the waste
was last sent to on-site or off-site treatment, storage, or disposal. The record
retention time is extended if an enforcement action occurs within five years of
waste generation.
• In general, the types of information required in all of the aforementioned records
include:
Hazardous waste numbers
Manifest numbers
Waste analysis data if applicable
Treatment standards (including codes for required treatment technologies.)
Certification statements signed by the generator
Any waste analysis plans
Issues to consider When Using a Leach Test for Risk Assessment
When determining whether to use the TCLP for risk assessment, it is important to
remember that the TCLP simulates worst case management of hazardous waste in
a landfill. Much caution must be used before TCLP data are used in risk
assessment because the TCLP conditions rarely reflect actual site conditions.
EPA's Science Advisory Board Report outlines many limitations of using TCLP for
risk assessment at industrial sites. The Science Advisory Board recommends
developing leach tests which are appropriate to site conditions. One major concern
is that the TCLP model assumes there is no attenuation in concentration over the
leaching time.
EPA's 1991 Science Advisory Board report on Leachability Phenomena concluded
that:
1. Many of the proposed uses of the EP and TCLP test have been inappropriate
because the waste management scenarios of concern were not within the
range of conditions used in the development of the tests themselves. In
most cases of inappropriate use of the EP or TCLP tests, the justification
given was that it was necessary to cite "standard" or "approved" methods.
Even if it is acknowledged that the tests cannot be applied without
significant change in test protocol itself, the need to use a previously
"approved" test has been cited, (page 3)
2. A variety of contaminant release tests and test conditions which incorporate
adequate understanding of the important parameters that affect leaching
should be developed and used to assess the potential release of
contaminants from sources of concern. In scientific terms, no "universal"
test procedure is likely to be developed that will always produce credible and
relevant data for input to all decision making exercises, (pages 7-8)
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3. Leach test conditions appropriate to the situations being evaluated should be
used for assessing long-term contaminant release potential. The best way to
estimate the extent of contaminant release from a waste matrix of interest is
to have a test that reflects realistic field conditions, (page 13)
4. To facilitate the evaluation of risk implications of environmental releases, the
EPA should coordinate the development of leach tests and the development
of models in which the release terms are used, (page 17).
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2.3 Analytical Method Selection
Strategy for Analytical Method Selection:
• Determine the analytes.
• Determine the methods of analysis.
• Specify detection limits and regulatory action levels.
• Specify quality control samples and requirements.
To specify appropriate analytes to demonstrate compliance with the TC regulations, the
data requester needs to understand the basic groupings of analytes which are performed
by each analytical method. The data requester also must understand the typical detection
limits and the issues which revolve around not being able to achieve these limits. The
following tables outline the TC constituent, the category of the analyte, and the potential
methods of sample preparation and analysis. The current CLP contract required detection
limits/quantitation limits and the SW-846 practical quantitation limits are also presented in
this section.
The analytical method information should be used in conjunction with process knowledge
and Table 2-1, which lists the TC constituents and regulatory levels, to plan the sampling
and analysis.
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Table 2-1
TOX/C/TY CHARACTERISTIC CONSTITUENTS - ALPHABETICAL
EPA HW1
Number Constituent
D004*
D005*
D018
D006*
D019
D020
D021
D022
D007*
D026
D023
D024
D025
D016*
D027
D028
D029
D030
D012*
D031
D032
D033
D034
D008'
D013*
D009]
D014*
D035
D036
D037
D038
D010*
D011*
D039
D015*
D040
D041
D042
D0 17.*
DC43
*
1
2
Arsenic
Barium
Benzene
Cadmium
Carbon tetrachloride
Chlordane
Chlorobenzene
Chloroform
Chromium
Cresol
o-Cresol
m-Cresol
p-Cresol
2,4-D
1,4-Dichlorobenzene
1,2-Dichloroethane
1,1-Dichloroethylene
2,4-Dinrtrctcluene
Endrin
Heptachlor (and its
epoxide)
Hexachlorobenzene
Hexachloro-1 ,3-butadiene
Hexachloroethane
Lead
Lindane
Mercury
Methoxychlor
Methyl ethyl ketone
Nitrobenzene
Pentachlorophenol
Pyridine
Selenium
Silver
Tetrachloroethylene
Toxaphene
Trichloroetnvjene
2,3,5-Trichiorophenol
2,4,6-Trichlorophenol
. . 2,4.5-TP (Silvex)
Vinyl Chloride
CTRL
Basis
MCL
MCL
MCL
MCL
MCL
RSD
RfD
RSD
MCL
RfD
RfD
RfD
RfD
MCL
MCL
MCL
MCL
RSD
MCL
RSD
RSD
RSD
RSD
MCL
MCL
MCL
MCL
RfD
RfD
RfD
RfD
MCL
MCL
RSD
MCL
MCL
RfD
RSD
MCL
MCL
14 original constituents based on drinking water
Hazardous waste number
If o-, m-, and p-Cresol concentrations
cannot be
CTRLs
(mg/l) x of
0.05
1.0
0.005
0.01
0.005
0.0003
1.0
0.06
0.05
2.0
2.0
2.0
2.0
0.1
0.075
0.005
0.007
0.0005
0.0002
0.00008
0.0002
0.005
0.03
0.05
0.004
0.002
0.1
2.0
0.02
1.0
0.04
0.01
0.05
0.007
0.005
0.005
4.0
0.02
0.01
0.002
standards.
differentiated,
DAF Regulatory .
100 = Level (mg/l)
5.0
100.0
0.5
1.0
0.5
0.03
100.0
6.0
5.0
200.02
200.02
200.02
200.02
10.0
'7.5
0.5
0.7
0.13
0.02
0.008
0.13
0.5
3.0
5.0
0.4
0.2
10.0
200.0
2.0
100.0
5.03
1.0
5.0
0.7
0.5
0.5
400.0
2.0
1.0
0.2
the total Cresol
concentration is used. Total Cresol regulatory level: 200 mg/l.
3
(f quantrtation limit is greater than the
limit becomes regulatory level.
calculated
regulatory level, quantrtation
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General Method Information
Method Selection
• There are two categories of permissible methods used to analyze TCLP extracts:
1. SW-846 methods are required to demonstrate compliance with the Land Ban
regulations. Appendix X explains when SW-846 methods are mandatory.
2. Any appropriate EPA approved method may be used to demonstrate
compliance with the TC regulations. However, if the data is going to be
validated, Contract Laboratory Program (CLP) methods are recommended.
Two semi-volatile TC analytes (m-cresol, pyridine) are not included in the
CLP target compound list of analytes. Therefore, the method must be
slightly modified to incorporate these two compounds.
Specifying detection limits and regulatory action levels
• The method or contract detection limits must be evaluated versus the regulatory TC
limits. The method or contract limits must be lower than the regulatory limits.
• There are three compounds which have quantitation limits that exceed the
regulatory limits: 2,4-dinitrotoluene, hexachlorobenzene, and pyridine. In these
cases, the quantitation limit becomes the regulatory limit.
• The EPA Region II TCLP SAS Request (Appendix IX), shows recommended TC
detection limits which are increased in order to minimize matrix effects.
Metals Analysis Information
Metals analysis can be performed by three methods: Inductively Coupled
Plasma (ICP), Flame Atomic Absorption (FAA) and Graphite Furnace Atomic
Absorption (GFAA).
Laboratories usually analyze metals, except mercury, in the TCLP
extract by ICP.
Mercury is usually analyzed by Cold Vapor Atomic Absorption
(CVAA).
The GFAA generates lower detection limits than ICP method.
The CLP Contract Required Detection Limits (CRDLs) are the same for both
ICP and GFAA.
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Table 2-2 Metals Analysis Method By ICP
Analyte
Arsenic
Barium
Cadmium
Chromium
Lead
Selenium
Silver
SW 846
Preparation/
Analysis
3010/6010
3010/6010
3010/6010
3010/6010
3010/6010
3010/6010
7760 (prep
only)/6010
SW 846 PQL,
mg/L(1)
.05
.002
.004
.007
.04
.07
.007
CLP CRDLs,
mg/L (2)
.01
.2
.005
.01
.003
.005
.01
(1) PQL = Practical Quantitation Limit = EQL = Estimated Quantitation Limit
(2) ' Contract Laboratory Program, Statement of Work for Inorganic Analysis, ILM03.0
Table 2-3 Metals Analysis Methods by GFAA and Mercury by CVAA
Analyte
Arsenic
Barium
Cadmium
Chromium
Lead
Selenium
Silver
Mercury
SW 846
Preparation/
Analysis
7060/7060
3020/7080
3020/7131
3020/7191
3020/7421
7740/7740
7760 (prep
only)/7760
7470
SW 846 PQL,
mg/L(1)
.001
.1
.001
.001
.001
.002
.01
.0002
CLP CRDLs,
mg/L (2)
.01
.2
.005
.01
.003
.005
.01
.0002
(1) PQL = Practical Quantitation Limit = EQL = Estimated Quantitation Limit
(2) Contract Laboratory Program, Statement of Work for Inorganic Analysis, ILM03.0
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Table 2-4 Pesticide and Herbicide Quantitation Limits by SW 846 and CLP
Analyte
Pesticides
endrin
lindane
(gamma BHC)
methoxy-chlor
heptachlor
toxaphene
chlordane
Herbicides
2,4-D
2,4,5-TP (Silvex)
SW 846
Preparation/
Analysis
3510 or 3520/
8080B
35 10 or 3520/
8080B
3510 or 3520/
8080B
3510 or 3520/
8080B
3510 or 3520/
8080B
3510 or 35207
8080B
8150A
8150A
SW 846 PQL,
ug/L(1)
0.06
0.04
1.76
0.03
2.4
0.14
12
2.0
CLP CRQL,
ug/L (2)
0.10
0.05
0.05
0.05
5.0
0.05
(3)
(3)
(1) PQL = Practical Quantitation Limit = EQL = Estimated Quantitation Limit
(2) Contract Laboratory Program, Statement of Work for Organic Analysis, OLM01.8
(3) No CLP methods exist for these compounds.
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Table 2-5 Quantitation Limits for Volatile TC Constituents
Volatiles
benzene
carbon tetrachloride
chloroform
chlorobenzene
1 ,2-dichloroethane
1,1-dichloroethylene
(1,1 -dichloroethene)
methyl ethyl ketone
(2-butanone)
tetrachloroethylene
(tetrachloroethene)
trichloroethylene
(trichloroethene)
vinyl chloride
SW 846 Preparation/
Analysis
8240B or 8020B
8240Bor 8010B
8240Bor 801 OB
8240Bor 8010 or
8020B
8240B or 801 OB
8240Bor 801 OB
8240B (2) or 8015
8240Bor8010B
8240Bor 801 OB
8240Bor 801 OB
SW846
8240 PQL,
ug/L(1)
5
5
5
5
5
5
100
5
5
10
CLP
CRQL,
ug/L (3)
10
10
10
10
10
10
10
10
10
10
(1) PQL = Practical Quantitation Limit = EQL = Estimated Quantitation Limit
(2) Poor purging efficiency by this method produces a high detection limit.
(3) Contract Laboratory Program (CLP) Statement of Work for Organic Analysis, OLM01.8
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Table 2-6 Quantitation Limits for Semivolatile TC Constituents
Semivolatiles (BNAs)
o-cresol
(2-methylphenol)
m-cresol
(3-methylphenol)
p-cresol
(4-methylphenol)
1 ,4-dichlorobenzene
2,4-dinitrotoluene
hexachlorobutadiene
(hexachloro-1,3-butadiene) (4)
hexachloroethane
hexachlorobenzene
nitrobenzene
pentachlorophenol
pyridine
2,4,5-trichlorophenol
2,4,6-trichlorophenol
SW 846
Preparation/
Analysis
3510/8270B
3510/8270B
3510/8270B
3510 or 35207
8270B
35 10 or 3520/
8270B
3510 or 3520/
8270B
35 10 or 3520/
8270B
3510 or 3520/
8270B
35 10 or 3520/
8270B
3510 or 3520/
8270B
3510 or 8270B
35 10 or 3520/
8270B
3510 or 35207
8270B
SW 846
PQL,
ug/L(1)
10
10
10
10
10
10
10
10
10
50
ND (2)
10
10
CLP CRQL,
ug/L (5)
10
(3)
10
10
10
10
10
10
10
25
(3)
25
10
(1) PQL = Practical Quantitation Limit = EQL = Estimated
Quantitation Limit
(2) ND = Not Determined. If these methods are used, the method detection limits must be determined.
(3) These analytes are not routinely part of the CLP method. IF required for TC, these analytes must be
specially requested. The CLP 2/88 extraction procedure must be used for the TC semivolatile analytes if
these enalytes are desired.
(4) Other methods quantitate this in the volatile fraction.
(5) Contract Laboratory Program, Statement of Work for Organic Analysis, OLM01.8
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o
g
•o
S
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Chapter 3
TC AND TCLP PROJECT PLANNING
Data Quality Objectives
Sampling and Analysis Design
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3.0 TC AND TCLP PROJECT PLANNING
Planning a project prior to sampling and analysis promotes successful
implementation. The conclusion of the planning process should result in an
efficient sampling and analysis design which allows the collection of
appropriate data. The appropriate data should promote making an appropriate
decision as to the storage, treatment or disposal of the waste. This chapter
provides information in the following areas which are critical to project
planning.
• Data Quality Objectives (DQOs)
• Sampling and analysis design
Sample containers, preservation, and storage
Sample volumes
Sample decontamination
Holding times
Field QC
Documentation
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3.1 Data Quality Objectives
Environmental samples are often collected and analyzed without proper
planning. The data collected may not allow a correct decision to be made.
In response to this problem, EPA has developed a planning process to facilitate
clear definition of the decision to be made and the data required to make these
decisions. This process is the Data Quality Objective (DQO) process. Prior to
initiating sampling, the questions to be answered should be listed, prioritized
and one primary question identified. These should be agreed upon by all
parties, including the regulatory agencies and TSDFs, the site owners and
operators/generators, and the technical staff.
The DQO Process should identify:
• What question will the data resolve?
• Why is a specific type, quantity and quality of data needed?
• How will the customer use the data to make a defensible decision?
• How much data are required?
• What resources are needed?
The information included in the DQO section describes the following
information:
• DQO definition
• DQO Planning Process (DQO-PP) description
Value of DQO-PP
• Example of DQO-PP implementation
The American Society of Testing and Materials (ASTM) Committee D34.02.10 is working
with Quality Assurance Management Staff (QAMS) and the Office of Solid Waste to
produce an ASTM Standard Practice which describes the DQO Planning Process (DQO-PP).
Many of the following flow charts, definitions and information are derived from these
discussions and from the draft ASTM document.
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DQOs are defined as:
Qualitative and quantitative statements describing the level of uncertainty that project
managers and decision makers are willing to accept in making a decision.
The DQO Planning Process is:
A Total Quality Management tool developed by the US EPA to facilitate the
planning of environmental data collection activities. The DQO Planning Process
asks planners to focus their efforts by specifying the use of the data (the decision),
the decision criteria, and their tolerance to accept an incorrect decision based on
the data.
Additional discussion by ASTM indicates:
DQOs result from an iterative process between the decision makers and the
technical team to develop qualitative and quantitative statements which describe
the certainty and uncertainty that a decision maker is willing to accept in the results
derived from the environmental data. The acceptable level of uncertainty should be
used as the basis for the design specifications for project data collection and data
assessment.
While the goal of this course is to understand the TC and TCLP regulations, one must
understand that if an appropriate sampling design is not utilized, the data may not allow a
waste generator to accurately determine if a solid waste is a hazardous waste. The DQO-
PP is essential for preparing an appropriate sampling and analysis design.
All sampling and analysis designs have potential error. Typically, laboratory error is more
defined and understood than sampling error. Therefore, it is essential to attempt to
quantitate acceptable sampling and analytical error. Since sampling is frequently
performed without adequate planning, potential sampling error is not always properly
quantitated. Using the DQO Process will assist in determining the amount and type of
information required, including the acceptable levels of error to answer the questions.
A second example of the DQO-PP, developed by the Quality Assurance Management Staff
of EPA, is presented in Appendix III.
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What is the value of using the DQO-PP?
The DQO-PP:
• helps users determine the amount and quality of data needed.
• saves resources by making data collection operations more efficient.
• encourages communication between the data users, technical experts, and decision
makers.
• helps focus studies by clarifying vague objectives and narrowing the questions to
the essential issues.
• helps provide a logical process which facilitates documentation.
Additional critical information about the DQO-PP
• A statistical design, which may result from the DQO-PP, allows the uncertainty in
the data to be quantified. Chapter 9 of SW-846 outlines strategies for statistical
design. The statistical design must be carefully applied to assure that the correct
assumptions are made and that the assumptions address the question(s) related to
the objectives.
• The DQO-PP is iterative. Projects should focus on essential questions and take a
phased approach to answering these questions. This allows reevaluation of the
DQOs as the data collection is completed. This iteration allows the resources to be
efficiently used.
• The term "decision maker" used in this document may include owners and
managers of facilities and regulators. Prior to undertaking large projects, the
owners and managers may choose to involve the regulators to assure consensus is
reached in the planning phase.
The following discussion presents summary information about each of the seven steps
within the DQO Planning Process shown in Figure 3-1.
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The DQO Planning Process has a logical problem solving structure which includes the
following seven steps:
1. State the question
2. Identify the decision
3. Identify the inputs to the decision
4. Define the study boundaries
5. Develop a decision rule
6. Specify acceptable limits on uncertainty
7. Optimize the design
1. State the question
The essential goal of this step is to focus the decision makers and the technical team on
one or more questions. These questions should be as narrowly stated as possible. For
waste generators, these questions may focus on whether a particular waste is hazardous.
2. Identify the decision
A clear, concise statement of the potential answer(s) to the question(s) should be agreed
upon by the decision makers and the technical team. This step results in a statement of
how the data will be used in making the decision.
3. Identify the inputs to the decision
The goal is to evaluate the data which are needed to make the decision. Questions such
as whether metals or organic data must be generated should be addressed. Production or
process data may be required if the task is related to a waste generator. Additionally,
knowledge about the homogeneity of the material to be sampled may need to be
determined.
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Figure 3-1
Overview of the Data Quality Objectives Planning Process
State the Question
I
Identify the Decision
I
Identify the Inputs to the
Decision
I
Define the Study Boundaries
I
Develop a Decision Rule
I
Specify Acceptable Limits on
Uncertainty
I
Optimize the Design
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This data should also include any time factors, physical limitations, process data, and
resources which may effect the sampling and analysis. The environmental characteristics
required should also be listed.
4. Define the study boundaries
The boundaries are the limitations on the study. Examples include time and budget
constraints, permit requirements, disposal requirements, and exposure levels. This step is
often performed simultaneously with the previous step.
5. Develop a decision rule
This is a statement which describes how the data will be summarized, collected, and
compared to the decision. The statement should include actions which will be based on
criteria and conclusions from the sampling and analysis. The statement should be an
"if...then..." statement that incorporates the action limits. An example statement: If 10
drums out of 100 contain greater than 1 mg/L of cadmium, the material will be disposed of
as a hazardous waste.
6. Specify acceptable limits on uncertainty
The decision maker should understand that results of all studies have uncertainty and
error. The goal is to quantitate the amount of uncertainty that the decision maker is
willing to accept in making the decision. The key step is to move from a qualitative
"feeling" of uncertainty to a quantitative level of uncertainty. The process for establishing
this, in the case of a hazardous waste determination, includes the following:
i. Identify the consequences of incorrectly deciding the waste is not hazardous, also
known as a false negative decision error.
ii. Identify the consequences of incorrectly deciding the waste is hazardous, also
known as a false positive decision error.
iii. Rank these consequences by severity.
iv. Estimate the health risk and financial risk associated with an incorrect result.
v. Estimate how far below the regulatory limit one wants to be in order to decrease
either the consequence of a false positive or negative. Some statistical experience
is normally needed to make this assessment.
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This information is incorporated into the decision rule. An example decision rule which
incorporates the uncertainty is:
Three samples per drum are collected and the concentrations from each drum are
averaged. If the individual average concentrations of cadmium in 90 drums out of
100 contain greater than 0.7 mg/L of cadmium, then the material will be disposed
of as a hazardous waste.
7. Optimize the design
In order to successfully characterize a site or waste, a sampling and analysis design must
be established. The sampling and analysis design includes development of statistical and
observational design alternatives, and specifies sampling, handling, and analysis methods.
The design indicates the number and locations of samples based on the acceptable error or
uncertainty which was agreed on during the DQO development. The most important input
from the DQO process is the degree of uncertainty which the decision maker will accept.
When preparing a sampling and analysis design, the time and budgetary constraints should
be evaluated to determine their import.
The preliminary design may contain the following information:
• Spatial areas of interest
• Hot spots versus average values of contamination
• Particular contaminants of concern
• Desired levels of detection
• Which matrices will be investigated
• Patterns of contamination
• Stratification of the contaminants
• Contaminant degradation
• Temporal considerations (changes of concentration over time)
• Quality control samples designed to allow estimation of precision and accuracy, and
background contamination
• Health and safety issues
Designs must be practical and achievable. There is no one correct design but rather an
optimum design which balances resources with the data required to make a decision.
Technical staff must work carefully to present several designs to decision makers outlining
the uncertainty, resources and benefits of each design.
Other factors used to select the appropriate measurement methods include:
DQOs.
• required regulatory or risk assessment detection limits.
• method precision and accuracy.
• contaminants of interest.
Improved accuracy, precision, and lower detection limits usually result in higher sampling
and analytical costs because larger sample sizes, improved instrumentation, and more
field/analytical expertise may be required. If matrix specific information about the
accuracy and precision are not available, preliminary precision and accuracy studies must
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be performed, and may require approval by appropriate regulatory agencies prior to using
the method.
Prior to sampling design implementation, the decision makers must approve the design.
Several designs may be presented to the regulators and decision makers. The level of
uncertainty, advantages and disadvantages, budgetary and time constraints, and other
relevant factors must be presented for each design. This approach allows the decision
makers and regulators to properly assess options and to agree upon the best sampling
design. Sampling designs are implemented after approval by the decision makers.
The technical team must continually evaluate the proposed designs with respect to the
DQOs, health and safety criteria, budget and time constraints. If the proposed design does
not meet the criteria, it must be altered. In extreme cases, the DQOs may need
adjustments if they are unattainable. The DQOs should only be changed after consultation
with the decision makers and team members. The DQOs may need to be reevaluated if a
decision cannot be made.
References for sampling design strategies are:
• U.S. EPA, Test Methods for Evaluating Solid Wastes, SW-846 (Chapter 9).
November 1986.
• U.S. EPA, Characterizing Heterogeneous Wastes: Methods and Recommendations.
EPA 600/R-92/033. February 1992.
Chapter 9 of SW 846 outlines several statistical design approaches. Many other design
strategies exist and may be better suited for the situation at hand. It is wise to examine
many statistical options and methods of evaluating the data during the planning phase.
An example of using the DQO-PP is presented in the following pages. This example
demonstrates how to design a sampling program to determine whether fly ash from a
municipal incinerator is a RCRA hazardous waste. This example is from a draft ASTM
standard practice on the use of DQO-PP in waste management activities. The ASTM
document was the product of a cooperative agreement between ASTM, QAMS and the
Office of Solid Waste. The example was written by Dr. Charles Bayne of the Oak Ridge
National Laboratory and the ASTM D.34.02.10 committee.
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3.2 DQO Case Study: Cadmium Contaminated Fly Ash Waste
Background
A municipal waste incineration facility located in the Midwest routinely removes fly ash
from its flue gas scrubber system and disposes it in a sanitary landfill. Previously, it was
determined that the ash was "non-hazardous" under RCRA regulations. However, the
incinerator has recently begun treating a new waste stream. As a result, a local
environmental public interest group has asked that the ash be retested against RCRA
standards before it is dumped. The group is primarily concerned that the ash could contain
hazardous levels of cadmium from the new waste sources. The facility manager has
agreed to test the ash and decides to employ the Data Quality Objectives process to help
guide decision-making throughout the project.
Cadmium is primarily used as corrosion protection on metal parts of cars and electrical
appliances. It is also used in some batteries. Cadmium and cadmium salts have toxic
effects for humans through both ingestion and inhalation exposures. Ingestion exposure
usually causes mild to severe irritation of the gastrointestinal tract which can be caused by
concentrations as low as 0.1 mg/kg/day. Chronic (long term) inhalation exposure can
cause increased incidence of emphysema and chronic bronchitis. However, the primary
target of inhalation exposure is the kidney. Severe and chronic inhalation exposure has
been shown to cause increased incidence of kidney stones and kidney disfunction.
Under the current Code of Federal Regulations (CFR), Part 261, the method for
determining if a solid waste is a hazardous waste by toxicity characteristic (for cadmium)
under RCRA is to sample a "representative portion" of the waste and perform a Toxicity
Characteristic Leaching Procedure (TCLP). During this process, the solid fly ash will be
"extracted" or mixed in an acid solution for 18 hours. The extraction liquid will then be
subjected to tests for specific metals and organic chemicals. For this example, the only
concern is with the concentration of cadmium. The primary benefit of the DQO process
will be to establish the sampling design needed to determine whether the waste is
hazardous under RCRA regulations with a quantifiable level of uncertainty.
DQO Development
The following is a representative example of the output from each step in the DQO
process.
Assemble the Team -- The Plant Manager assembled a skeletal team consisting of himself
and a representative of the current disposal facility staff. The two of them assembled the
team with the responsibility to deal with this problem.
The members of the evaluation team will include the incineration plant manager, a
representative of the environmental public interest group, a representative of the
community where the ash is currently being dumped, a statistician, a toxicologist, and a
chemist with sampling experience. There will not be a primary decision maker, individual
decisions will either be allocated to members of the evaluation team or decided by
consensus.
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Review Available Site Data
Since the concern is with a new waste stream, the team ordered a pilot study of the fly
ash to determine the variability in the concentration of cadmium between loads of fly-ash
leaving the facility. They have determined that each load is fairly homogeneous.
However, there is a high variability between loads due to the nature of the waste-stream.
Most of the fly ash produced is not a RCRA hazardous waste and may be disposed of in a
sanitary landfill. Because of this, the company has decided that testing each individual
waste load before it leaves the facility would be the most economical. In that way, they
could send loads of ash that exceeded the regulated cadmium concentrations to the higher
cost RCRA landfills and continue to send the others to the sanitary landfill.
Identify Contaminants of Concern, Media and Regulatory Limits - The team identified the
following factors critical to the problem:
• Contaminants of concern: cadmium soluble in the Toxic Characteristic Leaching
Procedure (TCLP).
• Sample Matrix: fly ash.
• Regulatory Limit: 1 mg/L.
Specific Project Budget and Time Constraints
The incinerator plant manager has requested that all stages of the operation be performed
in a manner that minimizes the cost of sampling, chemical analysis and waste disposal.
However, no formal cost constraints have been implemented.
Time - The environmental public interest group has threatened to file a law suit for
violation of environmental regulations if testing does not proceed within a
"reasonable time-frame.11
1. STATE THE PROBLEM
A description of the problem(s) and specifications of available resources and relevant
deadlines for the study.
Available Resources - The waste generator (the incineration company) wishes to
spend as little as possible to determine the concentration of cadmium. However,
the project will not be constrained by cost.
Statement of the Question
The problem is to determine which loads of fly ash are to be sent to a RCRA landfill and
which loads of fly ash are to be sent to a sanitary landfill.
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2. IDENTIFY THE DECISION
A statement of the decision that will use environmental data and the actions that could
result from this decision.
State the Decision(s) -- Determine whether the mean concentration of cadmium in
the waste fly ash exceeds the regulatory RCRA standard.
Identify the Decision(s) to be Made
i. Decision -- Determine whether the average concentration of cadmium in the waste
fly ash exceeds the regulatory RCRA standards.
ii. State the Actions That Could Result From the Decision --
a) If the average concentration of cadmium is greater than the action level,
then dispose the waste fly ash in a RCRA landfill.
b) If the average concentration of cadmium is less than the action level, then
dispose the waste fly ash in a sanitary landfill.
3. IDENTIFY THE INPUTS NEEDED FOR THE DECISION
List the environmental variables or characteristics that will be measured; and other
information needed to make the decision.
i. Data Necessary -- In order to evaluate the problem, the evaluation team must
collect a representative sample of fly ash waste and subject it to the TCLP analysis
and test for cadmium.
ii. Identify the variables that need to be measured -- The concentration of cadmium
should be measured in representative samples of the fly ash using the test methods
listed in 40 CFR Part 261, Appendix II.
iii. Identify the Regulatory Threshold - The "regulatory threshold" is the RCRA
standard for cadmium (1.0 mg/l), using the test listed in 40 CFR Part 261,
Appendix II.
iv. Confirm that each variable can be measured -- Cadmium can be measured in the
solid waste according to the methodologies specified in 40 CFR Part 261, Appendix
II. Chemical analysis methods for cadmium include Atomic Absorption, Inductively
Coupled Plasma or Inductively Coupled Plasma/Mass Spectrometry.
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Define the Boundaries of the Study
Define a detailed description of the spatial and temporal boundaries of the decision;
characteristics that define the environmental media, objects or people of interest; and any
practical considerations for the study.
i. Specify the Characteristics that Define the Sample Matrix -- Representative samples
of waste fly ash from the hazardous waste incinerator will be analyzed. The fly ash
should not be mixed with any other constituents except water that is used for dust
control.
ii. Identify Spatial Boundaries -- The waste fly ash will be tested after it has been
deposited in the trailer used by the waste hauler. Separate decisions about the
toxicity of the fly ash will be made for each load of ash leaving the incinerator
facility. Each load of ash should fill the waste trailer at least 70%. In cases where
the trailer is filled less than 70%, the trailer must wait on-site until more ash is
produced and can fill the trailer to the appropriate capacity.
iii. Identify Temporal Boundaries ( The temporal boundaries of the study include the
time frame over which the study should be conducted). -- Contained in the trucks,
the waste does not pose a threat to humans or the environment. Additionally,
since the fly ash is not subject to change, disintegration or alteration, the chemical
properties of the waste do not warrant any temporal constraints. However, in
order to expedite decision making, the evaluation team has placed deadlines on
sampling and reporting. The fly ash waste will be tested within 48 hours of being
loaded on to waste hauling trailers. The analytical results from each sampling
round should be completed and reported within 5 working days of sampling.
iv. Identify Practical Considerations that May Interfere with the Study - The most
important practical consideration that could interfere with the study is the ability to
take "representative" samples from the fly ash that is stored in waste hauling
trailers. Although the trailers have open access, special procedures and methods
will have to be implemented in order for the samples to be "representative" for the
entire depth of the ash. It has been suggested that "core" samples may be one
practical solution to this problem. Additionally, in order to get the best
representative sample from each truck and in order to minimize the cost,
compositing of core samples has been suggested.
Are Contaminant Distributions Appropriately Defined?
The pilot study shows that the standard deviation of cadmium concentration within a load
is Sw = 0.4 mg/L and the standard deviation of cadmium concentration between loads is
SB = 1.4 mg/L. These results indicated that the loads are fairly homogeneous within each
load but not between different loads. Therefore, a decision will be made for each load to
send it either to a RCRA approved landfill or a sanitary landfill. The data from the pilot
study also indicated that the normal probability distribution is an appropriate distribution
for the cadmium concentration measurements. Quality control data also indicates that a
constant measurement variance can be assumed for the concentration range being
investigated. This probability model for the concentration measurements will be used to
calculate the decision performance curve and optimal sample sizes.
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5. Develop a Decision Rule - The arithmetic mean of sample results will be compared
to the action level. The arithmetic mean will be determined by using the sample standard
deviation together with the number of samples results.
Decision Rule:
a) If the average concentration of cadmium is greater than the action level,
then dispose the waste fly ash in a RCRA landfill.
b) If the average concentration of cadmium is less than the action level, then
dispose the waste fly ash in a sanitary landfill.
Develop Uncertainty Constraints on the Decision Rule
The decision makers specify acceptable decision errors based on the consequences of
making an incorrect decision. Both error rates have negative consequences.
In this example, there are two types of error that the evaluation team could make:
i. false positive error — If the true cadmium concentration is below 1 mg/L, but the
average measured cadmium concentration is above the action level, the non-
hazardous fly-ash waste will be sent to a RCRA landfill. The consequence of a
false positive error is that the company will have to pay the additional cost of
disposing the waste at a RCRA facility as opposed to a less expensive method of
disposal in a sanitary landfill.
ii. false negative error -- If the true cadmium concentration is equal to or greater than
1 mg/L, but the average measured cadmium concentration is below the action level,
the hazardous fly-ash waste will be sent to a sanitary landfill. The consequence of
a false negative error is that the fly-ash waste may be disposed on in a manner that
will be harmful to human health or the environment. Legal consequences and
subsequent remedial costs are also possible consequences.
iii. number of samples -- The number of samples will depend on the uncertainty of
estimating the true cadmium concentration for each load and the resources
available to sample and to chemically analyze the samples.
6. DEVELOP THE DATA QUALITY OBJECTIVES BY SPECIFYING ACCEPTABLE LIMITS
ON UNCERTAINTY
The purpose of this stage of the process is to specify the probabilities of making an
incorrect decision on either side of the "action level" that are acceptable to decision
makers. These are the Data Quality Objectives.
i. False Positive Error. The consequences of a false positive error will be that the
incinerator will have to pay more for disposal of the fly ash at a RCRA facility than
at a sanitary landfill. Therefore, the incinerator will want to guard against these
errors. However, they do not find these consequences to be as severe as the false
negative error. The performance curve will indicate this distinction by allowing a
higher probability of false positive errors. The evaluation team has set the
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probability of allowing a false positive error at 20% by weighing the monetary cost
.with the potential consequences of error.
ii. False Negative Error. The consequence of making a false negative error is that the
incinerator company will improperly dispose of fly-ash waste that possibly
endangers human health and the environment. In this situation, they may be liable
for future damages and environmental cleanup. In addition, the reputation of the
incinerator company may be compromised, jeopardizing its future profitability. The
toxicologist on the evaluation team has decided that a significant increase in both
pulmonary and kidney toxicity could occur if the true cadmium concentration is
above the regulatory threshold. For this example, the evaluation team has set the
probability of making a false negative error at 10% when the true mean is 1.0 mg/l.
iii. Number of Samples: For each fly-ash waste load, the decision makers would like to
estimate the true cadmium concentration in the load with an uncertainty of ±0.2
mg/L. In addition, the decision makers are willing to allocate resources to know
that the true cadmium concentration is in this interval with a confidence of 95%.
Decision Performance Curve
The Decision Performance Curve will be calculated to determine the action level and
review the performance of the decision rule. To calculate the Decision Performance Curve,
decision makers use the following steps:
Step 1: Number of samples are calculated with L = 0.2 mg/L, o = Sw = 0.4
mg/L, and a = 0.05 (or Zg/2 = 1.960 for a 95% confidence level).
f 1.960 x 0.4 \
( 0.2 J
= 16 .
Step 2: Calculate the action level (AL) from the specified false negative error
of 10%. The probability calculations are based on an approximating
normal probability distribution for the cadmium concentration
measurements. This approximating normal probability has a mean =
RT = 1 .0 mg/L and a standard deviation = Sw = 0.4 mg/L. The
10% percentile point for the standardized normal probability
distribution is Z0 10 = 1 .282.
False Negative Error = Pr( Average < AL when the true concentration = RT) =
0.10.
or
AL - RT _
AL = I.OmgjL - (1.282)(0.4/ngf£) / 4 = 1.0/nfl/i - 0.13mfl/Z.
or
AL = 0.87 mgIL .
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Therefore, the decision rule is:
a) If (average concentration of cadmium) > 0.87 mg/L, then dispose the
waste fly ash in a RCRA landfill.
b) If (average concentration of cadmium) < 0.87 mg/L, then dispose the
waste fly ash in a sanitary landfill.
The decision performance curve for this decision rule would have a probability of
taking action (i.e., sending fly-ash waste to a RCRA landfill) of 0.90 at a possible
true concentration value of RT = 1.0 mg/L.
Step 3: Calculate the true concentration (say, 6 < RT) that corresponds to an
action level of AL = 0.87 mg/L and a false positive error of 20%.
The probability calculations are based on an approximating normal
probability distribution for the cadmium concentration measurements.
This approximating normal probability has a mean = 0 mg/L and a
standard deviation = Sw = 0.4 mg/L. The 20% percentile point for
the standardized normal probability distribution is Z020 = 0.848.
False Positive Error = Pr{ Average < AL when the true concentration = 6} =
0.20.
or
B = O.Q7mglL - (0.848)(0.4/77fl/Z.) / 4 = 0.87mgIL - 0.08 mg/L
or
6 = 0.79 mgIL .
The decision performance curve would have a probability of taking an action (i.e.,
sending fly-ash waste to a RCRA landfill) of 0.20 at a true cadmium concentration
of 8 = 0.79 mg/L. The possible true cadmium concentration values in the interval
(0.79 mg/L, 1.0 mg/L) represents values that cause the decision rule to send fly-ash
waste to a RCRA landfill even though the true concentration is below the regulatory
threshold. This interval can be reduced by increasing the number of samples, by
changing the false negative error or by changing the false positive error.
Step 4: Draw the decision performance curve by using the standardized
normal probability distribution. The standardized normal probability
distribution is defined as a normal probability distribution with mean
= 0 and standard deviation = 1.0. There are many tables and
computer programs that can be used to calculate probabilities for a
standardized normal random variable, Z. A normal random variable,
X, with mean = p and standard deviation = a can be transformed to
a standardized normal random variable by Z = (X - //)/a.
3-16
-------
Prob( Action ) = Pr( Average > AL when the true concentration = 6).
Prob(Action) = 1.0 - Prot
Prob(Action) = 1.0 - Protiz <. °'87 6
Figure D.1 plots the decision performance curve of Prob( Action ) versus possible
true concentration values 8.
7. OPTIMIZE THE DESIGN
The decision maker(s) will select the lowest cost sampling design that is expected to
achieve the DQOs
The optimal design(s) for sampling the fly-ash waste will be generated by the
statisticians on the evaluation team. The choice of sampling plan will be decided by
consensus.
Cadmium Contaminated Fly-Ash Waste
i.o
5
o
cc
a
^e.
.«
e
o.
0.9-
O.8-
O.7-
O.6-
0.5-
0.4-
O.3-
O.2-
O.1 -
O.O
False Negative = 10%
False
Positive = 20%
Action
Level
Regulatory
Threshold
0.6 0.7 0.8 O.9 1.O 1.1 1.2
True Cadmium Concentration (mg/L)
Figure 3-2 Decision performance curve for cadmium fly-ash waste example.
3-17
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Implementation -- After completion of the sampling and measurement process, the data
assessment is performed. The concentration measurements from each load of fly-ash
waste are averaged and compared to the action level. Those loads with average
concentrations less than the action level will be sent to a sanitary landfill, and those loads
with average concentrations greater or equal to the action level will be sent to a RCRA
landfill. These decision rules should have a long range performance with a false negative
error of 20% and a false positive error of 10%.
3-18
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3.3 Sampling and Analysis Design
The following issues discussed in this section are critical in sampling and
analysis design:
• Total constituents versus TCLP
• Specifying sample collection procedures
Total constituents versus TCLP - EPA Memorandum
EPA has several memoranda which address issues such as Characterizing Heterogeneous
Material and Total Analysis Versus TCLP. These are presented in Appendix VII. Pages 10
and 19-22 of the Office of Solid Waste - Methods Section, Notes on RCRA Methods and
QA Activities, Memorandum #36, January 12, 1993, will be helpful in delineating
sampling design related to the analysis of samples for total constituents versus leachable
constituents. The consequential portions of Memorandum #36 and a discussion of their
significance follows.
Office of Solid Waste Memorandum - Methods Section #36^ January 12, 1993
Page 10 Characterizing Heterogeneous Materials
Characterization of a solid waste is essential for determining whether a waste is
hazardous or for developing management and treatment standards for hazardous
materials. Current EPA regulations for characterizing waste includes determining
the average property of the "universe or whole." This task is difficult when applied
to heterogeneous wastes because conventional sampling and compositing
techniques are often inadequate in providing a "representative sample" of the
waste. As a result, analytical results are often biased and imprecise, making
compliance decisions difficult.
The above paragraph means that all of the samples collected from a heterogeneous waste
do not have to be below the regulatory action level for the waste to be considered non-
hazardous. What percent of the samples are allowed to be above regulatory action levels
without classifying the waste as hazardous? Chapter 9 of SW-846 recommends utilizing
the student "t" test to determine an appropriate percentage of samples that may be above
regulatory action levels without classifying a solid waste as "hazardous."
Please be aware that the above discussion is only for heterogenous wastes with no
obvious "hot spots" of highly concentrated hazardous wastes. Whenever regulatory
agencies collect samples to determine compliance with the TC regulations, only the most
contaminated media will be sampled. For example, if there is a one-acre mercury waste
pile surrounded by ninety nine acres of clean sand, TC inspectors will not collect samples
of the clean sand.
3-19
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The RCRA definition of "average property" is very different than the definition of
"average" we learned in elementary school. For example, if the TCLP extract regulatory
action level is 50 mg/L, and our sample results are 80 mg/L and 0 mg/L, we can not
compute the numerical average of analytical results as 40 mg/L, and affirm that the waste
is not hazardous. To properly characterize the above waste, we would declare the waste
hazardous because 50% of the samples were above regulatory action levels.
Pages 19-21 Totals Analysis Versus TCLP
Over the past year, the Agency has received a number of questions concerning the
issue of total constituent analysis with respect to the TCLP. Section 1.2 of the
TCLP allows for a compositional (total) analysis in lieu of the TCLP when the
constituent of concern is absent from the waste, or if present, is at such a low
concentration that the appropriate regulatory level could not be exceeded. A
number of persons have contacted the MICE Service and have requested
clarification on this issue with respect to a number of waste testing scenarios.
Wastes that contain /ess than 0.5% dry solids do not require extraction. The
waste, after filtration, is defined as the TCLP extract. The filtered extract is then
analyzed and the resulting concentrations are compared directly to the appropriate
regulatory concentration.
For wastes that are 100% solid as defined by the TCLP, the maximum theoretical
leachate concentration can be calculated by dividing the total concentration of the
constituent by 20. The dilution factor of 20 reflects the liquid to solid ratio
employed in the extraction procedure. This value then can be compared to the
appropriate regulatory concentration. If this value is below the regulatory
concentration, the TCLP need not be performed. If the value is above the
regulatory concentration, the waste may then be subjected to the TCLP to
determine it regulatory status.
The same principal applies to wastes that are less than 100% solid (i.e., wastes
that have filterable liquid). In this case however, both the liquid and solid portion of
the waste are analyzed for total constituency and the results
3-20
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are combined to determine the maximum teachable concentration of the waste.
The following equation may be used to calculate this value:
[AxB + fCxDJJ
= £
B + [20L/kg x D]
where: A = concentration of the analyte in liquid portion of the sample
(mg/U
B = Volume of the liquid portion of the sample (L)
C = Concentration of analyte in the solid portion of the sample (mg/kgj
D = Weight of the solid portion of the sample (kg)
E = Maximum theoretical concentration in leachate (mg/L)
To illustrate this point, the following example is provided:
An analyst wishes to determine if a lead processing sludge could fail the TC for
lead. The sludge is reported to have a low concentration of lead, and the analyst
decides to perform a compositional analysis of the waste instead of the TCLP. A
preliminary percent solids determination as described in the TCLP is performed. The
percent solids is found to be 75%. Thus, for each 100 grams of this waste filtered,
25 grams of liquid and 75 grams of solid are obtained. It is assumed for the
purposes of this calculation that the density of the filterable liquid is equal to one.
The liquid and solid portion of the sample are then analyzed for total lead. The
following data are generated:
Percent solids =75%
Concentration of lead in the liquid phase = 0.023 mg/L
Volume of filtered liquid = 0.025 L
Concentration of lead in the solid phase = 85 mg/kg (wet weight)
Weight of the solid phase = 0.075kg.
The calculated concentration is as follows:
fO.023 mo/L x .025LI + 185 ma/kg x .075kal = 4.18 mg/L
.025 L + [20 L/kg x .075kg]
In this case, the maximum teachable concentration is below the 5 mg/L regulatory
concentration for lead, and the TCLP need not be performed.
Non-aqueous based wastes (i.e., oily waste) may be calculated in the same manner
as described above, except the concentration of constituents from the liquid portion
of the waste (A in the above formula) are expressed in mg/kg units. Volumes also
would be converted to weight units (kg). The final leachate concentration is
expressed in mg/kg unit.
3-21
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This memorandum should significantly reduce the number of TCLP samples analyzed to
demonstrate compliance with the TC regulations. The profound regulatory impact of
Notes on RCRA Methods and QA Activities Memorandum #36, pages 19-21 are most
easily comprehended with the following uncomplicated monophasic examples. These
examples explain how the calculations are made and evaluated to determine whether to
analyze the total constituents or perform the TCLP.
Example 1. The TCLP Extract Regulatory Action Level for cadmium is 1 mg/L. A soil
(with no liquid phase) contains 10 mg/kg of cadmium. Is the TCLP required?
The TCLP test for a solid matrix leaches one part of waste with twenty parts of an acetic
acid buffer. Therefore, even if all of the cadmium was leached from the soil to the
solvent, the maximum concentration in the TCLP extract would be 0.5 mg/L.
Consequently, TCLP is not required.
Example 2. The TCLP Extract Regulatory Action Level for cadmium is 1 mg/kg. A soil
(with no liquid phase) contains 100 mg/kg of cadmium. Is the TCLP required?
The TCLP test for a solid matrix leaches one part of waste with twenty parts of acetic acid
buffer. Therefore, if all of the cadmium was leached from the soil to the solvent, the
maximum concentration in the TCLP extract would be 5 mg/L. Consequently, TCLP is
required.
Example 3. The TCLP Extract Regulatory Action Level for cadmium is 1 mg/L. A liquid
with no solid phase contains 0.5 mg/L cadmium. Is the TCLP required?
The TCLP test for a liquid with no solid phase consists of filtration. The filtrate is the
TCLP extract. Therefore, even if all of the cadmium passed through the filter, the
maximum concentration of cadmium in the TCLP extract would 0.5 mg/L. Consequently,
TCLP extraction is not required.
Example 4. The TCLP Extract Regulatory Action Level for cadmium is 1 mg/L. A liquid
(with no solid phase) contains 5 mg/L cadmium. Is the TCLP extraction required?
The TCLP test for a liquid with no solid phase consists of filtration. The filtrate is the
TCLP extract. Therefore, if all of the cadmium passed through the filter, the maximum
concentration of cadmium in the TCLP extract would be 5 mg/L. Since the filtrate equals
the TCLP extract, the waste exceeds the TC level for cadmium and is a hazardous waste.
Therefore, the TCLP extraction is not required.
Specifying Sample Collection Procedures
• The methods and equipment used for sampling waste materials vary with the
physical and chemical properties of the waste materials.
• 40 CFR part 261, Appendix I lists several representative sampling methods.
Unfortunately, for most matrices, selecting representative samples is an extremely
difficult objective.
3-22
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The methods in the above reference are recommended. NO PRIOR APPROVAL BY
EPA IS REQUIRED IF ALTERNATE SAMPLING METHODS ARE USED.
All procedures for sampling should be documented and referenced.
Sample Containers, Preservation, and Storage
Prior to Extraction or Filtration
• No preservatives are added to the initial waste collected for TCLP filtration and
extraction.
• Preservatives used after filtration and extraction are listed in Chapter 4 of this
document.
• If organics are being analyzed, samples must be collected in glass containers with
Teflon lid liners.
• Metals may be collected in polyethylene or glass containers.
• If practical, samples which will undergo ZHE for volatiles should be collected in 40
mL glass Volatile Organic Analysis (VOA) vials with Teflon lids. Clay type soil
samples, or other large particle size solid matrices which are difficult to put into
narrow-mouth containers, should be collected in 250 mL wide mouth glass jars.
• Any sample which will undergo ZHE should be collected with minimal head space in
the container.
• All samples should be stored at 4 "C ^2'C prior to extraction or filtration. Samples
should be placed in coolers immediately after collection.
Sample Volumes
• A minimum of 100g of waste is needed to determine the % solids, extraction fluid
type, and particle size.
A discussion of required sample volume is presented in Chapter 4.
• A second aliquot of 100g is the minimum which must be extracted for non-
volatiles. The amount of sample is dependent on the percent solids. The lower the
percent solids, the greater the sample volume required for leaching.
• Another aliquot of at least 25 g must be used for volatiles by ZHE. The amount of
sample is dependent on the percent solids. The lower the percent solids the more
material which must be collected for leaching.
• If multiple phases are collected and the solids appear to be _<.0.5%, each phase
may have to be analyzed individually. This is especially true of oily waste. If the oil
will not pass through the filter, it will be considered a solid.
3-23
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• Enough sample must be collected to allow for the Matrix Spike. Each matrix
requires a spike. The same amount of material is required for the spike as for the
sample.
• Extra sample volume may be needed if vessel leakage or breakage occurs. Multi-
phasic samples require much larger sample volumes than monophasic samples.
Sampling Equipment Decontamination
Acceptable sampling equipment decontamination should be performed before sample
collection. Decontamination may be required in the field if adequate sampling equipment is
not available.
Each EPA region and some states have special decontamination requirements. These
decontamination requirements should be verified for compliance in a particular region or
state. The RCRA decontamination procedures may differ from CERCLA decontamination
procedures in some locations. For most TCLP sampling events, there are no sampling
equipment decontamination criteria.
Paint or coatings on sampling equipment must be removed from any part of the equipment
that may contact the sample.
The USEPA Region II decontamination procedure for CERCLA sampling and RCRA RFI
sampling is as follows:
a. wash and scrub with low phosphate detergent
b. tap water rinse
c. rinse with 10% HNO3, ultra pure
d. tap water rinse
e. an acetone only rinse or a methanol followed by hexane rinse (solvents must be
pesticide grade or better)
f. thorough rinse with demonstrated analyte free water*
g. air dry, and
h. wrap in aluminum foil for transport
* The volume of water used during this rinse must be at least five times the volume
of solvent used in Step e.
If metal samples are not being collected, the nitric acid rinse may be omitted. If organic
samples are not being collected, the solvent rinse may be omitted.
Holding Times for TCLP
• TCLP has three sets of holding times. The first holding time commences with
sample collection and ends with TCLP extraction. The second holding time, which
is only applicable for extractable organic compounds, is from TCLP extraction to
preparative extraction. The final holding time is from preparative extraction to
analysis.
3-24
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The following table is from the November 24, 1992 Federal Register. In the table,
pesticides and herbicides are deemed semivolatiles.
Table 3-1 - TCLP Holding Times
Analysis Type
Volatiles
Semivolatiles
Metals, except
Mercury
Mercury
Days From Field
Collection to
TCLP Extraction
14
14
180
28
Days From TCLP
Extraction to
Preparative
Extraction
NA
7
NA
NA
Days From
Preparative
Extraction to
Determinative
Analysis
14
40
180
28
• Some regional and state agencies may alter these times. If CLP methods are used,
the holding times from extraction to preparation and from preparation to
determinative analysis will differ from the above times. However, to demonstrate
compliance with the TC or Land Ban regulations, sample holding times may not
exceed the holding times listed in the preceding table.
Field QC Samples
The following field QC samples may be collected during the sampling process:
• Trip Blanks are aliquots of analyte-free water brought to the field in sealed
containers and transported back to the lab with the sample containers. Trip blanks,
which are only analyzed for volatiles, are especially useful when aqueous volatiles
are collected. Trip blanks allow one to assess contamination from transport and
storage.
• Equipment Blanks are analyte-free water which is poured over the sampling
equipment in the field after the final rinsing of equipment. Equipment blanks allow
one to assess cross contamination and decontamination procedures.
Several key issues must be understood when evaluating the need for equipment
blanks. Equipment blanks are analyzed for total constituents while waste
undergoes extraction. The TCLP leaching process uses 20 grams of leaching fluid
per gram of wet weight sample. Therefore, TCLP equipment blanks may not be
cost effective for some types of TCLP sampling. However, if sampling is being
done for legal purposes, such as enforcement actions or potential litigation,
equipment blanks should be collected to assure that the data are legally defensible.
• The frequency of these samples varies, and depends on the different types of
waste collected, the time over which they are collected, and the regulatory
requirements.
3-25
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• Field Duplicates are samples collected from the same location and waste source at
the same time. The goal is to determine variability in the waste or sample matrix.
The frequency of these depends on the sampling design. Most agencies
recommend at least 5%. Duplicates provide information about sampling and
analysis precision.
• Laboratory Duplicates are samples which have sufficient volume to allow the
laboratory to homogenize the sample, split the sample and prepare and analyze both
aliquots as separate samples. The purpose is to assess precision between two
laboratory analyses on the matrix.
• Enough sample volume must be collected for the lab to generate matrix spikes and
laboratory duplicates.
Sampling Documentation
• All sample locations should be identified in a log book. Locations should be from a
surveyed point when applicable. Both horizontal and vertical points should be
documented.
• The sample numbers, collector, date and time of collection, container types, matrix
and analysis required (including TCLP and the extract/filtrate analysis) should be
documented in log books and on sample labels.
• In most cases, a chain of custody (COC) form should be used to document the
collection and transport of the samples to the laboratory. The chain of custody
form should be signed and dated by individuals who collect, transport or receive the
samples. Copies of COCs should be kept by sending and receiving parties.
• Any deviations from the sampling plan should be documented in the log books.
• The type of sampling equipment utilized must be documented in the log book.
• Ambient weather conditions at the sampling location(s) should be documented in
the log book.
3-26
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o
m
;o
•u
-------
Chapter 4
OVERVIEW OF THE TCLP METHOD
Preliminary Sample Preparation
Leaching Procedure for Nonvolatiles
Leaching Procedure for Volatiles
TCLP Method QC
-------
4.0 OVERVIEW OF THE TCLP METHOD
This chapter provides an overview of the method. Appendix I of this document
includes a copy of the method and Appendix IV provides worksheets which will
be useful in understanding method calculations. The following topics are
covered in this chapter:
• Preliminary sample preparation for leaching
• Leaching procedure for nonvolatiles
• Leaching procedure for volatiles
TCLP method QC
4-1
-------
4.1 Preliminary Sample Preparation for Leaching
Prior to performing the leaching procedure, several preliminary determinations
must be made. These include:
• Are there enough solids present for the leaching process?
• Is particle size reduction required?
• Are immiscible liquids present?
• Which leaching fluid should be used for non-volatile analytes?
Figure 4-1 outlines a flow chart which delineates preliminary determinations. The first step
is to take 100g of the waste, pass it through a 0.6 to 0.8 um filter up to 50 psi and
determine the percent solids. If the percent solids are greater than or equal to 0.5% on a
dry weight basis, the solid must be leached. Any material which remains in the filtration
apparatus is considered a solid. When liquids remain on the filtration apparatus because
they are too viscous to pass through the filter, they are treated as solids. Any material
which passes through the filter is the filtrate and considered a liquid. Therefore, viscous
oils which do not pass through the filter are classified as solids. Oily waste will be
discussed further at the end of this document. If the percent solids are less than 0.5%,
the filtrate is the TCLP extract, and the laboratory analyzes the filtrate.
Particle Size
If the percent solids is > 0.5%, the laboratory analyst must determine whether particle
size reduction will be required.
• The requirement is NOT to measure the size. However, the surface area and
particle size must conform with one of the following criteria:
The solid must have a surface area per gram of material equal to or greater
than 3.1 square centimeters.
The solid must be smaller than 1 cm in its narrowest dimension [i.e. pass
through a 9.5 mm (0.375 inch) standard sieve].
• If the particle size is too large, cutting, grinding, or crushing may be utilized to
decrease particle size.
Choosing the Leaching Solution
Figure 4-1 outlines the determination of the type of leaching fluid for use. If the solid
content is greater than or equal to 0.5%, and if the sample is being analyzed for metals or
semivolatiles, the type of leaching solution must be determined. Note that the leaching
solution determination step requires a smaller (1mm) particle size than the analytical
4-2
-------
method because the leaching solution determination allows much less contact time
between the leaching solution and the sample.
After weighing a 5.0 g subsample of the solid, adding 96.5 ml of reagent water, and
stirring for 5 minutes, the pH is measured. If the pH is < 5.0, fluid #1 is used. If the pH
is > 5.0, 3.5 mL of HCI is added. The mixture is heated to 50'C for 10 minutes and
cooled. If the measured pH is less than 5.0, fluid # 1 is used. If the pH is greater than
5.0, extraction fluid #2 is used.
The heating cycle is a critical step. After the sample has been heated, it should be cooled
to room temperature. The pH must be measured immediately after the sample has
reached room temperature. If the solid waste does not remain in contact with the acidic
solution under specified time and temperature conditions, an erroneous pH may be
measured.
The leaching fluid for all volatiles is fluid #1. Fluid #1 is an acetic acid and sodium
hydroxide solution of pH 4.93 +_ 0.05. Fluid #2 is an acetic acid solution of pH 2.88 _+.
0.05.
4-3
-------
-No-
1
Waste is 100% Solids.
jse Extraction Fluid
. pH =4.93
Does 100 g of waste
yield liquid when
pressure filtered
(50 psi)?
Figure 4-1
TCLP Preliminary
Determinations
Yes
Dry solids on filter
to constant weight
determine % solids.
solidsj^O.5%?
Ye
s,
paper
and
Is %
No, ^
liquid™
Solid
Will solids pass 1 mm*
standard sieve for solution
determination?
Yes
Weigh 5.0g solids into 500 ml
beaker or erlenmeyer flask.
Add 96.5 ml reagent water.
Cover and stir vigorously for 5
min. Measure and record pH. Is
pH < 5.0?
-Yes
-Yes
Sample filtrate. No
further preliminary
tests are needed. Go
to start of Figs. 4-2
or 4-3 for
preservation,
combination with
Jeachate and storage.J
Crush, cut or grind
solids to pass a 1 mm*
sieve.
Add 3.5 ml 1 N HCI, mix,
cover, heat to 50C for 10
min. Cool. Measure pH.
Is pH<5.0?
*Note 1mm size is
used only for
determination of
leachate solution.
3.1 sq. cm or 1cm
diameter is used to
determine need for
size reduction.
No
Use Extraction fluid
#2. pH=2.88
-------
4.2 Leaching Procedure for Nonvolatiles
The nonvolatiles include semivolatiles, which are also called base, neutral, and
acid extractables (BNAs), pesticides, herbicides, and metals. If the percent
solids exceeds 0.5%, the solid is leached with the appropriate extraction fluid
after any required particle size reduction. The following topics are discussed in
this section:
• Determination of extraction fluid weight
• Sample and QC sample volumes
• Extract volumes required
• Issues when dealing with multi-phasic waste
• Initial filtrate versus TCLP leachate
The non-volatile extraction or leaching process is outlined in Figure 4-2. The extraction
process includes placing the appropriate fluid in the bottle extraction vessel for 18 _+. 2
hours and filtering the extract for subsequent analysis. The bottle extraction vessel is
described in Section 4.2.2 of 40 CFR Part 261 Appendix II, which is Appendix I of this
document. In order to generate scientifically valid and legally defensible data, appropriate
weights of environmental samples and leaching fluids must be used.
4-5
-------
Figure 4-2
Nonvolatile Extraction
Complete preliminary
determinations, Figure 4-
Sample is 100%
solids.
Weigh out at least
lOOg of sample.
±
Multiphase sample. Filter a weighed
amount of sample to produce enough
solids which, when extracted, will
create sufficient extract for all
analyses. (100g minimum.) It may be
necessary to perform % solids on
exact sample used for this extraction
due to subsampling error.
I
Solid
T
Solids are£0.5%of
sample. Filter
enough sample to
provide for all
analyses. Discard
solids. Filtrate =
TCLP extract.
If particle size reduction is needed,
decrease size until waste solids will pass
a 9.5mm sieve (3/8")
Liquid
Phase
Quantitatively transfer solids to an
extraction vessel. Include filter used to
separate phases if sample was
multiphasic
Add an appropriate amount of extraction
fluid to the extraction vessel. (Fluid weight
=20 x solids weight)
Close extraction vessel using Teflon tape
and secure in rotary agitation device.
Rotate at 30 + 2rpm for 18 +2hrs. Ambient
temperature of extraction room shall be 23
±2°C.
Filter slurry through glass filter fiber (acid
wash if metals are measured). Several
filters may be used. Discard solids. Collect
filtrate.
Analyze liquids
separately and
combine results
mathematically
according to
volume ratio of
original phases.
Is filtrate miscible
with initial filtered
liquid if sample was
multiphase?
Re
* St
V r r fe
Main filtrate.
ore at 4 °C.
\
r
Combine initial
liquid with
filtrate. This
becomes the
TCLP extract.
7
Immediately after TCLP extract is produced,
record the pH of the extract. (For immiscible
liquids, record the pH of each.)Aliquot and
preserve the extract. Unless analyzed
immediately, store aliquot at 4 °C until analyzed.
4-6
-------
Determination of Extraction Fluid Weight
The following formula is used to compute the required weight of TCLP extraction fluid:
Weight of Extraction = 20 x %Solids x Weight of Waste Filtered
Fluid 100
The amount of extraction fluid required per extraction is 20 times the weight of filtered
solids used in the extraction.
A minimum of 100g of waste material must be filtered to generate the solids utilized in the
extraction. If the sample is 100% solids, a minimum of 100g must be used in the
extraction. When aqueous environmental samples contain between one-half and ten
percent solids, several kilograms of sample are required for analysis.
Sample and QC Sample Volumes
The generation of sufficient extract volume to perform all analysis is critical.
• The required volumes vary with the laboratory. CHECK WITH THE LABORATORY
FOR ACTUAL VOLUMES.
• Depending on which metal analytes are selected, two or three digestions may be
required.
• If matrix spikes or duplicates are performed, additional volume will be required.
Labs may charge additional fees for these QC samples.
Table 4-1 Volume of Extract Required for One Nonvolatile Analysis
Analysis Type
BNA
Chlorinated Pesticides
Herbicides
Metals
Volume of TCLP Leachate Typically
Required per Test
1 L
1 L
1 L
300 mL/digestion
The previous table outlines the "typical" volumes of extract or total leachate required for
non-volatile analysis. THESE VOLUMES MAY VARY WITH THE LABORATORY. IT IS
IMPERATIVE THAT YOU CHECK WITH THE LAB AS TO THE AMOUNT OF WASTE
REQUIRED FOR THEIR ANALYSIS PROCESS. The amount of waste varies with the
percent solids. The lower the percent solids, the more waste will be needed for TCLP
preliminary and final testing. If the waste sample is a filterable liquid with less than 0.5%
solids, the volume listed in the previous table can be used as a guide for the minimum
volume needed for the analysis.
4-7
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Issues When Dealing with Multi-phasic Waste
• Subsampling stratified waste is difficult. Therefore, the analyst should consider
calculating percent solids from the same sample container used for the TCLP
extraction instead of compositing all the sample containers. This is the largest
source of error in the TCLP leaching process. The laboratory must consider the
amount of each phase present in each bottle and adjust the calculations
accordingly.
• The particle size of multi-phasic material may be difficult to assess. The lab should
identify procedures to classify multi-phasic samples which are not amenable to size
measurement.
• Five grams of sample are usually used to determine the appropriate TCLP leaching
fluid. If there is not enough volume of any individual phase, less material may be
used.
• The pH of the filtrate should be recorded. This provides useful information when
validating field or laboratory duplicates.
• The filtrate volume should also be measured. This information will be needed if the
multiple phases must be mathematically combined.
Initial Filtrate Versus TCLP Leachate
Two liquids are generated when a multi-phasic waste is analyzed.
• Initial filtrate
• Leachate
• If the filtrate is miscible with the leachate, the two solutions are mixed prior to
analysis.
• If the two solutions are not miscible, they are analyzed separately, and the results
combined mathematically.
The mathematical calculations are performed via the following equation if the TCLP filtrate
and extract are not miscible.
Final analyte = (V1) (CD + (V2) (C2)
Concentration V1 + V2
where:
V1 = The volume of the first phase (L).
C1 = The concentration of the analyte of concern in the first phase (mg/L).
V2 = The volume of the second phase (L).
C2 = The concentration of the analyte of concern in the second phase (mg/L).
4-8
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After generating the TCLP extract, the pH of the extract should be recorded. If the filtrate
and TCLP extract are mixed, record the pH of the mixture as well as the original TCLP
extract and filtrate. The TCLP extract or filtrate/extract mixture should be aliquoted for
each analysis. The metals aliquot should be preserved to a pH<2 with nitric acid. Adjust
the pH of a small portion of the TCLP extract or mixture prior to adjusting the entire metals
aliquot. If a precipitate forms, do not adjust the pH of the sample extract. If nitric acid is
not added, the sample should be analyzed as soon as possible after TCLP extraction.
Metals analysis must include digestion prior to analysis. Aliquots for BNAs, herbicides and
pesticides do not require preservation. All aliquots must be stored at 4*C ±2'C prior to
analysis.
Example
The following example demonstrates how to calculate the weight of extraction fluid
required to perform a TCLP extraction. In this example, the environmental sample contains
40% solids. Only metals will be analyzed since the waste is from a metals finishing shop.
In order to determine the total amount of waste required to generate 100g of solids, the
following equation is used:
Amount of multi-phasic material = (10000)/ (weight percent wet solids)
If 100g of original waste yields 40g of solid, the total amount of waste required to
generate 100g of solid is 250g.
250g of total waste required = 10000/40
Using the equation in 40 CFR Part 261, Appendix II Section 7.2.11, which is Appendix I of
this document.
Weight of extraction = 20 x % solids x weight of waste material filtered
fluid 100
20 x j40 x 250g = 2,000g of extraction fluid
100
Labs typically assume a density of 1 g/mL for the extraction fluid. Also, note that 40% is
used not 0.40, for the percent solids. Since 300 mL of extraction fluid is required for one
complete metals digestion, using 250g of the multi-phasic waste will provide enough
volume for the metals analysis. This allows enough volume to analyze one matrix spike.
The use of matrix spikes will be discussed in the QC section of this chapter. The matrix
spike sample size requirement is the same as for original environmental sample analysis.
If organic analysis were required, at least three times as much waste would have been
used in the TCLP extraction. For matrix spikes analyses, a triple volume of TCLP leachate
will be required. The terms analytical batch and waste type are not defined in the TCLP
regulation. Most methods, including CLP and SW-846, indicate that a batch is the number
of samples processed through preparation and analysis simultaneously, and should not
exceed 20 samples of the same matrix. Most methods require that matrix spikes and
matrix spike duplicates (MS/MSD) for organics be performed at 1 MS/MSD per processed
batch, with a batch containing no more than 20 samples.
4-9
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4.3 Leaching Procedure for Volatiles
Volatile organics are leached using different equipment than nonvolatiles.
Figures 4-3 and 4-4 are the flow charts describing the volatile leaching procedure using the
Zero Headspace Extractor (ZHE). The ZHE must be used when leaching volatiles. In order
to minimize evaporation of volatiles, the volatile leaching procedure is performed on a
separate aliquot of waste. The aliquot should be stored in a 40mL VOA vial when
feasible. Due to the small width of the vial and the low volume, multi-phasic and oily
wastes may be stored in larger glass containers prior to leaching. Once the percent solids
has been determined in the preliminary sample preparation phase, a second aliquot of the
liquid is used to generate the volatile analysis extract. In all cases, no more than 25g of
solids should be placed in the ZHE because the total volume of the ZHE is 500-600 ml_s.
In order to prevent the loss of volatile compounds, heating or excessive sample
manipulation must be kept to a minimum. The samples and equipment used in the process
should be cooled to 4'C when possible to prevent loss of volatiles.
If the sample contains less than 0.5% dry solids, the filtrate is defined as the TCLP
extract. The solid is discarded in this instance. The filtrate is collected in either a Tedlar
bag or a glass syringe which is described in the equipment section of the procedures in
Appendix I of this document. This filtrate becomes the TCLP extract.
Weight of Waste Charged to the ZHE
If the solids are > 0.5% dry solids, the material must be extracted.
If the solids are > 0.5% and < 5.0 %, a 500 g subsample
of the waste is weighed and recorded.
If the solids are > 5.0%, the following formula is used to determine the
amount of waste to place in the ZHE:
Weight of Waste = 25 x 100
Charged in ZHE Percent wet solids
If the solids are greater than 0.5% and the sample is multi-phasic, any solids must be
examined for particle size prior to filtration. The sieve is NOT used to verify particle size
for the volatile sample. Particles are measured with a ruler and should be less than 1 cm
diameter. Any particle size reduction should be done with minimal exposure to air and
without heat production. All apparatus used in this process should be cooled to 4*C.
4-10
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Figure 4-3
Volatile by Zllli
(Complete preliminary
solids determination, Fig.
4-1
Solids are <0.5%of
sample. Filter sufficient
sample through ZHE to
provide for all analysis.
Discard solids. Filtrate =
TCLP extract.
Store at 4 °C under
minimal headspace and
analyze.
4-No
Is the amount of filterable solids.;? Q.5%?
Yes
Place the ZHE piston in body of the ZHE
and adjust position of piston to minimize
distance piston will travel when charged
with sample
Solids are >5%.
Weigh (2500 / %
solids).
Adjust particle size of solids, if necessary, so size is <1
cm in its narrowest dimension. DO NOT SIEVE,
measure with ruler. Adjust without heat production and
with minimal air exposure.
Quantitatively transfer sample quickly to ZHE. Secure
filter and support screen to top flange and attach top
flange to body of ZHE. Tighten all fittings. Place
vertically with gas inlet/outlet valve down.
• Yes-
Does sample contain liquid phase?
—No
Attach the gas line, open the
gas inlet/outlet valve and apply
gentle pressure (1-10psi) to
force all headspace form ZHE.
When liquid first appears, close
liquid inlet/outlet valve and
discontinue pressure.
T
Liquid Phase
T
Sample is 100% solids. Attach
gas line to gas intlet/outlet
valve, open liquid inlet/outlet
valve, and gradually apply
pressure in 10 psi increments
until 50 psi is reached.
Attach pre-weighed filtrate
collection container to liquid
inlet/outlet valve. Open liquid valve
and gradually apply pressure in 10
psi increments until 50 psi is
reached. After no further liquid is
expelled after 2 minutes at 50 psi,
close valves, disconnect and
weigh filtrate collection container.
Solid k
-Phase~
Add an appropriate weighed
amount of extraction Fluid #1 by
pumping in through the liquid
inlet/outlet valve. (Fluid weight = 20
x solids weight)
Store filtrate at 4 °C under minimal
head space. See Fig. 4-4.
Rotate ZHE end-over-end 2 or 3 times.
With liquid inlet/outlet valve pointed
up, pressurize ZHE to 5-10 psi, and
bleed off any air which might have
been introduced with the extraction
fluid. Close the liquid inlet valve and
pressurize to 5-10 nsi again
Connect preweighed
filtrate/extract collection
container to liquid i/o valve.
Apply up to 50 psi in 10 psi
increments. See Fig.4-4.
Place ZHE in rotary device and
rotate at 30 ± 2rpm for 18 ± 2 hrs in a
room held at 23± 2° C.
Check pressure in ZHE by
quickly opening and closing
the gas inlet valve. Is
pressure present?
-No*
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Figure 4-4
Volatiles by ZHE Continued
Store initial filtrate at 4 °C under
minimal head space. See Fig. 4-3.
Analyze liquids
separately and
combine results
mathematically
according to
volume ratio of
original phases.
Connect preweighed
filtrate/extract collection
container to liquid input/
output valve. Apply up to 50
psi in 10 psi increments.
Collect the extraction filtrate.
See Fig.4-3.
-No —
Is filtrate miscible
with initial filtered
liquid if sample was
multiphase?
-Yes
Combine initial
liquid with
filtrate. This
becomes the
TCLP extract.
Store at 4 °C under minimal head space
prior to analysis.
4-12
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Any liquid waste which remains in the ZHE after reaching a pressure of 50 psi is
considered solid phase and undergoes leaching. Any liquid which is removed during
filtration is considered liquid phase filtrate. The filtrate is captured in either a Tedlar bag or
glass syringe. The solids are leached with fluid #1.
If the percent solids is 100%, a 25g sample of the solid is placed in the ZHE after any
necessary particle size reduction, if required, is performed. The particle size reduction
follows the same protocol requirements as volatile extraction of waste with solids content
greater than 0.5% but less than 100%. The extraction is similar to the TCLP extraction of
multi-phasic material.
When performing TCLP extraction for volatile analysis, extraction fluid #1 is always used.
The quantity of extraction fluid is 20 times the solid weight used in the extraction.
The extraction is performed by placing the ZHE in the rotary agitator at 30 _+. 2 rpm for 18
±2 hours. The ambient temperature is maintained at 23 _+2*C during agitation. At the
end of the agitation period, the ZHE piston pressure must be measured to verify that
pressure was maintained during the extraction. If pressure was not maintained, the
extraction must be repeated after the ZHE is examined for mechanical problems. If the
pressure was maintained, the material in the ZHE is separated into solid and liquid phases
by pressure filtration. A small amount of the liquid extract should be examined for
miscibility with the previously captured filtrate. If these fluids are miscible, the liquid
extract and the filtrate may be stored in the same container {Tedlar bag or syringe) with
minimal or no headspace. This mixture becomes the TCLP extract for volatile analysis. If
the two fluids are not miscible, they are stored in separate containers with minimal or no
headspace. The volatile analysis are performed separately and combined mathematically
using the same equation as for the non-volatile analysis. All extracts and fluids are kept at
4'C +_2'C prior to analysis.
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4.4 TCLP Method Quality Control
• TCLP extraction blank
• Method preparation blanks
• Calibration
• Matrix spikes
BIAS CORRECTION IS NO LONGER REQUIRED.
• Method of standard additions
TCLP Extraction Blanks
• A minimum of one TCLP extraction blank is generated for every 20 extractions
processed in a given extraction vessel using the same fluid. Most labs have
multiple extraction vessels. The common industry strategy is to generate one TCLP
extraction blank for each group of samples processed simultaneously using the
same batch of fluid.
Calibration
• Calibration should follow the respective method requirements. Typically a three to
five point initial calibration followed by a single point continuing calibration is
specified.
Method Preparation Blanks
• Preparation blanks performed for a specific analysis should follow the frequency
and requirements of the method. Typical requirements are one per preparative
batch from similar matrix for every 20 samples.
Matrix Spikes
• Matrix spikes are used to monitor the performance of the analytical methods on the
matrix and to assess the presence of interferences.
• A matrix spike shall be performed for each waste type (waste water, soil, etc.)
unless the result exceeds the regulatory level and the data are being used solely to
indicate that the regulatory level is exceeded.
• A minimum of one sample from each "analytical batch" must be spiked. For spike
samples, a double or triple volume of TCLP leachate will be required. The term
analytical batch is not defined in the regulation. Most methods, such as CLP and
4-14
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SW846, indicate that a batch is no more than 20 samples of the same matrix
processed through preparation and analysis simultaneously. Based on this criteria,
the minimal matrix spike frequency of analysis is one per 20 samples. However,
many process batches may include from one to 19 samples and the frequency may
increase with fewer samples processed. Some regions define each type of waste
as a matrix, and require matrix spikes for each matrix.
• Matrix spikes (MS) are to be added after initial filtration but prior to preservation.
Spikes are NOT to be added prior to the TCLP leaching.
• The spike should be added to the same nominal volume of TCLP extract as the
unspiked sample.
• The spike concentration "should" be added at the regulatory level. If the expected
concentration in the sample is as low as half the regulatory level, the spike
concentration can be decreased to half the regulatory level. In all cases, the spike
must be greater than 5 times the method detection limits.
• Matrix Spike Recoveries are calculated by:
%Recovery = 100 ( Measured value for the spiked sample minus
measured value of the unspiked sample)/ known value of the spike
• When the matrix spike recovery falls below the expected analytical performance,
alternate methods of analysis may be required to measure analyte concentration in
the TCLP extract. The matrix spike recovery limits from the Contract Laboratory
Protocol methods are used when the method is used.
If the matrix spike recoveries exceed limits, other analytical methods such as
isotopic dilution may be used to deal with the matrix effects. Typically, the holding
times will be exceeded or near the limits when this occurs. If possible, resampling
of the waste may be required to assure that the appropriate method is used and
holding times are met.
BIAS CORRECTION IS NO LONGER REQUIRED.
Surrogate Spikes
Surrogates are compounds which are not expected to be in the samples but are chemically
similar to those being determined. Surrogates are typically deuterated and are added to
samples analyzed for organics prior to sample extraction or purging. The concentrations
and specific compounds are listed in the appropriate methods. The recovery of the
compounds are monitored with specific criteria either being found in the method or
determined by statistical quality control in the laboratory.
Method of Standard Addition
Four equal volume pre-digestion aliquots of sample are measured and known amounts of
standards are added to three aliquots. The fourth aliquot is the unknown and no standard
is added to it. The concentration of standard added to the first aliquot should be 50% of
4-15
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the expected concentration. The concentration of standard added to the second aliquot
should be 100% of the expected concentration and the concentration of standard added to
the third aliquot should be 150% of the expected concentration. The volume of the
unspiked and spiked standard should be the same.
In order to determine the concentration of analyte in the sample, the analytical value of
each solution is determined and a plot or linear regression performed. On the vertical axis
the analytical value is plotted versus the concentrations of the standards on the horizontal
axis. An example plot is shown in Figure 4-5. When the resulting line is extrapolated back
to zero absorbance, the point of interception of the horizontal axis is the concentration of
the unknown.
Concentration
'Cone, of
Sample
Addn 0
No Addn
Addn I
Addn of 50%
of Expected
Amount
Addn 2
Addn of 100%
of Expected
Amount
Addn 3
Addn of 150%
of Expected
Amount
FI6URE4-5 STANDARD ADDITION PLOT
4-16
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When must Standard Addition be used?
The method of standard additions is used for metallic contaminant determinations if both
of the following criteria are met:
1. The matrix spike recovery from the TCLP extract is less than 50% and the unspiked
sample concentration is less than the regulatory level.
2. The contaminant measured in the sample is within 20% of the regulatory level.
For the method of standard additions to be correctly applied, the following limitations must
be taken into consideration:
• The plot of sample and standards must be linear over the concentration range of
concern. For best results, the slope of the curve should be similar to that of a plot
of the aqueous standard curve.
• The effect of the interference should not vary as the ratio of the standard added to
the sample matrix changes.
Holding Times
As previously discussed in Section 3, the holding times must be met. Data collected on
samples which exceed holding times is not acceptable for establishing that a waste does
not exceed regulatory levels. If the waste exceeds regulatory levels and the holding times
are exceeded, the data should not be invalidated.
4-17
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o
m
50
-------
Chapter 5
DATA VALIDATION AND
DATA DELIVERABLES
-------
5.0 DATA VALIDATION AND DELIVERABLES
This chapter addresses the following questions:
• What is data validation?
• When must TCLP data be validated in EPA Region II?
• Which analytical deliverables are needed to validate TCLP data when
utilizing the USEPA Region II Organic, Inorganic, and TCLP Data
Validation Protocols?
• Which analytical deliverables are recommended for TCLP data which will
not be validated?
• How should these deliverables be utilized to assess data quality and
usability?
5-1
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5.1 Data Validation
What is Data Validation?
"Data validation is a systematic process for reviewing a body of
data against a set of criteria to provide assurance that the data
are adequate for their intended use. Data validation consists of
data editing, screening, checking, auditing, verifying, certifying
and reviewing." (EPA Region II CERCLA QA Manual)
The most important criteria which the data reviewer evaluates are:
1. Holding times
2. Instrument tuning
3. Calibration and retention time windows
4. Blank contaminants
5. Surrogates (a measure of extraction efficiency)
6. Chromatographic performance (baseline, interference, retention time shift and peak
resolution)
7. Emission interferences or spectral interference from other elements when reviewing
metals data
8. Calculations
9. Transcription of numerical values to the required forms in the data package
10. Matrix effect errors; interference from the sample itself
11. Degradation of compounds during analysis
There is a substantial amount of uncertainty in all chemical data. In addition to lab error,
there are field sampling errors, such as improper decontamination of field equipment, air
bubbles in VOA vials, loss of samples, and failure to ship samples in a timely manner after
collection. Different analytes have varying degrees of uncertainty.
TCLP data are expected to have significantly more inherent error than routine chemical
analysis because additional procedures are performed by the laboratory analyst.
5-2
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What is data qualification?
Qualifying data is a method of notifying the data user that some data have additional
uncertainty. The Region II TCLP data validation protocol qualifies analytical data with the
following flags:
• R Rejected (unusable)
• J Estimated
• UJ Estimated detection limit
• N Presumptively present (cannot positively identify an analyte)
• JN Presumptively present at an estimated concentration
The above qualification "flags" provide QC information to the data user. The Region II
TCLP data validation protocol qualifies analytical data as unusable, estimated,
presumptively present, or presumptively present at an estimated concentration.
Unusable data are rejected and qualified with an "R". When data are rejected, it doesn't
mean that the analyte wasn't there - it means that either the test was not correctly
performed or that the test was not appropriate for the matrix. Examples of reasons for
rejecting data include: poor calibration, low surrogate recoveries, and air bubbles in
volatile sample vials. If the data are needed, resampling and reanalysis must be
performed. For example, the holding time for TCLP VOAs is 14 days from sampling until
TCLP leaching, and then 14 days until analysis. If a sample is held for 30 days from
collection until leaching, all non-detects and positive results below regulatory action levels
will be rejected because analytes could have been present above regulatory action levels.
Results above the regulatory action levels would be accepted. However, the site owner
may still want resampling and reanalysis to assure that a false positive did not occur.
When data are qualified as estimated with a "J", it means that the data .should be used
with caution. The data could be significantly imprecise, and the reported value given is
little more than an estimate. Estimated means that the compound is present, but the
exact concentration is uncertain.
When data are qualified with a "UJn, it means that the detection levels are uncertain. For
example, this qualifier would be used when surrogate recoveries in organics are greater
than 10% but not within the method criteria. The "UJ" notifies the data user that the
detection limits are estimated.
When the analyte identity is uncertain, the qualifier "N" is used to indicate that it is
presumptively present. This is used in data validation when a mass spectrum differs
slightly from the required spectral criteria. Data validators use the qualifier "JN",
presumptively present at an estimated concentration, much more often than the qualifier
"N". The"JNn flag denotes both qualitative and quantitative uncertainty. This is typically
used when tentatively identified compounds (TICs) from semivolatile gas
chromatography/mass spectrometry analysis are presented. The concentration and
identities of the TICs are uncertain and are flagged with "JN".
5-3
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When Must TCLP Data Be Validated?
EPA Region II requires TCLP data for RCRA RFIs and many types of CERCLA sampling
events to be validated. The RCRA program does not explicitly require the validation of
routine TCLP analysis of waste materials to determine compliance with TC or LDR
regulations.
Data validation reduces false negatives, false positives, and misquantitation in reported
data. Misquantitation includes both laboratory arithmetic errors, and data qualified as
estimated or presumptively present because of analytical problems. The costs for TCLP
validation are quite variable, and depend specifically on which tasks the data user instructs
the data validator to perform, and the quality of the laboratory analyzing the environmental
samples. The cost of validation of a single sample containing the 39 TC analytes is about
$300-$500 per sample analyzed by a competent laboratory. In addition to the data
validation cost, the laboratory will charge an additional fee, which is estimated at $200-
$400 per sample, for generating analytical deliverables. The more a data user knows about
a specific waste, the less useful data validation becomes. For example, if the data user
knows which raw materials, final products, and by-products are in a waste, and has
historical data that demonstrates that the TC analytes in the TCLP extract are far below
regulatory action levels, TCLP validation would not be cost effective. Alternatively, when
the data user has very limited knowledge of a waste's characteristics, decisions based on
that data can result in significant disposal cost for management. Therefore, many
businesses believe that it is prudent and cost effective to validate this type of TCLP data.
Some regulatory agencies, especially in the CERCLA program, do not allow laboratories to
validate their own data. All laboratories review their own data for contractual compliance
and analytical problems. Unfortunately, this assessment of contractual compliance may
also be called data validation. Many laboratories now call their contractual compliance
review "data review" to differentiate this review from data validation.
Contractual compliance is NOT the same as data validation. A lab can contractually fail
and still produce technically valid data. An example of this occurrence is when contractual
requirements for metals data indicated that results would be delivered to the client 40
days from receipt of the sample. If the laboratory did not deliver for 60 days, the
laboratory failed the contract criteria, but the technical criteria were still met.
Alternatively, a laboratory can contractually meet criteria but produce data which is not
useable.
In order to validate TCLP data, the following must be ascertained:
• Are any specific data validation protocols required by a regulatory agency?
• What are the regulatory action levels?
The TC regulatory action levels are listed in Table 1. The Land Disposal Restrictions
regulatory action levels are listed in Appendix II.
The EPA Region II TCLP, Inorganic and Organic Validation protocols are included in
Appendix V. If your region or state does not have a TCLP validation procedure, the Region
II data validation protocol could be used. If the applicable sampling and analysis plan
5-4
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requires regulatory approval, the data user, lab and regulator must agree on validation
criteria prior to sample collection.
Phenols
When validating TCLP phenols, the TCLP extraction fluid may cause a matrix effect. This
matrix effect may lower surrogate and matrix spike recoveries for phenols. As long as the
matrix spike and surrogate recoveries are above 10%, the data should not be rejected.
After determining whether the project will require validation, the appropriate deliverables
must be specified to allow the validation to occur. For example, if the validation requires
calibration verification, raw instrument calibration data must be present for the validation
to be performed.
5-5
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5.2 Data Deliverables
General TCLP Data Deliverables
In order to validate and assess TCLP data, appropriate deliverables must be
specified. Deliverables will differ depending on whether validation is required.
These analytical deliverables must be specified before samples are collected.
The following topics are discussed:
• Deliverables when no validation is required
• Additional deliverables which may assist in review
• USEPA Region II analytical deliverables
• Specifying data deliverables
Deliverables When No Validation is Required
When TCLP data are not validated, we recommend that the laboratory furnish the data
user the following deliverables:
1. Sample description and sample identification numbers.
2. Analytes, concentrations, and units.
3. Level of contaminant(s) in method and TCLP blanks.
4. Matrix spike, QC check sample when applicable, and surrogate recoveries.
5. A description of matrix problems and analytical problems observed during analysis,
and an assessment of how those problems will affect data usability.
6. A certification that samples were analyzed within method holding times (from the
date of sample collection). This certification must include the sampling date, TCLP
extraction dates, preparatory extraction dates, and analysis dates.
The laboratory staff are not always familiar with data validation protocols or with data
usability on a project specific level. Therefore, in addition to information about the QC
supplied by the laboratory, it may be beneficial to work with a specialist in this area.
Some firms specialize in validating and assessing data quality.
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Additional Deliverables Which May Assist in Review
While the data is the key factor, some information is not always captured in the analytical
result. For example, if a procedure is modified due to a matrix problem, the procedure
must be documented and the validator provided this information. The following
information may facilitate validation.
• Chain of Custody records
• Analytical procedures used by the laboratory
• An example of a data calculation
The data user must specify the information (analytical deliverables) desired from the
laboratory. If this is not done, only the final result, or the final result plus a QC summary,
will be provided.
Region II Analytical Deliverables
The following TCLP analytical deliverables are required by the Region II TCLP data
validation Protocol:
1. The TCLP and preparative extraction dates and analyses dates.
2. Selection of extraction fluid data.
3. A physical description of the samples.
4. The sample weights and the extraction fluids weights.
5. The final volume of TCLP extract and the volume of extract analyzed.
6. The data used to compute percent dry solids and the weight of the liquid phase (if
applicable).
7. Extraction logs for each sample, indicating the volume and pH of acid added. Were
inorganic sample extracts properly preserved?
8. A description of the materials of construction for extraction vessels, filtration
devices, and ZHE extraction devices (i.e. glass, Teflon, PVC, stainless steel, etc.).
9. The data used to compute TCLP extract concentrations for multi-phasic samples.
10. When VOA samples consist of oily waste that cannot be filtered, describe how the
TCLP aqueous extract is separate from the oily waste.
11. A copy of the sampling log or trip report.'
12. Any evidence of leakage in the ZHE device.
"Item 11, which requires the presentation of the sampling log, may not be available from
the laboratory. The sampling team may supply this information.
In order to facilitate analysis and validation. Associated Design and Manufacturing
Corporation and Dr. Larry Jackson have developed work sheets (Appendix IV) which may
be used by the analytical laboratory to generate the above listed analytical deliverables.
5-7
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Specifying Data Deliverables
EPA Region II requires TCLP data to be validated for RCRA RFIs and many types of
CERCLA sampling events.
When validating TCLP data to demonstrate compliance with the TC regulations, Region II
recommends using CLP methodology and analytical deliverables. However, specific
regulations such as Land Ban as noted in Chapter 2 and Appendix X require SW-846. SW-
846 methods cannot be validated by CLP validation criteria because SW-846 methods do
not specify analytical deliverables, and have different QC criteria than CLP methods.
Therefore, validation protocols must be prepared for non-CLP methods such as those in
SW-846.
For non-CLP methods, data validation criteria must include:
• Holding times for sample preparation and analysis
• Preparation logs
• Calibration
• Method and instrument blank data review
• Calculations
• Matrix spike data
• Duplicate results
For organic analysis the following additional items must be included:
• Instrument tuning if GC/MS is used
• Surrogate recoveries
• Chromatographic performance ( baseline, interference, shift and peak resolution)
• Mass spectral interpretation or compound identification
For metals analysis the following additional items must be included:
• Whether method of standard addition or serial dilution were needed and performed
correctly. The November 24, 1992 modification to the TCLP procedure mandates
the use of method of standard additions under certain circumstances.
• Post digestion spike recoveries versus pre-digestion spike recoveries.
• The frequency of analysis of QC samples must be validated.
5-8
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7)
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Chapter 6
ANALYZING AND ASSESSING MULTI-PHASIC
AND OILY WASTES
Definition of Oily Waste
Problems/Issues
Suggestions
Most Commonly Asked TCLP Question
Analytical Options
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6.0 ANALYZING AND ASSESSING MULTI-PHASIC AND OILY WASTES
Analyzing and Assessing Multi-Phasic and Oily Wastes
This chapter provides strategies which may be beneficial in characterizing oily
wastes. There is no single correct method to analyze these wastes.
• Definition of oily waste
• Problems/Issues
• Suggestions
• Most commonly asked TCLP question
• Analytical options
This chapter outlines the current issues and difficulties in performing TCLP on multiple
phase and oily waste. This chapter is not meant to provide unequivocal answers, but to
provide suggestions and strategies which may be successful. There is no single correct
method in dealing with these materials. The initial discussion in this chapter provides
references and information indicating that EPA understands the difficulties in applying the
TCLP to multi-phasic and oily wastes. Subsequent discussions summarize possible
strategies which may be used in leaching and analysis.
6-1
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6.1 Definition of Oily Waste
Appendix VI contains several papers presented at the EPA's 1992 Waste
Testing & Quality Assurance Symposium Work Shop on oily waste. The
following is Clifford Marquis's of BP Research, definition of oily waste (see
Appendix VII):
Although it is nearly impossible to precisely define the term "oily
waste", the following analysis can provide a basis for further discussion:
a) An oil is generally an immiscible or relatively insoluble
liquid, varying in composition but consisting of organic
constituents. Petroleum oil principally consist of hydrocarbons;
vegetable and animal oils are glycerides, and fatty acids; and
essential oils are terpenes, alkaloids, etc.
b) An oily waste is an industrial process waste or residua/
bearing oil in a visual and/or measurable proportions.
c) Oil in oily wastes can occur in any matrix, including:
sorbed to dry solids; in sludges or slurries; multi-phasic liquids or
sludges/slurries with multi-phasic liquids, if water is present.
Proper treatment and disposal of all such matrices is a concern of
the petroleum industry.
d) Oily wastes possess a wide variety of compositions and
physical and toxicological properties.
6-2
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6.2 Problems/Issues
Problems with the TC Model
• The model does not differentiate between oily and aqueous liquids.
• The model assumes a person drinks 2 liters a day of well water for 70
years. This assumption is not applicable for oily wastes.
• The disposal scenario depicted by EPA is not an accurate description of
today's practices. For example, liquids are no longer accepted in
municipal landfills.
c The model does not correct for absorption of oily waste on soils. Oil
may also adhere to other landfill matrices instead of mixing with the
aqueous phases.
The difficulty in analyzing oily wastes by TCLP may be categorized as modeling, analytical
and regulatory problems.
The Leachability Subcommittee of the EPA Science Advisory Board's Environmental
Engineering Committee has published its recommendations. A copy of this report is in
Appendix VIII of this document. This document outlines the properties of an optimum
leach test.
Issues with Oily and Multi-phasic Waste and TCLP
• It is difficult to separate the phases.
• Volatiles may evaporate during handling.
• The tumbling action of the two liter extraction vessel can form emulsions which are
difficult to separate.
• The oily material may obstruct the filter. When this happens with the ZHE, the test
must be repeated.
o Oily materials often yield oil and aqueous leachate which must be analyzed
separately. This increases costs and time of analysis.
o The method requires determination of dry weight percent solids. When the "solid"
is actually oil or organic, drying can be hazardous and inappropriate. It may be
impossible to achieve a constant weight when performing a percent solids
determination.
6-3
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When multiple phases and multiple bottles are used in sampling, each container will
show different amounts of each phase.
It may be impossible to separate solids from oil. If volatiles are analyzed, additional
sample manipulation to remove solids will result in loss of volatiles.
6-4
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6.3 Suggestions
Suggestions for performing TCLP extractions on oily wastes include the
following:
Planning
Regulatory approval
Separate phases for analysis
Documentation of phase type and volumes
As previously indicated, these are suggestions. There are no consistently and absolutely
appropriate methods when performing TCLP extractions on oily wastes.
• Planning is more critical when oily or multi-phasic samples are collected and
analyzed. Discuss the sample matrix with the laboratory before collecting samples.
• Once an approach is formulated, regulatory approval may be needed. This approval
is of greater importance if deviations from the TCLP extraction method are required
due to the matrix.
• If two liquid phases are present, each phase should be separated and analyzed
individually.
o The SW-846 Methods specify several procedures for analyzing oily waste. BNA
methods include 3580B for preparation followed by 8270B. The pesticides method
includes 3580B using hexane as the extraction solvent followed by 8080B. The
VOAs are analyzed by 8240B. Metals can be prepared by method 3040B and
analyzed by appropriate analytical methods.
• The number, appearance, and volume of each phase should be documented before
collection of the sample. The phase volume can be estimated by measuring the
height of the phase in the container and the diameter of the container. This
information can be used to estimate the amounts of material available for testing.
• Phase volume should be estimated after sample collection and prior to analysis.
• In multi-phasic liquid samples, the relative density of each phase should be
documented.
. When multiple containers of multi-phasic waste are received, each container will
have different amounts of each phase. If multiple sample containers are collected
6-5
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and each container is multi-phasic, the number, appearance, volume and relative
density should be documented for each container.
If regional and state regulators will allow, one container can be mixed and analyzed.
By knowing the volumes in the other sample containers, the total composition can
be mathematically calculated.
If one phase is organic and contains <.5% solids, this may be directly
characterized by the appropriate analytical method after filtration without TCLP
extraction.
Subsampling increases the possibility of sampling error.
The percent solids should be determined in multi-phasic samples before filling the
ZHE. This prevents overfilling the ZHE.
The TCLP method requires drying the solids at 100*C +_ 20'C to determine percent
dry solids. This may not be achievable for organic multi-phasic material because of
safety considerations. If this cannot be done, the reason should be documented.
The percent wet solids is used to calculate the weight of extraction fluid. If this
occurs, the lab should discuss this with the client prior to using the percent wet
solids as the solids content. This will greatly effect the final analyte
concentrations.
Particle size reduction is difficult on oily material because the solids congeal. This
is especially true if the material cannot be dried.
Extreme caution should be taken when adding acid to organic waste. Heating the
organic waste in the presence of acid to 50*C should be done with great caution.
This may be required in order to determine which extraction fluid is used.
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6.4 Most Commonly Asked TCLP Question
I have an oily waste, which flows through a filter. My detection limits are
higher than the regulatory action levels. What should I do?
You have four options:
1. Recycle or burn.
2. Classify by prior knowledge as non-hazardous.
3. Treat the waste as hazardous.
4. If the oil passes through the filter, analyze the TCLP leachate.
1. If the oily waste can be classified as used oil, it can be burned or recycled and a
TCLP analysis is not needed (40 CFR 266.40; 261.6(a)).
2. The waste can be treated as hazardous if no information is available to allow
classification by prior knowledge.
3. By knowledge of the generation of the oily waste, the generator may be able to
certify that the waste could not contain any of the TC analytes at concentrations
above the regulatory action levels. (40 CFR 262.11c(2)). The waste may be a
regulated hazardous waste under other EPA waste code classifications.
4. The liquid which passes through the filter can be analyzed to determine whether it
contains TC analytes. If the SW 846 methods are not appropriate for TC analytes,
any method which is sensitive enough to meet regulatory limits and has
documented QC may be used.
The following pages includes correspondence on oily waste explaining EPA's strategy for
classifying oily wastes as hazardous or non-hazardous.
6-7
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OhteEF*
State of Ohio Environmental Protection Agency
P.O. Box 1049, 1800 WaterMark Dr.
Columbus, Ohio 43266-0149 Richard F. Celeste
(614)644-3020 Fax (614) 644-2329 Governor
Ocrober 30, 1990
Gail Hansen
U.S. Environmental Protection Agency
Office of Solid Waste
Methods Section
Washington, D.C. 20460
Dear Ms. Hansen:
I receive many inquiries on SW-846 detection limits. One caller stated that
he had samples analyzed under SW-846 protocol which totaled over $75,000, only
to find that many of the constituents had detections limits above regulated
values. Another caller had industrial waste (baghouse residue) tested under
TCLP and noted that the detection limits of the constituents were all below
regulated levels except for chlordane which in eight out of nine samples was
0.045 mg/L, versus the regulated value of 0.03 mg/L. I need suggestions on
the appropriate response to these inquiries, specifically:
(1) Assuming a given laboratory has followed proper protocol, If
detection limits of constituents in a waste sample are in excess of
but close to regulated values, is the sample considered hazardous?
(2) Using the chlordane situation (above) as an example, what
analytical procedures can a laboratory use, for example clean-up
and dilution, outside of procedures specified under a given method
(eg. TCLP), which are permissible by the U.S. EPA? Can Method 8250
( semi-volatiles) , for example, be used to confirm or as a
substitute for TCLP in analyzing chlordane?
(3) Is there an upcoming FR updating and clarifying analytical problems
in the TCLP analytical section?
Your help will be appreciated 1n resolving the concerns outlined in this
communication. If you need additional information, I may be contacted at
(614) 644-2956.
Sincerely,
Art Coleman
Technical Assistance Section
Division of Solid and Hazardous Waste Management
ALC/pas
cc: Karl Bremer, USEPA, Region V Steve McBride, DERR
Dr. Gary Davidson, Chief, Public Health Laboratories, ODH
David E. Vanderberg, Regional Manager, Kemron Environmental Services
Gerry G. loannldes, Chief, EnVfftrtimental Services, Ohio EPA
6-8
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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
WASHINGTON, D.C. 20460
NOV 8 (990 OFF.CC o?
SOLID v:-ST = A.VJO :VE=GE\CY RESPONSE
Art Coleman
Technical Assistance Section
Division of Solid and Hazardous Waste Management
Ohio EPA
P.O. Bex 1049
1800 WaterMark Dr.
Columbus, OH 43266-0149
Dear Mr. Coleman:
I am writing in reponse to your letter of October 30,1990
concerning the questions you raised with Method 1311 (TCLP).
In answer to your first question, there are situations when
a laboratory is.asked to perform an inappropriate test. "The TCLP
was not intended to be applied to certain matrices, such as oils
or neat solvents. In these instances, the waste usually goes
through the filter and is, by definition, a liquid and its own
extract. The analysis of this liquid extract for organics
entails diluting it before injecting it into a GC or GC/MS. The
dilution often results in detection limits being much higher than
the regulatory thresholds. If this is the case, you must assume
your waste is hazardous since the laboratory cannot demonstrate
non-hazardousness with TCLP for these materials. We currently do
not have the technology to address this issue.
In answer to your second question, a laboratory must use the
TCLP if testing for hazardousness under the Toxicity
Characteristic or if assessing effectiveness of waste treatment
under the Land Disposal Restrictions Program. These two
regulations actually contain the method as an appendix and it is,
therefore, part of the law. However, the extract obtained from
the TCLP may be analyzed by any method as long as that method has
documented QC and the method is sensitive enough to meet the
regulatory limit. In other words, the lab does not have to use
SW-846 methods because these methods are intended to serve only
as a guidance for the regulated community. SW-846 methods that
are currently in draft form (e.g., 8250 for chlordane) may also
be used to analyze the extract.
6-9 Primed on Recycled Paptr
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In 'answer to your third question, .there are no plans to
prepare a clarifying FR update in the near future.
I hope these answers have sufficiently addressed your
concerns. If you have any further questions, please give me a
call at (202) 475-6722 or write me again at the above address.
Sincerely yours,
Gail Hansen
Health Scientist
Methods Section
(OS-331)
cc: Alec McBride
Jeanne Hankins
Hugh Davis, OWPE
Leon Lazarus, Region II
6-10
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RECEIVED
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY FFRn-
WASHINGTON, D.C. 20460 CD ^ 3 1991
Toxic .& j-iaz. Wactc
E OF
SOLID WASTE AND EMERGENCY RESPONSE
FbS 5 !39!
Mr. Art Coleman
Technical Assistance Section
Division of Solid and Hazardous Waste Management
Ohio EPA
P.O. Box 1049
1800 WaterMark Drive
Columbus, Ohio 43226-0149
Dear Mr. Coleman:
The purpose of this letter is to clarify resposes provided
to you my November 8, 1990 letter that was in response to your
letter dated October 30, 1990 (copies attached).
In the second paragraph of my letter to you, I indicated
that because of the need to dilute the liquid extract for
organics before injecting it into a GC or GC/MS, problems will
manifest with respect to detection limits being much higher than
the TC regulatory levels. I indicated that in the event that
this occurs, it may not be possible for the laboratory to
determine conclusively that a waste is in fact a hazardous waste.
I further indicated that in this situation, a generator must
assume that their waste is hazardous. ~I want to clarify and
correct this response.
The RCRA hazardous waste regulations allow a generator to
use his/her knowledge of a waste or the processes that generated
a waste to determine if it would be regulated as a hazardous
waste. Thus it is not a requirement with respect to the above
scenario that the generator must assume that his/her waste is
hazardous. A generator may use his/her knowledge to determine
that it is not hazardous. The point I meant to make is that if
no other information is available to assist a generator to make a
hazardousness determination and in light of the inconclusive TCLP
results, it would generally be prudent for the generator to
manage that waste as a hazardous waste.
j
With respect- to used oil destined for recycling or for
blending as fuel, there is no requirement to make a hazardous
waste- determination. In those cases, therefore, there is no need
to run a TCLP; thus the analytical problems mentioned above would
vX1 Printed on fiV>. •,, • ,-j
6-11 ^
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not be an issue. This is consistent with and should further the
Agency's goal of encouraging recycling as opposed to disposal of
used oils. If a generator is going to dispose of used oil
(either in a landfill or. by incineration), however, then a
hazardous waste determination will have to be made and the above
analytical issues may arise.
I want to apologize for any misunderstanding that may have
arisen from my initial letter. If you have any further
questions, please feel free to call me at (202) 475-6722.
Sincerely yours,
Gail Hansen
Health Scientist
Methods Section
(OS-331)
cc: Alec McBride
Jeanne Hankins
Hugh Davis, OWPE
u-£eon Lazarus, Region II
6-12
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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
WASHINGTON, D.C. 20460
O—CE
5CLID '.\A5'£ -.'.; =Vi:
RECEIVED
Ms. Elaine McPherson ..... « p. .Qg,
Technical Sales Representative JUN t u 193]
IT Corporation
17605 Fabrica Way
cerritos, CA 90701 Toxic & H a/T Waste
Dear Ms. McPherson:
I am writing in reference to your letter of April 11, 1991
concerning the handling of TCLP extractions as they apply to oily
wastes.
We ..do not ..recommend performing the extract on the oily waste
that passes through the filter as Margo Jackisch of SAIC
suggested to you. First of all, the TCLP determines release
potential in two steps, the first of which I will discuss here as
it specifically applies to your situation. The initial
filtration step separates the solid phase of a waste from its
liquid phase. This liquid phase represents the primary waste
leachate or the liquid fraction of a waste that is mobile and can
be released from a landfill. In your case, the oil goes through
the filter and, by definition, becomes its own leachate which is
then analyzed directly.
If your waste is a used oil that is destined for recycling,
there is no need to characterize the waste since it would be
exempt under 40 CFR Section 261.6(a)(2)(iii) and (a)(3)(iii). It
is the decision to dispose of the waste, in lieu of recycling,
that triggers the waste characterization requirement. If your
waste is a used oil that cannot be recycled and is destined for
disposal, generators are required to make a hazard determination.
If the generator chooses to test for the Toxicity Characteristic,
the generator must use the TCLP or an approved alternative
method, as described in 40 CFR 261.24. The extract obtained from
the TCLP may be analyzed by any method, provided the method used
has documented QC and is sensitive enough to meet the regulatory
threshold for the constituents of concern.
In cases where the TCLP results on used oil or oily wastes
are inconclusive, including cases where the detection limit for a
constituent is higher than the regulatory threshold, generators
may use their knowledge of the processes involved in the
6-13
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generation of the waste to make a hazard determination or resort
to an alternative analytical method to get an answer. This has
been necessary with volatile organics. At this time, the Agency
is conducting studies of an automated headspace analysis
methodology coupled with isotope dilution mass spectrometry . in
order to achieve greater analytical sensitivity for all TC
volatile analytes, including vinyl chloride. We suggest the use
of this approach where needed. Currently, only a working draft
method (copy enclosed) is available. Pending the outcome of
Agency studies, the draft method will be revised and proposed for
inclusion in SW-846.
For further assistance, please call the MICE (Methods
Information Communications Exchange) at (703) 821-4789. Calls
are recorded on an answering machine and, for the majority of
questions, responses are provided within 24 hours. I hope this
information has sufficiently addressed your questions.
Sincerely yours,
Gail Hansen
Environmental Health Scientist
Methods Section (OS-331)
cc: David Bussard
Alec McBride
Steve Cochran
Mike Petruska
John Austin
Leon Lazarus, Region II
Hugh Davis, OWPE
RCRA/ Super fund Hotline
MICE Line
6-14
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6.5 Analytical Options
The methods discussed from SW 846 may not provide adequate identification
and quantification of the waste. Inadequate method performance may be
caused by matrix interferences. The following methods may assist in dealing
with organic matrix problems. This list is not exhaustive. Method
developement may be required to accomodate specific interferences. If
developement is required, method validation should be performed and approvals
may be required when SW 846 is required by the regulations.
• Isotopic dilution
• High resolution GC/MS
Isotopic Dilution
One option outlined by EPA in the memos is the use of isotopic dilution methods. The
isotopic dilution methods use stable isotopically labeled analogs of the compounds of
interest. These labeled compounds are added prior to sample preparation and analysis. In
the case of volatiles and semivolatile analyses by GC/MS, they are added prior to purging
or extraction. Two methods are currently listed in 40 CFR Part 136 Appendix A which use
the isotopic dilution technique. One is a purge and trap capillary GC/MS, method 1624,
and the other is semivolatile extraction followed by capillary GC/MS, method 1625.
In both methods, the calibration is established by relative responses based on a ratio of the
isotopically labeled compound versus the unlabeled compound over five concentration
ranges. The relative response of the labeled versus unlabeled compound in the sample is
compared to the calibration curve or average response factor to quantitate the analyte in
the sample.
An example of a labeled compound is toluene-d8, which is deuterated toluene (all
hydrogens are replaced by deuterium). Carbon-13 labeled compounds may also be used.
The advantages of isotopic labeling are greater accuracy in quantitation and the ability to
quantitate despite interferences. The disadvantages are the expense and difficulty in
obtaining labeled analogs of the compounds of interest, and the time needed to develop
the procedure. Laboratories which have experienced GC/MS staff who have done dioxin
analyses or who have many years of GC/MS experience should be capable of providing
these analyses.
High Resolution GC/MS
High resolution GC/MS could also be used to quantitative the compounds. There are no
published methods for waste analysis by high resolution GC/MS. However, this technique
should provide greater sensitivity, lower detection limits and the ability to deal with
interferences. The disadvantages are the same as isotope detection.
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TJ
•o
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z
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Appendix I
TCLP Methods From
40 CFR 261 Appendix II
SW 846 Method 1311 (Method Without
Typographical Errors)
November 24, 1 992 Update
-------
PI. 261, App. I
(10) The name and mode) numbers
of the Instrument(s) used In perform-
ing the tests:
(11) QA/QC documentation: and
(12) The following statement signed
by the generator or his authorized rep-
resentative:
I certify under penalty of law that all
process equipment required lo be cleaned or
replaced under 40 CFR 261.35 was cleaned
or replaced aa represented In the equipment
cleaning and replacement plan and accom-
panying documentation. I am aware that
there are significant penalties for providing
false Information. Including lhe>posslblllty
of fine or Imprisonment.
155 FR 50482. Dec. 6. 1000. an amended at 5fl
PR 30105. July 1. 10011
EFFECTIVE DATE NOTE: At 55 FR 50482,
Dec. 6. 1000, i 261.35 was added. Paragraph
(c) contains Information collection and rec-
ordkeeplng requirements and will not
become effective until approval has been
given by the Office of Management and
Budget. A notice will be published In the
FEDERAL REGISTER once approval has been
obtained.
APPENDICES TO PART 261
APPENDIX I TO PART 281 —
REPRESENTATIVE SAMPLING METHODS
The methods and equipment used for
sampling waste materials will vary with the
form and consistency of the waste materials
to be sampled. Samples collected using the
sampling protocols listed below, for sam-
pling waste with properties similar to the In-
dicated materials, will be considered by the
Agency lo be representative of the waste.
Extremely viscous liquid—ASTM Standard
D140-10 Crushed or powdered material—
ASTM Standard D348-75 Soil or rock-like
malerlal-ASTM Standard D420-60 Soil-
like material—ASTM Standard D1452-65
Fly Ash-like material—ASTM Standard
D2234-76 (ASTM Standards are available
from ASTM, 1016 Race St.. Philadelphia.
PA 101031
Containerized liquid wastes—"COLIWASA"
described In "Test Methods for the Eval-
uation of Solid Waste, Physical/Chemical
Methods." • U.S. Environmental Protec-
•These methods are also described In
"Samplers and Sampling Procedures for
Hazardous Waste Streams," EPA 600/2-80-
018, January 1980.
40 CFR Ch. I (7-1-92 Edition)
lion Agency. Office of Solid Wasle. Wash-
ington. D.C. 20460. (Copies may be ob-
tained from Solid Waste Information, U.S.
Environmental Protection Agency. 26 W.
St. Clalr St.. Cincinnati. Ohio 452061
Liquid waste In pits, ponds, lagoons, and
similar reservoirs.—"Pond Sampler" de-
scribed In "Test Methods (or the Evalua-
tion of Solid Waste. Physical/Chemical
Methods." *
This manual also contains additional In-
formation on application of these protocols.
APPENDIX II 'TO PART 261—METHOD
1311 TOXICITY CHARACTERISTIC
LEACHING PROCEDURE (TCLP)
1.0 Scopf. and Application
1.1 The TCl.P Is designed to determine
the molilllly of both organic and Inorganic
analylcs present In liquid, solid, and multi-
phasic wastes.
1.2 If a total analysis of the waste dem-
onstrates that Individual analytes are not
present In the waste, or that they arc
present but at such low concentrations that
the appropriate regulatory levels could not
possibly be exceeded, the TCI.P need not be
run.
1.3 If an analysis of any one of the liquid
fractions of the TCLP extract Indicates that
a regulated compound Is present at such
high concentrations that, even after ac-
counting for dilution from the other frac-
tions of the extract, the concentration
would be equal lo or above the regulatory
level tor that compound, then the waste Is
hazardous and It Is not necessary lo analyze
the remaining fractions of the extract.
1.4 If un analysis of extract obtained
using a bottle extractor shows llmt the con-
cenlrallnn of any regulated volatile analylc
equals or exceeds Ihc regulatory level for
that compound. uU:n the waste Is hazardous
and extraction using the Z1IE Is not neces-
sary. However, extract from a bottle extrac-
tor cannot be used lo demonstrate that the
concentration of volatile compounds Is
below the regulatory level.
2.0 Summary o/Method
2.1 For liquid wastes (I.e., those contain-
ing less than 0.5% dry solid material), the
waste, after (Miration through a 0.0 to 0.11
lim glass fiber filler, In defined as the TCI.r
extract.
2.2 For wasles containing greater than or
equal lo 0.5% solids, the liquid. If any, Is
separated from the solid phase and stored
(or later analysis; the particle size of the
solid phase Is reduced. l( necessary. The
solid phase Is extracted with an amount of
extraction fluid equal lo 20 limes Die weight
Environmental Protection Agency
of Ihe solid phase. The extraction fluid em-
ployed Is a function of the alkalinity of the
solid phase of the waste. A special extractor
vessel Is used when testing for volatile ana-
lyles (see Table 1 (or a list o( volatile com-
pounds). Following extraction, the liquid ex-
tract Is separated from the solid phase by
(Miration through a 0.0 to O.n ,nn glass fiber
(Illcr.
2.3 If compatible (I.e.. multiple phases
will not (orm on combination), the Initial
liquid phase of the waste Is added lo the
liquid extract, and these arc analyzed to-
gether. If Incompatible, the liquids arc ana-
lyzed separately and the results.are mathe-
matically combined to yield a volume-
weighted average concentration.
3.0 Interferences
3.1 Potential Intcrlercnccs thai may be
encountered during analysis arc discussed In
the Individual analytical methods.
4.0 Apparatus and Materials
4.1 Agitation apparatus: The agitation
apparatus must be capable of rotating the
extraction vessel In an end-over-cnd fashion
(see Figure 1) at 30 ±2 rpm. Suitable devices
known lo EPA are Identified In Table 2.
4.2 Extraction Vessels.
4.2.1 Zero-lleadspRce Extraction Vessel
(7.IIE). This device Is (or use only when the
waste Is being tested for the mobility of
volatile analylcs (I.e., those listed In Table
1 1). The ZHE (depicted In Figure 2) allows
(or liquid/solid separation within Ihe
device, and effectively precludes headspacc.
This lype of vessel allows (or Initial liquid/
solid separation, extraction, and final ex-
tract filtration without opening the vessel
(see section 4.3.1). The vessels shall have an
Internal volume of 500-600 mL. and be
equipped to accommodate a 00-110 mm
(liter. The devices contain V1TON' ' O-rhiRS
which should be replaced frequently. Suita-
ble '/111': devices known to KI'A are Identi-
fied In Table :i.
For the ZIIF: lo be acceptable for use. the
piston within the 7.\\K should be able to be
moved wllh approximately 15 pounds per
square Inch (psl) or less. If II lakes more
pressure lo move the piston, the O-rlngs In
Ihe device should be replaced. If this does
not solve the problem. Ihe 7.IIE Is unaccept-
able (or TCLP analyses and Ihe manufac-
turer should be contacted.
The '/.HE should he checked (or leaks
a(lcr every exlractlon. K Ihe device contains
a built-in pressure KIUIRC. pressurize Ihe
device lo 50 psl. allow II lo sland unattended
(or 1 hour, and rcchcck Ihe pressure. If Ihe
device docs nol have a built-in pressure
gauge, pressurize the device lo 50 psl, sub-
1 V1TON1 Is a registered trademark of
nul'onl.
PI. 261, App. II
merge It In waler, and check for the pres-
ence of air bubbles escaping from any of the
fillings. If pressure Is lost, check all fittings
and Inspect and replace O-rlngs. If neces-
sary. Relest the device. If leakage problems
cannot be solved, the manufacturer should
be contaclcd.
Some ZHEs use gas pressure lo actuate
the /HE piston, while others use mechani-
cal pressure (sec Table 3). Whereas Ihe vola-
lllcs procedures (sec section 7.3) rc(crs to
pounds per square Inch (psl). (or the me-
chanically actuated piston, the pressure ap-
plied Is measured In torque-lnch-pounds.
Refer lo Ihe manufacturer's Instructions as
to the proper conversion.
4.2.2 Bollle Extraction Vessel. When the
waste Is being evaluated using the nonvola-
tile extraction, a jar with sufficient capacity
lo hold the sample and the extraction fluid
Is needed, lleadspuce Is allowed In this
vessel.
The extraction bottles may be constructed
(rom various materials, depending on the
analytes lo be analyzed and the nature of
the waste (see section 4.3.3). It Is recom-
mended that boroslllcate glass bottles be
used Instead of other types of glass, espe-
cially when Inorganics are of concern. Plas-
tic hollies, other than polytelrafluoroelhy-
lene, shall nol be used if organlcs are lo be
Investigated. Dottles are available (rom a
number o( laboratory suppliers. When this
lype of extraction vessel Is used, the filtra-
tion device discussed In section 4.3.2 Is used
(or Initial liquid/solid separation and final
extract filtration. ,
4.3 Filtration Devices: It Is recommended
that all nitrations be performed In a hood.
4.3.1 Zcro-Headspace Extractor Vessel
(ZIIE): When the waste Is evaluated for vo-
tallies. Ihe zero-headspace extraction vessel
described In section 4.2.1 Is used (or (Mira-
tion. The device shall be capable o( support-
Ing and keeping In place the glass (Ibcr
(Illcr and be ahlt: lo withstand the pressure
needed to accomplish separation (50 psl).
NOTE: When It Is suspected that the glass
fiber filler has been ruptured, an In-line
glass (Iber (Illcr may be used to (liter the
material within Ihe ZIIE.
4.3.2 Filler Holder: When Ihe wasle Is
evaluated (or other than volatile analylcs,
any filler holder capable of supporting a
glass (Iber (Illcr and able to withstand Ihe
pressure needed to accomplish separation
may he used. Suitable filter holders range
from simple vacuum unlls lo rclallvcly com-
plex syslems capable of exerting pressures
o( up lo 50 psl or more. The type of (liter
holder used depends on the properties of
the material lo be filtered (sec section 4.3.3).
These devices shall have a minimum Inter-
nal volume of 300 mL and he equipped lo ac-
commodate a minimum (Illcr size of 47 mm
-------
PI. 361, App. II
(filter holders having on Internal capacity
of 1.6 L or greater, and equipped to accom-
modate a 142 mm diameter filter, are recom-
mended). Vacuum filtration can only be
used for wastes with low solids content
«10%) and for highly granular, liquid-con-
taining wastes. All other types of wastes
should be filtered using positive pressure fil-
tration. Suitable- filler holders known to
EPA are shown In Table 4.
4.3.3 Materials of Construction: Extrac-
tion vessels and filtration devices shall be
made of Inert materials which will not leach
or absorb waste components. Glass, polyle-
trafluoroethylene (PTFE). or type 316 stain-
less steel equipment may be used when eval-
uating the mobility of both organic and In-
organic components. Devices ma'de of high
density polyethylene (HOPE), polypropyl-
ene (PP). or polyvlnyl cltlorlde (PVC) may
be used only when evaluating the mobility
of metals. Doroslllcate glass bottles are rec-
ommended for use over oilier types of glass
bottles, especially when Inorganics are ana-
lytes of concern.
4.4 Filters: Filters shall be made of boro-
silicate glass fiber, shall contain no binder
materials, and shall have an effective pore
size of 0.6 to 0.8 urn. or equivalent. Filters
known to EPA which meet these specifica-
tions are Identified In Table 5. Pre filters
must not be used. When evaluating the mo-
bility of metals, fillers shall be acid-washed
prior to use by rinsing with IN nitric acid
followed by three consecutive rinses with
delonlzed distilled water (a minimum of 1 L
per rinse Is recommended). Glass fiber filter
are fragile and should be handled with care.
4.5 pH Meters: The meter should be ac-
curate to ± 0.05 units at 25'C.
4.6 ZHE Extract Collection Devices:
TEDI.AR® ' bags or glass, stainless steel or
PTFE gag-light syringes are used to collect
the Initial liquid phase and the final extract
of the waste when using the ZHE device.
The devices listed are recommended for use
under the following conditions:
4.6.1 If a waste contains an aqueous
liquid phase or If a waste does not contain a
significant amount of nonaqueous liquid
(I.e.. <1% of total waste), the TEDLAR®
bag or a 600 mL syringe should be used to
collect and combine the Initial liquid and
solid extract.
4.6.2 If a waste contains a significant
amount of nonaqueous liquid In the Initial
liquid phase (I.e.. >1% of total waste), the
syringe or the TEDLAR® bag may be used
for both the Intltlal solid/liquid separation
and the final extract filtration. However,
analysts should use one or the other, not
both.
• TEDLAR® Is a registered trademark of
Dupont.
40 CFR Ch. I (7-1-92 Edition)
4.6.3 If the waste contains no Initial
liquid phase (Is 100% solid) or has no signifi-
cant solid phase (Is 100% liquid), either the
TEDLAR® bag or the syringe may be used.
If the syringe Is used, discard the first 5 mL
of liquid expressed from the device. The re-
maining allquols arc used for analysis.
4.7 ZIIE Extraction Fluid Transfer DC-
vices: Any device capable of transferring the
extraction fluid Into the /.111'.: without
changing the nature of the extraction fluid
Is acceptable (e.g, a positive displacement or
peristaltic pump, a gas tight syringe, pres-
sure filtration unit (see section 4.3.2). or
other ZHE device).
4.8 Laboratory Balance: Any laboratory
balance accurate to within ± 0.01 grams
may be used (all weight measurements are
to be within ± 0.1 grams).
4.0 Dcakcr or Krlcnmeycr flask, \t\nnx.
500 ml,
4.10 Walchglass. appropriate diameter to
cover beaker or erlenmeyer flask.
4.11 Magnetic stlrrer.
5.0 Reagents
5.1 Reagent grade chemicals shall be
used In all tests. Unless otherwise Indicated.
It Is Intended that all reagents shall con-
form to the specifications of the Committee
on Analytical Reagents of the American
Chemical Society, where such specifications
are available. Oilier grades may be used,
provided It Is first ascertained thai the rea-
gent Is of sufficiently high purity to penult
Its use without lessening the accuracy of the
determination.
5.2 Reagent water. Reagent water Is de-
fined as water In which an Interfernnt Is not
observed at or above the methods detection
limit of the analyle(s) of Interest. For non-
volatile extractions. ASTM Type II water or
equivalent meets the definition of reagent
water. For volatile extractions. It Is recom-
mended that reagent water be generated by
any of the following methods. UenKent
water should be monitored periodically for
Impurities.
5.2.1 Reagent water for volatile extrac-
tions may be generated by passing lap water
through a carbon filter bed containing
about 500 grams of activated carbon
(Calgon Corp.. Flllrosorb-300 or equivalent).
5.2.2 A water purification system (MIDI-
pore Huper-Q or equivalent) may also be
used to generate reagent water for volatile
extractions.
5.2.3 Reagent water for volatile extrac-
tions may also be prepared by boiling water
for 16 minutes. Subsequently, while main-
taining the water temperature at 1)0 I 5 de-
grees C. bubble a contaminant-free Inert gas
(e.g., nitrogen) through the water for 1
hour. While still hot. transfer the water to a
narrow mouth screw-cap bottle under zero-
Environmental Protection Agency
headspacc and seal with a Teflon-lined
septum and cap.
5.3 Hydrochloric acid (IN), I1C1. made
from ACS reagent grade.
5.4 Nitric acid (IN). IINOi. made from
ACS reagent grade.
5.5 Sodium hydroxide (IN). NnOH. innde
from ACS reacenl grade.'.
5.0 Claclal ncclli: acid. C1I.CI 1,0011. ACS
reagent Kfade.
5.7 Extraction fluid.
5.7.1 Extraction fluid #1: Add 5.7 ml, gla-
cial CHiCIIiOOH to 500 mL, of reagent
water (Sec section 6.2), add 64.3 mL of IN
NaOH. and dilute to a volume of 1 liter.
When correctly prepared, the pH of this
fluid will be 4.03±0.05.
5.7.2 Extraction fluid #2: Dilute 5.7 ml.
glacial CH,CHiOOH with reagent water
(See Huctlon 5.2) to a volume of I llli:r.
When con roily prepared, the pll of Mils
fluid will he 2.UU±0.05.
NOTE: These extraction fluids should be
monitored frequently for Impurities. The
pll should be checked prior to use to ensure
that these fluids are made up accurately. If
Impurities are found or the pH Is not within
the above specifications, the fluid shall be
discarded and fresh extraction fluid pre-
pared.
5.n Analytical standards shall be pre-
pared according to Ihc approprlalc analyti-
cal method.
6.0 Sample Collection. Preservation, and
Handling
6.1 All samples shall be collected using
nn appropriate sampling plan.
6.2 The TCLP may place requirements
on the minimal size of the field sample, de-
pending upon the physical state or stales of
the waste and the analyles of concern. An
nlkiuol is needed for preliminary evaluation
of which extraction fluid Is to be used (or
Ihc nonvolatile annlylc extraction proce-
dure. Another aliquot may be needed to ac-
tually couducl the nonvolatile extraction
(see section 1.4 concerning the use of this
extract for volatile organlcs). If volatile or-
ganlcs are of concern, another aliquot may
be needed. Quality control measures may re-
quire additional allquou. Further. It Is
always wise to collect more samples Just In
case something goes wrong with Hie Initial
allcmpt to conduct the lest.
0.3 Preservatives shall not be added to
uamples before extraction.
0.4 Samples may be refrigerated unless
refrigeration results In Irreversible physical
change to the waste. If precipitation occurs,
the entire sample (Including precipitate)
should be extracted.
0.5 When the waste Is to be evaluated for
volatile analyles, care shall be taken lo min-
imize the loss of volatlles. Samples shall be
collected and stored In a manner Intended
Pt. 261, App. II
to prevent the loss of volatile analytes (e.g..
samples should be collected In Teflon-lined
septum capped vials and stored at 4 'C.
Samples should be opened only Immediately
prior lo extraction).
0.0 TCI.P extracts should be prepared
for analysis and analyzed as soon as possible
following extraction. Extracts or portions cif
extracts for metallic analytc determinations
must be acidified with nitric acid to a pll
<2. unless precipitation occurs (sec section
7.2.14 If precipitation occurs). Extracts
should be preserved for other analytes ac-
cording lo the guidance given In the Individ-
ual analysis methods. Extracts or portions
of extracts for organic analylc determina-
tions shall not be allowed to come Into con-
tact with the atmosphere (I.e., no head-
space) in prevent losses. Sec section 8.0 (QA
requirements) for acceptable mirnple and ex-
tract holding times.
7.0 Procedure
7.1 Preliminary Evaluations. Perform
preliminary TCLP evaluations on a mini-
mum 100 gram aliquot of waste. This ali-
quot may not actually undergo TCLP ex-
traction. These preliminary evaluations In-
clude: (1) Determination of the percent
solids (section 7.1.1): (2) determination of
whether the waste contains Insignificant
solids and Is. therefore. Its own extract after
filtration (section 7.1.2): (3) determination
of whether the solid portion of the waste re-
quires particle size reduction (section 7.1.3):
and (4) determination of which of the two
extraction fluids are lo be used for the non-
volatile TCLP extraction of the waste (sec-
tion 7.1.4.).
7.1.1 Preliminary determination of per-
cent solids: Percent solids Is defined as that
fraction of a waste sample (as a percentage
of the lota) sample) from which no liquid
may bi: forced out by an applied pressure, as
described below.
7.1.1.1 If the waste will obviously yield
no liquid when subjected lo pressure filtra-
tion (I.e.. Is 100% solids) proceed to section
7.1.3.
7.1.1.2 If the sample Is liquid or multi-
phasic, liquid/solid separation to make a
preliminary determination of percent solids
Is required. This Involves the filtration
device described In section 4.3.2 and Is out-
lined In sections 7.1.1.3 through 7.1.1.0.
7.1.1.3 Prc-welgh the filler and Ihc con-
tainer thai will receive the filtrate.
7.1.1.4 Assemble Ihe filter holder and
filler following the manufacturer's Instruc-
tions. Place the filler on the support screen
and secure.
7.1.1.5 Weigh out a subsamplc of the
woslc (100 gram minimum) and record Ihe
weight.
7.1.1.6 Allow slurries to stand lo permit
the solid phase to settle. Wastes that settle
-------
PI. 261, App. II
atowly may be centrlfuged prior to filtra-
tion. Cenlrlfugatlon U to be used only as an
aid to filtration. If used, the liquid should
be decanted and filtered followed by filtra-
tion of the solid portion of the waste
through the same filtration system.
7.1.1.7 Quantitatively transfer the waste
sample to the filler holder (liquid and solid
phases). Spread the waste sample evenly
over the surface of the filter. If filtration of
the waste at 4 'C reduces the amount of ex-
pressed liquid over what would be expressed
at room temperature then allow the sample
to warm up to room temperature In the
device before filtering.
NOTE: If waSte material (>1% of original
sample weight) haa obviously adhered to
the container used to transfer the sample to
the filtration apparatus, determine the
weight of this residue and subtract It from
the sample weight determined In section
7.1.1.6 to determine he weight of the waste
sample that will be filtered.
Gradually apply vacuum or gentle pres-
sure of 1-10 pal. until air or pressurizing gas
moves through the filter. If this point U not
reached under 10 psl. and If no additional
liquid has passed through the filter In any 2
minute Interval, slowly Increase the pres-
sure In 10 psl Increments to a maximum of
60 psl. After each Incremental Increase of 10
pal. If the pressurizing gaa has not moved
through the filter, and If no additional
liquid has passed through the filter In any 2
minute Interval, proceed to the next 10 psl
40 CFR Ch. I (7-1-92 Edition)
Increment. When the pressurizing gas
begins to move through the filter, or when
liquid flow has ceased at SO psl (I.e.. filtra-
tion does not result In any additional fil-
trate within any 2 minute period), stop the
filtration.
NOTE: Instantaneous application of high
pressure can degrade the glass flhcir (liter
and may cause premature plugging.
7.1.1.6 The material In the filter holder Is
defined as the solid phase of the waste, and
the filtrate Is defined as the liquid phase.
NOTE: Some wastes, such as oily wastes
and some paint wastes, will obviously con-
lain some material that appears to be a
liquid. Even after applying vacuum or pres-
sure filtration, as outlined In section 7.1.1.7.
this material may not filter. If this Is the
case, the malcrlnl wllliln the filtration
device Is defined as a solid. Do not replace
the original filler with a fresh filler under
any circumstances. Use only one filler.
7.1.1.0 Determine the weight of the
liquid phase by subtracting the weight of
the filtrate container (see section 7.1.1.3)
from the total weight of the filtrate-filled
container. Determine the weight of the solid
phase of the waste sample by subtracting
the weight of the liquid phase from the
weight of the total waste sample, as deter-
mined In section 7.1.1.6 or 7.1.1.7.
Record the weight of the liquid and solid
phases. Calculate the percent solids as fol-
lows:
Percent solids - •
Weight of solid (section 7.1.1.9)
Total weight of waste (section 7.1.1.5 or 7.1.1.7)
xlOO
7.1.2 If the percent solids determined In
section 7.1.1.0 Is equal to or greater than
0.6%. then proceed either to section 7.1.3 to
determine whether the solid material re-
quires particle size reduction or to section
7.1.2.1 If It Is noticed that a small amount of
the filtrate Is entrained In wetting of the
filler. If Ihe percent solids determined In
section 7.1.1.9 Is less than -0.6%, then pro-
ceed to section 7.2.9 If the nonvolatile TCLP
Is to be performed and to section 7.3 with a
fresh portion of the waste If the volatile
TC1JP Is to be performed. •' •
7.1.2.1 Remove the solid phase and filler
from the filtration apparalus.
7.1.2.2 Dry the filler and solid phase al
100± 20'C until Iwo successive weighings
yield Ihe same value within ± 1%. Record
Ihe final weight.
NOTE: Caution should be taken to ensure
that the subject solid will not flash upon
heating. It Is recommended that the drying
oven be vented to a hood or other appropri-
ate device.
7.1.2.3 Calculate Ihe percent dry solids as
follows:
% dry solids — •
(Weight of dry waste-t-filter)—tared weight of filler
Initial weight, of waste (section 7.1.1.5 or 7.1.1.7)
XlOO
Environmental Protection Agency
7.1.2.4 If the percent dry solids Is less
than 0.5%. then proceed to section 7.2.0 If
the nonvolatile TCLP Is to be performed.
and to section 7.3 If the volatile TCLP Is to
be performed. If the percent dry solids Is
greater than or equal to 0.5%. and If Ihe
nonvolatile TCLP Is lo be performed, relurn
to the beginning of this auction (7.1) and.
wllli a fresh portion of waste, determine
whether particle size reduction la necessary
(section 7.1.3) and determine the appropri-
ate extraction fluid (section 7.1.4). If only
llic volatile TCLP Is to be performed, sec
the note In section 7.1.4.
7.1.3 Determination of whether the
waste requires particle size reduction (parti-
cle size Is reduced during this step): Using
the solid portion of the waste, evaluate the
solid for particle size. Particle size reduction
Is required, milcus the solid has a surface
area per gram of material equal lo or great-
er than 3.1 cm1, or Is smaller limn 1 cm In
Its narrowest dimension (I.e.. Is capable of
passing Ihrough a 0.5 mm (0.375 Inch)
standard sieve). If the surface area Is small-
er or the particle size larger than described
above, prepare the solid portion of the
waste for extraction by crushing, culling, or
grinding the waste to a surface area or par-
ticle size as described above. If the solids arc
prepared for organic volatlles extraction.
special precautions must be taken (see sec-
tion 7.3.0).
NOTE: Surface area criteria are meant for
filamentous (e.g.. paper, cloth, and similar)
waste materials. Actual measurement of sur-
face area Is not required, nor Is It recom-
mended. For materials thai do not obviously
meet the criteria, sample-specific methods
would need to be developed and employed
to measure the surface area. Such method-
ology Is currently not available.
7.1.4 Determination of appropriate ex-
traction fluid: If the solid content of the
waste In grealer than or equal lo 0.5% ciml If
the sample will be extracted for nonvolatile
constituents (section 7.2). determine the ap-
proprlale fluid (section 5.7) for the nonvola-
tile: extraction as follows:
NOTE: TCLP extraction for volatile con-
stlluents uses only extraction fluid HI (sec-
tion 5.7.1). Therefore, If TCLP extraction
for nonvolatlles Is not required, proceed lo
section 7.3.
7.1.4.1 Weigh oul a small cvibsamplc of
the solid phase of the waste, reduce the
solid (If necessary) to a particle size of ap-
proximately 1 mm In diameter or less, and
transfer 5.0 grams of the solid phase of the
waste lo a BOO mL beaker or Erlenmeyer
flask.
7.1.4.2 Add 00.5 mL of reagent woler lo
the beaker, cover with a walchglass. and stir
vigorously for 5 minutes using a magnetic
sllrrer. Measure and record the pll. If the
Pi. 261, App. II
Pll Is <5.0, use extraction fluid #1. Proceed
lo section 7.2.
7.1.4.3 If the pH from section 7.1.4.2 Is
>5.0. add 3.6 mL IN NCI, slurry briefly.
cover with a walchglass, heat to 50'C. and
hold at 50'C for 10 minutes.
7.1.4.4 Let Ihe solution cool to room tern-
pcralurc and record the pll. If llic pll Is
<5.0. line extraction fluid #1. If the nil Is
>5.0. use extraction fluid #2. Proceed lo sec-
tion 7.2.
7.1.5 If the aliquot of the waste used for
the preliminary evaluation (sections 7.1.1-
7.1.4) was determined lo be 100% solid at
section 7.1.1.1, then It can be used for the
section 7.2 extraction (assuming at least 100
grams remain), and the section 7.3 extrac-
tion (assuming at least 25 grams remain). If
the aliquot was subjected to Ihe procedure
In section 7.1.1.7, then another aliquot shall
be used for the volatile extracllon proce-
dure In section 7.3. The aliquot of the waste
subjected lo Ihe procedure In section 7.1.1.7
might be appropriate for use for the section
7.2 extraction If an adequate amount of
solid (as determined by section 7.1.1.9) was
obtained. The amount of solid necessary Is
dependent upon whether a sufficient
amount of extract will be produced to sup-
port the analyses. If an adequate amount of
solid remains, proceed to section 7.2.10 of
the nonvolatile TCLP extracllon.
7.2 Procedure When Volatlles are not In-
volved. A minimum sample size of 100 grams
(solid and liquid phases) Is recommended. In
some coses, a larger sample size may be ap-
propriate, depending on the solids content
of the waste sample (percent solids. See sec-
tion 7.1.1). whether the Initial liquid phase
of the waste will be mlsclble with the aque-
ous extract of the solid, and whether Inor-
ganics, semlvolatlle organlcs. pesticides, and
herbicides are all analyles of concern.
Enough solids should be generated for ex-
traction such that the volume of TCLP ex-
trad will be sufficient to support all of the
analyses required. If the amount of extract
generated by a single TCLP extraction will
not be sufficient to perform all of the analy-
ses, more lhan one extraction may be per-
formed and the extracts from each com-
bined and allquoted for analysis.
7.2.1 If Ihe waste will obviously yield no
liquid when subjected lo pressure filtration
(I.e.. Is 100% solid, see section 7.1.1). weigh
out a subsample of the waste (100 gram
minimum) and proceed to section 7.2.9.
7.2.2 If the sample Is liquid or mulllpha-
slc. liquid/solid separation Is required. This
Involves the filtration device described In
section 4.3.2 and Is outlined In sections 7.2.3
to 7.2.8.
7.2.3 Pre-weigh the container thai will
receive Ihe filtrate.
7.2.4 Assemble the filter holder and filter
following Ihe manufacturer's Instructions.
-------
PI. 261, App. II
Place the filter on the support screen and
secure. Acid-wash the filter If evaluating the
mobility of metals (see section 4.4).
NOTE: Acid-washed filters may be used for
all nonvolatile extractions even when metals
are not of concern.
7.2.5 Wclfih out a subsample of the waste
(100 gram minimum) nnd record the weight.
If the waste contains <0.5% dry solids (sec-
tion 7.1.2). the liquid portion of the waste.
after filtration. Is defined as the TCLP ex-
tract. Therefore, enough of the sample
should be filtered so that the amount of fil-
tered liquid will support all of the analyses
required of the TCLP extract. For wastes
'containing >0.6% dry solids .(sections 7.1.1
or 7.1.2). use the percent solids Information
obtained In section 7.1.1 to determine the
optimum sample size (100 gram minimum)
for filtration. Enough solids should be gen-
erated by filtration to support the analyses
to be performed on the TCLP extract.
7.2.0 Allow slurries to stand to permit
the solid phase to settle. Wastes that settle
slowly may be centrlfuged prior to filtra-
tion. Use ccnlrlfugallon only as on aid to fil-
tration. If the waste Is centrlfuged. the
liquid should be decanted and filtered fol-
lowed by filtration of the solid portion of
the waste through the same filtration
system.
7.2.7 Quantitatively transfer the waste
. sample (liquid and solid phases) to the filter
holder (see section 4.3.2). Spread the waste
sample evenly over the surface of the filler.
If filtration of the waste at 4 'C reduces the
amount of expressed liquid over what would
be expressed at room temperature, then
allow the sample to warm up to room tem-
perature In the device before filtering.
NOTE: If waste material (>1% of the origi-
nal sample weight) has obviously adhered to
the container used to transfer the sample to
the filtration apparatus, determine the.
weight of this residue and subtract It from
the sample weight determined In section.
7.2.5, to determine the weight of the waste
sample that will be filtered.
Gradually apply vacuum or gentle pres-
sure of 1-10 pal. until air or pressurizing gas
moves through the filter. If this point Is
reached under 10 psl, and If no additional
liquid has passed through the filler In any 2
minute Interval, slowly Increase the pres-
sure In 10 psl Increments to a maximum of
50 pal. After each Incremental Increase of 10
psl. If the pressurizing gas has not moved
through the filter, and If no additional
liquid has passed through the filter In any 2
minute Interval, proceed to the next 10 psl
Increment. -When the pressurizing gas
begins to move through the filter, or when
the liquid flow has ceased at 60 psl (I.e.. fil-
tration does not result In any additional fil-
trate within a 2 minute period), atop the fil-
tration.
40 CFR Ch. I (7-1-92 Edition)
NOTE: Instantaneous application of high
pressure can degrade the glass fiber filler
and may cause premature plugging.
7.2.8 The material In the filter holder Is
defined as the solid phase of the waste, and
the flllrntc Is defined as the liquid phase.
WclKh the flllrtile. The liquid iilin.se may
now he either unnly/.eil (See section 7.2.12)
or stored ul 4'C until time of analysts.
NOTK: Some wastes, such us oily wastes
and some paint wastes, will obviously con-
tain some material that appears to be a
liquid. Even after applying vacuum or pres-
sure filtration, as outlined In section 7.2.7,
this material may not filler. If this Is Ihe
cose, Ihe material within the flllrallon
device Is defined as a solid and Is carried
through Ihe extraction as a solid. Do not re-
place the original filter with a fresh filler
under any circumstances. Use only one
filler.
7.2.0 If the waste contains <0.5% dry
solids (sec section 7.1.2), proceed to section
7.2.13. If the waste contains >0.6% dry
solids (see section 7.1.1 or 7.1.2), and If parti-
cle size reduction of the solid was needed In
section 7.1.3, proceed lo section 7.2.10. If the
waste as received passes a 0.5 mm sieve,
quantitatively transfer the solid material
Into the extractor bottle along with the
filler used to separate the Initial liquid from
the solid phase, and proceed to section
7.2.11.
7.2.10 Prepare the solid portion of the
waste for extraction by crushing, culling, or
grinding Ihe wasle to a surface area or par-
ticle sl?,e as described In section 7.1.3. When
the surface area or particle size has been ap-
propriately altered, quantitatively transfer
the aolld material Into an extractor bottle.
Include the filter used lo separate the Ini-
tial liquid from the solid phase.
NOTE: Sieving of the waste Is not normally
required. Surface area requirements arc
meant for filamentous (e.g., paper, cloth)
and similar waste materials. Actual meas-
urement of surface area Is not recommend-
ed. If sieving Is necessary, a Teflon-coated
sieve should be used to avoid contamination
of Ihe sample.
7.2.11 Determine the amount of extrac-
tion fluid lo add lo Ihe extractor vcascl as
follows:
Weight of
extraction
. fluid
30x percent solids (section
7.l.l)xwelght of waste
tillered (section 7.2.5 or
7.2.7)
100
Slowly add this amount of appropriate ex-
traction fluid (sec section 7.1.4) lo Ihe ex-
tractor vessel. Close the extractor bottle
Environmental Protection Agency
lightly (It Is recommended thai Teflon tape
be used lo ensure a tight seal), secure In
rotary agitation device, and rotate at 30 ± 2
rpm for 18 ± 2 hours. Amblenl lempcrulure
(I.e., lempcralurc of room In which extrac-
tion takes place) shall be maintained at 23
± 2'C during the cxlracllon period.
NOTE: As agitation continue*, pressure
tuny build within Ihe cxlraclnr hollle fnr
some types of wastes (e.g.. limed iir ciilclum
curbonale conlalnlng waste may evolve
gases such as carbon dioxide). To relieve
excess pressure, the exlraclor bolllc may be
periodically opened (e.g., aflcr 15 minutes.
30 minutes, and 1 hour) and vented Into a
hood.
7.2.12 Following Ihe 18 ± 2 hour exlrac-
tlon. separate the material In Ihe exlraclor
vessel Into Its component liquid and solid
phases by filtering through a new gln.s.s
fiber filler, as outlined In secllon 7.2.7. For
final flllrallon of Ihe TCI.I' extracl. Ihe
glass fiber filler may he changed. If neces-
sary, lo facilitate filtration. Flllcr(s) shall
be acid-washed (see secllon 4.4) If evaluating
the mobility of metals.
7.2.13 Prepare the TCLP extract as fol-
lows:
7.2.13.1 If the waste contained no Initial
liquid phase, the filtered liquid material ob-
tained from section 7.2.12 IK defined as the
TCLP cxlracl. Proceed to section 7.2.14.
7.2.13.2 If compatible (e.g.. multiple
phases will not result on combination), com-
bine Ihe filtered liquid resulting from sec-
tion 7.2.12 with the Initial liquid phase of
the wasle oblalned In secllon 7.2.7. This
combined liquid Is defined as the TCLP ex-
tract. Proceed to section 7.2.14.
7.2.13.3 If the Initial liquid phase of the
waste, as obtained from section 7.2.7. Is not
or may not be compatible with the filtered
liquid resulting from section 7.2.12, do not
combine these liquids. Analyze these liquids,
collectively defined as the TCLP extracl,
and combine Ihe results mathematically, as
described In secllon 7.2.14.
7.2.14 Following collection of Ihe TCLP
extract, the pll of Ihe extract should be re-
corded. Immediately aliquot and preserve
the extract for analysis. Metals allquots
must be acidified with nitric acid lo pll <2.
If precipitation Is observed upon addition of
nitric acid lo a small aliquot of the extract.
then Ihe remaining porllon of Ihe extract
'or metals analyses shall not be acidified
and the extract shall be analyzed as soon as
possible. All other allquots must be stored
under refrigeration (4 'C> until analyzed.
The TCLP extract shall be prepared and
analyzed according to appropriate analytical
methods. TCLP extracts to be analyzed for
metals shall be acid digested except In those
Instances where digestion causes loss of me-
tallic analytes. If an analysis of the iindl-
nested cxlracl shows that the concentration
Pt. 261, App. II
of any' regulated metallic analyle exceeds
Ihe regulatory level, then Ihe wasle Is haz-
ardous and digestion of Ihe exlracl Is nol
necessary. However, dala on undigested ex-
tracts alone cannot be used to demonstrate
that the waste is not hazardous. If the Indi-
vidual phases are lo be analyzed separately.
determine Ihe volume of the Individual
phases (lo •_': 0.5%). conduct Ihe appropriate
analyses, and combine the results mnlhe-
mallcally by u.stng a simple volumc-wclghl-
ed average:
Final Analyle
Concenlrallon
V, + V,
where:
Vi =The volume of Ihe flrsl phase (L).
Ci=Thc concentration of the analytc of
concern In the first phase (mg/L).
Vt^Thc volume of Ihe second phase (L).
Ci=The concentration of the analyte of
concern In the second phase (mg/L).
7.2.15 Compare the analyte concentra-
tions In the TCLP'exlracl with the levels
Identified In the appropriate regulations.
Refer to secllon 8.0 for quality assurance re-
quirements.
7.3 Procedure When Volatlles are In-
volved. Use Ihe ZHE device lo oblaln TCLP
cxlracl for analysis of volatile compounds
only. Exlract resulting from the use of Ihe
ZIIE shall nol be used lo evaluate the mo-
bility of nonvolatile analytes (e.g., metals.
pesticides, etc.).
The ZHE device has approximately a 500
mL Internal capacity. The ZHE can thus ac-
commodate a maximum of 25 grams of solid
(defined as that fraction of a sample from
which no additional liquid may be forced
out by an applied pressure of 50 psl), due lo
Ihe need lo add an amount of cxlracllon
fluid equal lo 20 times the weight of the
solid phase.
Charge Ihe ZHE with sample only once
and do nol open the device until the final
extracl (of the solid) has been collected. Re-
peated filling of the ZHE lo oblaln 25 grams
of solid Is not permitted.
Do nol allow the waste, the Initial liquid
phase, or the extract lo be exposed lo Ihe
atmosphere for any more lime than Is abso-
lutely necessary. Any manipulation of Ihcse
materials should be done when cold (4'C) to
minimize loss of volallles.
7.3.1 Pre-wclgh Ihe (evacualed) filtrate
collection container (See secllon 4.6) and scl
aside. If using a TEDLAU' bag. express all
liquid from Ihe ZHE device Into Ihe bag.
whether for Ihe Initial or final liquid/solid
separation, and take an aliquot from the
liquid In the bag for analysis. The contain-
ers listed In section 4.S are recommended for
-------
PI. 761, App. II
use under the conditions staled In sections
4.8.1-4.6.3.
1.3.2 Place the ZHE piston within the
body of the ZHE (It may be helpful first to
moisten the piston CD-rings slightly with ex-
traction fluid). Adjust the piston within the
ZHE body to a height that will minimize the
distance the piston will have to move once
the 7.IIE Is charged with snmplc (based
upon sample size requirements determined
from section 7.3, section 1.1.1 and/or 1.1.2).
Secure the gas Inlet/outlet flange (bottom
flange) onto the ZHE body In accordance
with the manufacturer's Instructions.
Secure the glass fiber filter between the
support screens and set aside. Set liquid
Inlet/outlet flange (top flantfc)'aslde.
7.3.3 If the waste Is 100% solid (sec sec-
tion 7.1.1). weigh out a subsample (25 gram
•p.S.f-^
40 CFR Ch.
(7-1-92 Edition)
maximum) of the waste, record weight, and
proceed to section 7.3.5.
7.3.4 If the waste contains <5% dry
solids (section 7.1.2). the liquid portion of
waste, after filtration. Is defined as the
TCLP extract. Filler enough of the sample
so thai the amount of filtered liquid will
support all of the volatile analyses required.
For wiuiles containing >f>% dry solids (sec-
lions 7.1.1 and/or '/.1.2). use Ihi: percent
solids Information obtained In section '/.I.I
to determine the optimum sample sl/.c to
charge Into the ZI1I5. The recommended
sample size Is as follows:
7.3.4.1 For wastes containing <5% solids
(see Section 7.1.1), weigh out a 500 grain
subsample of waste and record the weight.
1.3.4.2 For wastes containing > 5% solids
(sec Section 7.1.1), determine the amount of
waste In charge Into (he 71 IK n.s follows:
Weight of waste to charge 7HE =
25
xlOO
Weigh out a subsample of the waste of the
appropriate size and record the weight.
7.3.5 If particle size reduction of the solid
portion of the waste was required In section
7.1.3, proceed to section 7.3.8. If particle size
reduction was not required In section 7.1.3,
proceed to section 1.3.1.
1.3.6 Prepare the waste for extraction by
crushing, culling, or grinding Ihe solid por-
tion of Ihe waste to a surface area or parti-.
cle size as described In section 7.1.3.1.
Wastes and appropriate reduction equip-
ment should be refrigerated. If possible, to
4'C prior to particle size reduction. The
means used lo effect pnrtlcle size reduction
must not generate heal In and of Itself. If
reduction of Ihe solid phase of the waste Is
necessary, exposure of the waste to the at-
mosphere should be avoided to the extent
possible.
NOTE: Sieving of the waste Is not recom-
mended due to the possibility that volatlles
may be lost. The use of an appropriately-
graduated ruler Is recommended as an ac-
ceptable alternative. Surface area require-
ments are meant for filamentous (e.g.,
paper, cloth) and similar waste materials.
Actual measurement of surface area Is not
recommended.
When the surface area or particle size has
been appropriately altered, proceed lo sec-
lion 1.3.1.
1.3.7 Wasle slurries need nol be allowed
to Eland to permit the solid phase lo settle.
Do nol centrifuge wastes prior lo filtration.
7.3.8 Quantitatively transfer the entire
sample (liquid and solid phases) quickly lo
Ihe ZHE. Secure the filler and supporl
purcr.nl solids (suction 7.1.1)
screens onto the top flange of the device
anil secure the lop flange lo the 7.1 IE body
In accordance with the manufacturer's In-
slrucllons. Tighten all ZHE flltlngs uiul
place the device In the vertical position (gas
inlet/outlet flange on the bottom). Do not
attach the extract collection device to the
lop plate.
NOTE: If waste material (>1% of original
sample weight) has. obviously adhered to
the container used to transfer the sample to
the '/.HE, determine the welghl of this resi-
due and sublracl It from the sample weight
determined In section 7.3.4 to determine the
welghl of the waste sample that will be fil-
tered.
Attach a gas line to the gas Inlet/outlet
valve (bottom flannel and. with the liquid
Inlet/outlet valve (lop flange) open, begin
applying gcnllc pressure of 1-10 psl (or
more If necessary) lo force all hcadspacc
slowly out of the ZHE device Into a hood. At
the first appearance of Mould from the
liquid Inlet/outlet valve, quickly close the
valve and discontinue pressure. If filtration
of the waste al 4 'C reduces the amount of
expressed liquid over what would he ex-
pressed al room lempcralure, then allow
Die sample lo warm up to room temperature
In the device before filtering. If the waste Is
100% solid (sue section 7.1.1). slowly In-
crease the pressure to a maximum of 50 psl
lo force most of the hcadspacc out of Die
device and proceed lo section 7.3.12.
7.3.0 Attach the evacuated prc-wulghed
filtrate collection container lo the liquid
Inlet/outlet valve and open the valve. Begin
Environmental Protection Agency
applying gentle pressure of 1-10 psl lo force
the liquid phase of the sample Into the fil-
trate collection container. If no additional
liquid has passed through the filler In any 2
minule Interval, slowly Increase Ihe pres-
sure In 10 psl Increments lo a maximum of
50 psl. After each Incremental Increase of 10
psl. If no additional liquid has passed
through the filler In any 2 minute Interval.
proceed to the nexl 10 psl Increment. When
liquid flow has censed such that continued
pressure filtration al 50 psl dues not result
In any additional flllralc within a 2 minute
period, stop the llllrallon. Close Die liquid
Inlcl/outlcl valve, discontinue pressure lo
the piston, and disconnect and weigh the fil-
trate collection container.
NOTE: Instantaneous application of high
pressure can degrade the glass fiber filler
and inuy cause premature plugging.
V.II.IO The material In Die '/.ID1: Is defined
as thi: solid phase of the waste and Die: fil-
trate Is defined as Die liquid phase.
Welghl of extraction
fluid
' IC* "'PI. 261, App. II
NOTE: Some wastes, such as oily wastes
and some paint wastes, will obviously con-
tain some material that appears to be a
liquid. Even after applying pressure filtra-
tion, this material will not filler. If this Is
the case, the material within the filtration
device Is defined as a solid and Is carried
through Die TCL.P extraction as a solid.
If Die original waste contained <0.5% dry
solids (sec scr.llon '(.1.2). Dils filtrate Is de-
fined as the TCL.P extract and Is analyzed
directly. Proceed lo section 7.3.15.
7.3.11 The liquid phase may now be
either analyzed Immediately (See sections
7.3.13 through 1.3.15) or stored al 4'C under
minimal hcadspacc conditions until lime of
analysts.
Dclcrmlne the weight of extraction fluid
#1 lo add to the 7IIK an follows:
20xpercent solids (section
l.l.Dxwclghl of waste filtered
(suction 1.3.4 or 1.3.8)
100
7.3.12 The following suctions detail how
lo add the appropriate amount of extraction
fluid lo the solid material within the ZHE
and agllatlon of the ZHE vessel. Extraction
fluid #1 Is used In all cases (See section 5.7).
7.3.12.1 With the ZHE In Ihe vertical po-
sition, attach a line from the extraction
fluid reservoir lo Ihe liquid Inlet/outlet
valve. The line used shall contain fresh ex-
traction fluid and should he preflushcd with
fluid to eliminate any air pockets In Du:
line, llclea.se gas pressure on the /.lite
piston (from Die KO.S Inlet/outlet valve).
open the liquid Inlet/outlet valve, and begin
transferring extraction fluid (by pumping or
similar means) Into the ZIIE. Continue
pumping extraction fluid Into the XIIK until
the appropriate amount of fluid has been
Introduced Into the device.
1.3.12.2 After the exlraclion fluid has
been added. Immediately close the liquid
Inlcl/oullel valve and disconnect the extrac-
tion fluid line. Check the 7.I1K lo ensure
Hint nil valves are in their closed positions.
Manually rotate Die device In an end-ovcr-
cnd fashion 2 or 3 times. Deposition Die
'/.111': in the vertical position with the liquid
Inlel/oullel valve on lop. Pressurize Die
7MK to 5-10 psl (If necessary) and slowly
open the liquid Inlel/oullel valve lo hlecd
out any hcadspacc (Into a hood) Dial may
have been Introduced due lo the addition of
extraction fluid. This bleeding shall be done
quickly and shall be stopped at the first ap-
pearance of liquid from Die valve. Re-pres-
surlzc Die ZHE with 5-10 psl and check all
Zllr: fittings lo ensure Dial they are closed.
7.3.12.3 Place the ZHE In the rotary agl-
lallon apparatus (If It Is nol already there)
and rotate at 30 ± 2 rpm for 18 ± 2 hours.
Ambient lemperature (I.e., temperature of
room In which extraction occurs) shall be
maintained at 22 ± 3'C during agitation. <
7.3.13 Following the 111 :l: 2 hour agita-
tion period, check Die pressure behind Die
'/.HE piston by quickly opening and closing
Die gas Inlet/outlet valve and noting the
escape of gas. If the pressure has not been
maintained (I.e., no gas release observed).
Die device Is leaking. Check Ihe ZHE; for
leaking as specified In sccllon 4.2.1. and per-
form the extraction again with a new
sample of waste. If the pressure within Die
device has been maintained. Die material In
Die cxlractor vessel Is once again scparaled
Into Its component liquid and solid phases.
If the waslc contained an Initial liquid
phase, the liquid may be filtered directly
Into the same filtrate collection container
(I.e.. TKDIJVR' bag) holding the Initial
liquid phase of the waslc. A separate flllralc
collection container must be used If combin-
ing would crcalc multiple phases, or there Is
not enough volume left within the filtrate
collection container. Filler through the
glass fiber filter, using the ZHE device as
-------
ft. 261, App. II
dlaeuued In section 7.3.0. All extract shall
be filtered &nd collected If the TEDLAR'
bag la used. If the extract la multlphaalc, or
If the waste contained an Initial liquid phase
(see sections 4.6 and 7.3.1).
NOTI: An In-line glass fiber filter may be
used to filter the material within the ZHE If
It Is suspected that the gloss fiber filter has
been ruptured.
7.3.14 If the original waste contained no
.Initial liquid phase, the filtered liquid mate-
rial obtained from section 7.3.13 Is defined
as the'TCLP. extract. If the waste contained
an Initial liquid .phase, the filtered liquid
material obtained from • section 7.3.13 and
. the Initial- liquid- phase (section 7.3.9) are
collectively defined as the TCt£* extract.
7.3.16 Following collection of the TCLP
extract. Immediately prepare the extract for
analysis and store with minimal hendspace
at 4'C until analyzed. Analyze the TCL.I' ex-
tract according to the appropriate analytical
methods. If the Individual phases are to be
analyzed separately (I.e.. are not mlsclble).
determine the volume of the Individual
. phases (to 0.5%), conduct the appropriate
analyses, and combine the results.mathe-
matically by using a simple volume-weight-
ed average:
Final Anallye
Concentration
V. + V.
40 CFR Ch. I (7-1-92 Edition)
ijptke Addition guidance provided In each an-
alytical method.
8.2.1 Matrix spikes are to be added after
filtration of the TCLP extract and before
preservation. Matrix spikes should not be
added prior to TCLP extraction of the
sample.
8.2.2 In moat cases, matrix spikes should
be added nt a concentration equivalent to
the corresponding regulatory level. If the
analyte concentration Is less than one hulf
the regulatory level, the spike concentration
.. may be as low as one half of the analyte
concentration, but may not be not less than
• five times the method detection limit. In
order to avoid differences In matrix effects,
• the matrix spikes must be added to the
same'nominal volume of TCl.r extract as
that which was analyzed tor the unsplked
sample.
0.2.3 The purpose of the matrix Rplke Is
to monitor the performance of the analyti-
cal methods used, and to determine whether
matrix Interferences exist. Use of other In-
ternal calibration methods, modification of
the analytical methods, or use of alternate
analytical methods may be needed to accu-
rately measure the analyte concentration of.
the TCLP extract when the recovery of the
matrix spike Is below the expected analyti-
cal method performance.
8.2.4. Matrix spike recoveries are calculat-
ed by the following formula:
%Il (% necovery)=100 (X.-XJ/K
where:
Vi-The volume of the first phases (L).
Ci-The concentration of the onalyte of
concern In the first phase (mg/L).
Vi-The volume of the second phase (L).
Ci-The concentration of the analyte of
. concern In the second phase (mg/L).
7.3.16 Compare the analyte concentra-
tions In the TCLP extract with the levels
Identified In the appropriate regulations.
Refer to section 8.0 for quality assurance re-
quirements.
8.0 Quality Assurance
8.1 A minimum of one blank (using the
same extraction fluid as used for the sam-
ples) must be analyzed for every 20 extrac-
tions that have been conducted In an extrac-
tion vessel.
8.2 A matrix spike shall be performed for
each waste type (e.g., wostewater treatment
sludge, contaminated soil, etc.) unless the
result exceeds the regulatory level and the
data Is being used solely to demonstrate
that the waste properly exceeds the regula-
tory level. A minimum of one matrix spike
must be analyzed for each analytical batch.
The bias determined from the matrix spike
determination shall be used to correct the
measured values. (See sections 8.2.4 and
8.2.5.) As a minimum, follow the matrix
where:
X.=mcasured value for the spiked sample,
Xu = meosured value for the unsplked
sample, and
K= known value of the spike In the sample
8.2.5 Measured values are corrected (01
analytical bias using the following formula
where:
X.ucorrectcd value, and
X,, = mcasurcd value of the unsplked sainpli
8.3 All quality control measures de-
scribed In the appropriate analytical meth-
ods shall be followed.
8.4 Samples must undergo TCLP extrac-
tion within the following time periods:
SAMPLE MAXIMUM HOLDING TIMES o
NA
From',
prepara-
extraction
cwlotml
emalym
1BO
Total
oiapaod
tmiu
360
HA-Not applicable.
If sample holding times are exceed-
ed, the values obtained will be consid-
ered minimal concentrations. Exceed-
ing the holding time Is not acceptable
In establishing that a waste does not
exceed the regulatory level. Exceeding
the holding time will not Invalidate
characterization If the waste exceeds
the regulatory level.
TABLE 1—VOLATILE ANALYTES '•*
Compound
U -Dichlofoelnytone
Ethyl tciUta .
IwtxiUrx))
Uiihary*
Utuiylono chkvtrio
Uot!iyl othyl koton*
Uetbyi itobutyt keione
1sbichloroethyton«
To-utrw.
TncHorooihyton*
TnchlofOlluoromolhano
U.2-Tnchtofo-1 2 2-Uiflooroethin*
Vnyi cWondo
Xytww..
CAS No.
67-64-1
71-43-2
71-36-3
75-15-0
56-23-5
106-00-7
67-66-3
107-O6-2
75-35-4
141-76-6
100-4t-4
67-50-1
75-00-2
78 03-3
106-10-1
127-16-4
106-86-3
71-55-6
70-01-6
75-60-4
76-13-1
1 Whan tosling lor any or •!) of those anatytos, the 1010-
^••dipace oitiactor vessel ahall bo usod insload ol the
""TOo e.Uiclor.
'Beniene. carbon letrachlorlde. chlorobenzene. chloro-
«"n. 1,2-dichloiolhano. M-dichloroolhylene. mothyl olhyl
'•Una. lotiacliloroolhylana. tilchloroolhylene. and vinyl chlo-
«* «a loandria VA.
(703) &49-JON.
Wnitmore Lake,
Ml. (313) 440-
4118.
Bodlord. MA,
(BOO) 225-3314.
Lynchburg. VA,
(8O4) 945-9424.
Model Mo.
C102. Mechanical
Pretsure
Devic«. '
3745-2HE. Gai
Pressure
Oevic*.
ZHE-11, Gas
Pressure
Device.
YT30000HW. Gaa
Pressure
Device.
VOLA-TOX1. G«
Pressure
Device.
1 Any devicA that m»ais ln« specifications Usted In SAction
4.2.1. ol Iht method it accApubla.
• This dovice u&ot • 1 10 mm
TADLE A—SUITABLE FILTER HOLDERS
Company
Nucleopore
Corpora-
lion
Location
Ptoasanion.
CA. (800)
882-
7711.
Model/catalogue
No.
425810
410400
Siie
142mm,
47 mm.
-------
PI. 261, App. II
TABLE 4—SUITABLE FILTER HOLDERS '—
Continued
Company
Mlcio
Filtration
Byatamt.
Uttipara
Corpora-
Don. ,
Location
Dublin. CA,
(800)
334-
7102.
HIS)
B28-
6010.
Bxttonl.
UA.
(WO)
n s-
3304.
' Aov u4wfc* rtftfiAi nl
phaaa Ol th« »UU la auft
company* «(m itw wuu
MooX/ciulogiM
No.
302400
311400
YT30142HW
XX10O4700
Siio
142 mm.
47 nvn.
14Z mm.
47 mm.
MpwtUng In* HqiM from Itx «oW
«!*.. pravidkig thai « tl cnwrOcaDy
Mid th« conslhuanta to b« «na-
40 CFR Ch. I (7-1-92 Edition)
tyied. Plailie davteei (not Itaied abovo) moy bo usod when
only inotganic tnitylos aro o( concern. The U2 mm tli«
tiller holdof is racommandod.
TABLE 5—SUITABLE FILTER MEDIA l
Envlronmontaf Protection Agency
Pt. 261, App. II
Company
Milllpoio
GofporilLon.
Nucleopofo
Corporation.
Laboratory
Producti. Inc..
Miao Filuatkw
Syilama.
location
flod'ord. MA.
(300) 22S-33«4.
Pleaftanlon. CA.
(415) 463-2530.
Clillon. NJ. (201)
773-5400.
Dublin. CA, (600)
334-7132. (415)
826-eOIO.
Modol
AP40
2I182S
OFF
OF75
Poro
Size
(iirn)
0.7
0.7
. 0.7
0.7
1 Any Mter thai mo«U tha «p«clftcetk>ni In »*ctioo 4.4 of
th« Meinod te luitAbU.
(Extraction Vats«l Holdar
'
Figure 1. Rotary Agitation Apparatus
-------
Pt. 261, App. II
Top Flange—i
Support Scree
Fitter
Support Screerr
Vlton o-rings
Bottom Rang*
Preaaurlzed Gaa-
Inlet/Outlat Valve
40 CFR Ch. I (7-1-92 Edition)
Liquid Inlet/Outlet valve
MI
U • "•• >'.- ' ',',"'
I t I ' '- ' * ' I
",- y '. , ,'v ^v '
Piston
Qaa
Pressure
Gauge
Envlronmanlal Protection Agency
METHOD 1311
TOXICITY CHARACTERISTIC LEACHATE PROCEDURE
Pt. 261, App. II
Extract with
appropriate fluid
1) Bottle extractor
for non-volaliles
2) ZHE device (or
volatiles
Reduce
particle size
to <9.5 mm
-------
METHOD 1311
TOXICITY CHARACTERISTIC LEACHING PROCEDURE
1.0 SCOPE AND APPLICATION
1.1 The TCLP 1s designed to determine the mobility of both organic and
Inorganic analytes present 1n liquid, solid, and multlphasic wastes.
1.2 If a total analysis of the waste demonstrates that Individual
analytes are not present 1n the waste, or that they are present but at such low
concentrations that the appropriate regulatory levels could not possibly be
exceeded, the TCLP need not be run.
1.3 If an .analysis of any one of the liquid fractions of the TCLP
extract indicates that a regulated compound is present at such high-concentra-
tions that, even after accounting for dilution from the other fractions of the
extract, the concentration would be above the regulatory level for that compound,
then the waste 1s hazardous and it 1s not necessary to analyze the remaining
fractions of the extract.
1.4 If an analysis of extract obtained using a bottle extractor shows
that the concentration of any regulated volatile analyte exceeds the regulatory
level for that compound, then the waste is hazardous and extraction using the ZHE
is not necessary. However, extract from a bottle extractor cannot be used to
demonstrate that the concentration of volatile compounds 1s below the regulatory
level. • :
2.0 SUMMARY OF METHOD
2.1 For liquid wastes (LJL., those containing less than 0,5% dry solid
material), the waste, after filtration through a 0.6 to 0.8 p,m glass fiber
filter, 1s defined'as the TCLP extract.
2.2 For wastes containing greater than or equal to 0,5% solids, the
liquid, if any, 1s separated from the solid phase and stored for later analysis;
the particle size of the solid phase is reduced, 1f necessary. The solid phase
1s extracted with an amount of extraction fluid equal to 20 times the weight of
the solid phase. The extraction fluid employed is a function of the alkalinity
of the solid phase of the waste. A special extractor vessel 1s used when testing
for volatile analytes (see Table 1 for a list of volatile compounds). Following
extraction, the liquid extract 1s separated from the solid phase by filtration
through a 0.6 to 0:8 jum glass fiber filter.
2.3 If compatible (i.e.. multiple phases will not form on combination),
the Initial liquid phase of the waste 1s added to the liquid extract, and these
are analyzed together. If incompatible, the liquids are analyzed separately and
the results are mathematically combined to yield a volume-weighted average
concentration.
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3.0 INTERFERENCES
3.1 Potential- Interferences that may be encountered during analysis are
discussed In the Individual analytical methods.
4.0 APPARATUS AND MATERIALS
4,1 Agitation apparatus: The agitation apparatus must be capable of
rotating the extraction vessel in an end-over-end fashion (see Figure 1) at
30 ± 2 rpm. Suitable devices known to EPA are Identified in Table 2.
4.2 Extraction Vessels
4.2.1 Zero-Headspace Extraction Vessel (ZHE). This device is
for use only when the waste 1s being tested for the mobility of volatile
analytes (i.e.. those listed in Table 1). The ZHE (depicted 1n Figure 2)
allows for liquid/solid separation within the device, and effectively
precludes headspace. This type of vessel allows for initial liquid/solid
separation, extraction, and final extract filtration without opening the
vessel (see Section 4.3.1). The vessels shall have an internal volume of
500-600 ml, and be equipped to accommodate a 90-110 mm filter. The devices
contain VITON*1 0-rings which should be replaced frequently. Suitable ZHE
devices known to EPA are identified 1n Table 3.
For the ZHE to be-acceptable for use, the piston within the ZHE
should be able to be moved with approximately 15 psi or less. If it takes
more pressure to move the piston, the 0-rings 1n the device should be
replaced. If this does not solve the problem, the ZHE is unacceptable for
TCLP analyses and the manufacturer should be contacted.
The ZHE should be checked for leaks after every extraction. If the
device contains a built-in pressure gauge, pressurize the device to
50 psi, allow it to stand unattended for 1 hour, and recheck the pressure.
If the device does not have a built-in pressure gauge, pressurize the
device to 50 psi, submerge it in water, and check for the presence of air
bubbles escaping from any of the fittings. If pressure is lost, check all
fittings and inspect and replace 0-rings, if necessary. Retest the
device. If leakage problems cannot be solved, the manufacturer should be
contacted.
Some ZHEs use gas pressure to actuate the ZHE piston, while others
use mechanical pressure (see Table 3). Whereas the volatlles procedure
(see Section 7.3) refers to pounds per square inch (psi), for the
mechanically actuated piston, the pressure applied 1s measured in
torque-inch-pounds. Refer to the manufacturer's instructions as to the
proper conversion.
1 VITON* Is a trademark of Du Pont.
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4.2.2 Bottle Extraction Vessel. When the waste 1s being
evaluated using the nonvolatile extraction, a Jar with sufficient capacity
to hold the sample and the extraction fluid Is needed. Headspace 1s
allowed in this vessel.
The extraction bottles may be constructed from various materials,
depending on the analytes to be analyzed and the nature of the waste (see
Section 4.3.3). It 1s recommended that borosHlcate glass bottles be used
Instead of other types of glass, especially when inorganics are of
concern. Plastic bottles, other^than polytetrafluoroethylene, shall not
be used if organics are to be investigated. Bottles are available from a
number of laboratory suppliers. When this type of extraction vessel is
used, the filtration device discussed in Section 4.3.2 is used for Initial
liquid/solid separation and final extract filtration.
.4.3 Filtration Devices: It is recommended that all fUtrations be
performed in a hood,
4.3.1 Zero-Headspace Extractor Vessel (ZHE): When the waste is
1 evaluated for volatiles, the zero-headspace extraction vessel described in
Section 4.2,1 is used for filtration. The device shall be capable of
supporting and keeping in place the glass fiber filter and be able to
withstand the pressure needed to accomplish separation (50 psi). .
NOTE: When it 1s suspected that the glass fiber filter has been ruptured,
an in-line glass fiber filter may be used to filter the. material
within the ZHE.
4.3.2 ' Filter Holder: When the waste is evaluated for other than
volatile ahalytes, any filter holder capable of supporting a glass fiber
filter and able to withstand the pressure needed to accomplish separation
may be used. Suitable filter holders range from simple vacuum units to
relatively complex systems capable of exerting pressures of up to 50 psi
or more. The type of filter holder used depends on the properties of the
material to be filtered (see Section 4.3.3). These devices shall have a
minimum internal volume of 300 ml and be equipped to accommodate a minimum
•filter size of 47 mm (filter holders having an internal capacity of 1.5 L
or greater, and equipped to accommodate a 142 mm diameter filter, are
recommended). Vacuum filtration can only be used for wastes with low
solids content (<10%) and for highly granular, liquid-containing wastes.
All other types of wastes should be filtered using positive pressure
filtration. Suitable filter holders known to EPA are shown in Table 4.
4.3.3 Materials of Construction: Extraction vessels and
filtration devices shall be made of inert materials which will not leach
or absorb waste components. Glass, polytetrafluoroethylene (PTFE), or
type 316 stainless steel equipment may be used when evaluating the
mobility of both organic and inorganic components. Devices made of high
density polyethylene (HOPE), polypropylene (PP), or polyvinyl chloride
(PVC) may be used only when evaluating the mobility of metals. Borosili-
cate glass, bottles are recommended for use over other types of glass
bottles, especially when inorganics are analytes of concern.
•
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4,4 Filters: Filters shall be made of borosilicate glass fiber, shall
contain no binder materials, and shall have an effective pore size of 0.6 to
0.8 Aim, or equivalent.1 Filters known to EPA which meet these specifications are
Identified in Table S. Pre-fHters must not be used. When evaluating the
mobility of metals, filters shall be acid-washed prior to use by rinsing with IN
nitric add followed by three consecutive rinses with deionlzed distilled water
(a minimum of 1 L per rinse is recommended), Glass fiber filters are fragile and
should be handled with care. . "
4.5 pH Meters: The meter should be accurate to ± 0.05 units at 25 'C.
4.6 2HE Extract Collection Devices: TEDLAR*2 bags or glass, stainless
steel or PTFE gas-t1gnt syringes are used to collect the initial liquid phase and
the final extract of the waste when using the ZHE device. The devices listed are
recommended for use under the following conditions:
4.6.1 . If a waste contains an aqueous liquid phase or 1f a waste
does not contain a significant amount of nonaqueous liquid (1 .e.t <1% of
total waste), the TEDLAR bag or a 600 ml syringe should be used to collect
and combine the initial liquid and solid extract.
4.6.2 If a waste contains a significant amount of nonaqueous
liquid 1n the initial liquid phase (i.e., >1% of total waste), the syringe
or the TEDLAR* bag may be used for both the initial solid/liquid separation
and the final extract filtration. However, analysts should use one or the
other, not both.
.4.6.3 If the-waste contains no initial liquid phase (is 100%
solid^or has no significant solid phase (is 100% liquid), either the
TEDLAR* bag or the syringe may be used. If the syringe is used, discard
the first 5 mL of liquid expressed from the device. The remaining
aliquots are used for analysis.
4.7 ZHE Extraction Fluid .Transfer Devices: Any device capable of
transferring the extraction fluid into the ZHE without changing the nature of the
extraction fluid is acceptable (e.g.. a positive displacement or peristaltic
pump, a gas tight syringe, pressure filtration unit (see Section 4.3.2), or other
ZHE device).
4.8 Laboratory Balance: Any laboratory balance accurate to within
± 0.01 grams may be used (all weight measurements are to be within ±0.1 grams).
flask.
4.9 Beaker or Erlenmeyer flask, glass, 500 ml.
4.10 Hatchglass, appropriate diameter to cover beaker or Erlenmeyer
2
TEDLAR* is a registered trademark of Du Pont.
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4.11 Magnetic stlrrer,
5.0 REAGENTS
5.1 Reagent grade chemicals shall be used 1n all tests. Unless
otherwise Indicated, 1t 1s Intended that all reagents shall conform to the
specifications of the Committee on Analytical Reagents of the American Chemical
Society, where such specifications are available. Other grades may be used,
provided it is first ascertained that the reagent is of sufficiently high purity
to permit Its use without lessening the accuracy of the determination.
5.2 Reagent Water. Reagent water is defined as water in which an
interferant 1s not observed at or above the method's detection limit of the
analyte(s) of interest. For nonvolatile extractions, ASTH Type II water or
equivalent meets the definition of reagent water. For volatile extractions, it
1s recommended that reagent water be generated by any of the following methods.
Reagent water should be monitored periodically for Impurities.
5.2.1 Reagent water for volatile extractions may be generated
by passing tap water through a carbon filter bed containing about 500
grams of activated carbon (Calgon Corp., Filtrasorb-300 or equivalent).
5.2.2 A water purification system (Millipore Super-Q or
equivalent) may also be used to generate reagent water for volatile
extractions.
5.2.3 Reagent water for volatile extractions may also be
prepared by boiling water for 15 minutes. Subsequently, while maintaining
the water temperature at 90'± 5 degrees C, bubble a contaminant-free Inert
gas (e.g. nitrogen) through the water for 1 hour. While still hot,
transfer the water to a narrow mouth screw-cap bottle under zero-headspace
and seal with a Teflon-lined septum and cap.
5.3 Hydrochloric acid (IN), HC1, made from ACS reagent grade.
5.4 Nitric acid (IN), HN03, made from ACS reagent grade.
5.5 Sodium hydroxide (IN), NaOH, made from ACS reagent grade.
5.5 Glacial acetic acid, CH3CH2OOH» ACS reagent grade.
5.7 Extraction fluid.
5.7.1. Extraction fluid # 1: Add 5.7 ml glacial CH3CH2OOH to
500 ml of reagent water (See Section 5.2), add 64.3 mL of IN NaOH, and
dilute to a volume of 1 liter. When correctly prepared, the pH of this
fluid will be 4.93 ± 0.05.
5.7.2 Extraction fluid * 2: Dilute 5.7 ml glacial CH3CH2OOH with
reagent water (See Section 5.2) to a volume of 1 liter. When correctly
prepared, the pH of this fluid will be 2.88 ± 0.05.
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NOTE: These extraction fluids should be monitored frequently for
Impurities, The pH should be checked prior to use to ensure that
these fluids are made up accurately." If Impurities are found or
the pH is not within the above specifications, the fluid shall be
discarded and fresh extraction fluid prepared.
5.8 Analytical standards shall be prepared according to the appropriate
analytical method.
6.0 SAMPLE COLLECTION, PRESERVATION, AND HANDLING
6,1 All samples shall be collected using an appropriate sampling plan.
6.2 The TCLP may place requirements on the minimal size of the field
sample, depending upon the physical state or states of the waste and the analytes
of concern. An aliqugt Is needed for preliminary evaluation of which extraction
fluid is to be used for the nonvolatile analyte extraction procedure. Another
aliquot may be needed to actually conduct the nonvolatile extraction {see Section
1.4 .concerning the use of this extract for volatile organlcs). If volatile
organics are of concern, another aliquot may be needed. Quality control measures
may require additional aliquots. Further, it 1s always wise to collect more
sample Just 1n case something goes wrong with the initial attempt to conduct the
test.
6.3 Preservatives shall not be added to samples before extraction.
6.4 Samples may be refrigerated unless refrigeration results in
irreversible physical change to the waste. If precipitation occurs, the entire
sample (including precipitate) should be extracted.
6.5 When the waste is to be evaluated for volatile analytes, care shall
be taken to minimize the loss of volatile*. Samples shall be collected and
stored in a manner Intended to prevent the loss of volatile analytes (e.g..
samples should be collected in Teflon-lined septum capped vials and stored at 4
*C. Samples should be opened only immediately prior to extraction).
6.6 TCLP extracts should be prepared for analysis and analyzed as soon
as possible following extraction. Extracts or portions of extracts for metallic
analyte determinations must be acidified with nitric add to a pH < 2, unless
precipitation occurs (see Section 7.2.14 if precipitation occurs). Extracts
should be preserved for other analytes according to the guidance given in the
individual analysis methods. Extracts or portions of extracts for organic
analyte determinations shall not be allowed to come Into contact with the
atmosphere (i.e.. no headspace) to prevent losses. See Section 8.0 (QA
requirements) for acceptable sample and extract holding times.
7.0 PROCEDURE
7.1 Preliminary Evaluations
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Perform preliminary TCLP evaluations on.a minimum 100 gram aliquot of
waste. This aliquot may not actually undergo TCLP extraction. These preliminary
evaluations Include: (1) determination of the percent solids (Section 7.1.1);
(2) determination of whether the waste contains Insignificant solids and 1s,
therefore, Its own extract after filtration (Section 7.1.2); (3) determination
of whether the solid portion of the waste requires particle size reduction
(Section 7.1.3); and (4) determination of which of the two extraction fluids are
to be used for the nonvolatile TCLP extraction of the waste.(Section 7.1.4).
7.1.1 Preliminary determination of percent sol Ids: Percent
sol Ids is defined as that fraction of a waste sample (as a percentage of
the total sample) from which no liquid may be forced out by an applied
pressure, as described below.
7.1.1.1 If the waste will obviously yield no liquid when
subjected to pressure filtration (1.e.. 1s 100% sol Ids) proceed to
Section 7.1.3.
7.1.1.2 If the sample is liquid or multiphasic,
liquid/solid separation to make a preliminary determination of
percent solids is required. This involves the filtration device
described in Section 4.3.2 and is outlined in Sections 7.1.1.3
through 7.1.1.9.
7.1.1.3 Pre-we1gh the filter and the container that will
receive the filtrate,
7.1.1.4 Assemble the filter holder and filter following
the manufacturer's instructions. Place the filter on the support
screen and secure. "~ - -
7.1.1.5 Weigh out a subsample of the waste (100 gram
minimum) and record the weight:
7.1.1.6 Allow slurries to stand to permit the solid
phase to settle. Hastes that settle slowly may be centrifuged
prior to filtration. Centrifugatlon is to be used only as an aid
to filtration. If used, the liquid should be decanted and filtered
followed by filtration of the solid portion of the waste through
the same filtration system.
7.1.1.7 Quantitatively transfer the waste sample to the
filter holder (liquid and solid phases). Spread the waste sample
evenly over the surface of the filter. If filtration of the waste
at 4 *C reduces the amount of expressed liquid over what would be
expressed at room temperature then allow the sample to warm up to
room temperature In the device before filtering.
NOTE: If waste material {>!% of original sample weight) has obviously
adhered to the container used to transfer the sample to the
filtration apparatus, determine the weight of this residue and
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subtract it from the sample weight determined in Section 7.1.1.5 to
determine the weight of the waste sample that will be filtered.
Gradually apply vacuum or gentle pressure of 1-10 psi,
until air or pressurizing gas moves through the filter. If this
point is not reached under 10 psi, and if no additional liquid has
passed through the filter 1n any 2 minute Interval, slowly increase
the pressure in 10 psi increments"to a maximum of 50 psi. After
each incremental increase of 10 psi, if the pressurizing gas has
not moved through the filter, and if no additional liquid has
passed through the filter in any 2 minute interval, proceed to the
next 10 psi increment. When the pressurizing gas begins to move
through the filter, or when liquid flow has ceased at 50 psi (i.e..
filtration does not result in any additional filtrate within any 2
minute period), stop the filtration.
NOTE: Instantaneous application of high pressure can degrade the glass
fiber filter and may cause premature plugging.
7.1.1.8 The material in the filter holder 1s defined as
the solid phase of the waste, and the filtrate is defined as the
liquid phase.
NOTE: Some wastes, such as oily wastes and some paint wastes, will
obviously contain some material that appears to be a liquid. Even
after applying vacuum or pressure filtration, as outlined 1n
Section 7.1.1.7, this material may not filter. If this is the
case, the material within the filtration device is defined as a
solid. Do not replace the original filter with a fresh filter
under any circumstances. Use only one filter.
7.1.1.9 Determine the weight of the liquid phase by
subtracting the weight of the filtrate container (see Section
7.1.1.3) from the total weight of the filtrate-filled container.
Determine the weight of the solid phase of the waste sample by
subtracting the weight of the liquid phase from the weight of the
total waste sample, as determined in Section 7.1.1.5 or 7.1.1.7.
Record the weight of the liquid and solid phases.
Calculate the percent solids as follows:
Weight of solid (Section 7.1.1.9)
Percent solids - : x 100
Total weight of waste (Section 7.1.1.5 or 7.1.1.7)
7.1.2 . If the percent solids determined in Section 7.1.1.9 1s
equal to or greater than 0.5%, then proceed either to Section 7.1.3 to
determine whether the solid material requires particle size reduction or
to Section 7.1.2.1 if 1t is noticed that a small amount of the filtrate 1s
entrained 1n wetting of the filter. If the percent solids determined in
Section 7.1.1.9 4s less than 0.5%, then proceed to Section 7.2.9 1f the
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nonvolatile TCLP is to be performed and to Section 7.3 with a fresh
portion of the waste if the volatile TCLP Is to be performed.
7.1.2,1 Remove the solid phase and filter from the
filtration apparatus,
7.1,2.2 Dry the filter and solid phase at 100 ± 20 'C
until two successive weighing yield the same value within ±.1%.
Record the final weight.
NOTE: Caution should be taken to ensure that the subject solid will not
flash upon heating. It is recommended that the drying oven be
vented to a hood or other appropriate device.
7.1.2.3 Calculate the percent dry solids as follows:
(Wt. of dry waste + filter) - tared wt. of filter
Percent dry solids • x 100
Initial wt. of waste (Section 7.1.1,5 or 7.1.1.7)
7.1.2.4 If the percent dry solids is less than 0.5%,
then proceed to Section 7.2.9 if the nonvolatile TCLP is to be
performed, and to Section 7.3 if the volatile TCLP 1s to be
performed. If the percent dry solids is greater than or equal to
0.5%, and 1f the nonvolatile TCLP is to be performed, return to the
beginning of this Section (7.1) and, with a fresh portion of waste,
determine whether particle size reduction is necessary (Section
7.1.3) and determine the appropriate extraction fluid (Section
7.1.4). If only the volatile TCLP 1s to be performed, see the note
in Section 7.1.4. "
7.1.3 Determination of whether the waste requires particle size
•reduction (particle size 1s reduced during this step): Using the solid
portion of the waste, evaluate the solid for particle size. Particle size
reduction 1s required, unless the solid has a surface area per gram of
material equal to or greater than 3.1 cm2, or 1s smaller than 1 cm in its
narrowest dimension h.e.. is capable of passing through a 9,5 mm (0.375
Inch) standard sieve). If the surface area is smaller or the particle
size larger than described above, prepare the solid portion of the waste
for extraction by crushing, cutting, or grinding the waste to a surface
area or particle size as described above. .If the solids are prepared for
organic volatlles extraction, special precautions must be taken (see
Section 7.3.6).
NOTE: Surface area criteria are meant for filamentous (e.g.. paper, cloth, and
similar) waste materials. Actual measurement of surface area is not
required, nor 1s it recommended. For materials that do not obviously meet
the criteria, sample specific methods would need to be developed and
employed to measure the surface area. Such methodology 1s currently not
available.
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7.1.4 Determination of appropriate extraction fluid: If the
solid content of the waste is greater than or equal to 0.5% and if the
sample will be extracted for nonvolatile" constituents (Section 7.2),
determine the appropriate fluid (Section 5.7) for the nonvolatile?
extraction as follows:
NOTE: TCLP extraction for volatile constituents uses only extraction
fluid #1 (Section 5.7.1). Therefore, 1f TCLP extraction for
nonvolatiles is not required, proceed to Section 7.3.
7.1.4.1 Weigh out a small subsample of the solid phase
of the waste, reduce the solid (1f necessary) to a particle size of
approximately 1 mm in diameter or less, and transfer 5.0 grams of
the solid phase of the waste to a 500 ml beaker or Erlenmeyer
flask.
.7.1.4.2 Add 96.5 ml of reagent water to the beaker,
cover with a watchglass, and stir vigorously for 5 minutes using a
magnetic stlrrer. Measure and record the pH. If the pH is <5.0,
use extraction fluid #1. Proceed to Section 7.2.
7.1.4.3 If the pH from Section 7.1.4.2 is >5.0, add
3.5 ml IN HCl, slurry briefly, cover with a watchglass, heat to 50
•C, and hold at 50 'C for 10 minutes.
7,1.4.4 Let the solution cool to room temperature and
record the pH. If the pH is <5.0, use extraction fluid #1. If the
pH 1s >5.0, use extraction fluid #2. Proceed to Section 7.2,
7.1.5 If the aliquot of the waste used "for the preliminary
evaluation (Sections 7.1.1 - 7.1.4) was determined to be 100% solid at
Section 7.1.1.1, then 1t can be used for the Section 7.2 extraction
(assuming at least 100 grams remain), and the Section 7.3 extraction
(assuming at least 25 grams remain). If the aliquot was subjected to the
procedure in Section 7.1.1.7, then another aliquot shall be used for the
volatile extraction procedure 1n Section 7.3. The aliquot of the waste
subjected to the procedure in Section 7.1.1.7 might be appropriate for use
for the Section 7.2 extraction if an adequate amount of solid (as
determined by Section 7.1.1.9) was obtained. The amount of solid
necessary is dependent upon whether a sufficient amount of extract will be
produced to support the analyses. If an adequate amount of solid remains,
proceed to Section 7,2.10 of the nonvolatile TCLP extraction.
7.2 Procedure When Volatlles are not Involved
A minimum sample size of 100 grains (solid and liquid phases) is recommend-
ed, In some cases, a larger sample size may be appropriate, depending on the
solids content of the waste sample (percent solids, See Section 7.1.1), whether
the initial liquid phase of the waste will be misclble with the aqueous extract
of the solid, and whether Inorganics, semivolatile organics, pesticides, and
herbicides are all analytes of concern. Enough.solids should be generated for
extraction such that the volume of TCLP extract will be sufficient to support all
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of the analyses required. If the amount of extract generated by a single TCLP
extraction will not be sufficient to perform all of the analyses, more than one
extraction may be performed and the extracts from" each combined and all quoted for
analysis.
7.2.1 If the waste will obviously yield no liquid when subjected
to pressure filtration M.e.. is 100% solid, see Section 7.1.1), weigh out
a subsample of the waste (100 gram minimum) and proceed to Section 7.2.9.
7.2.2 If the sample is liquid or multiphasic, liquid/solid
separation 1s required. This Involves the filtration device described 1n
Section 4.3.2 and is outlined 1n Sections 7.2.3 to 7.2.8.
»
7.2.3 Pre-we1gh the container that will receive the.filtrate.
7.2.4 Assemble the filter holder and filter following the
manufacturer's instructions. Place the filter on the support screen and
secure. Acid wash the filter 1f evaluating the mobility of metals (see
Section 4.4),
NOTE: Acid washed filters may be used for all nonvolatile extractions
even when metals are not of concern.
7.2.5 Heigh out a subsample of the waste (100 gram minimum) and
record the weight. If the waste contains <0.5% dry sol Ids (Section
7.1.2), the liquid portion of the waste, after filtration, is defined as
the TCLP extract. Therefore, enough of the sample should be filtered so
that the amount of filtered liquid will support all of the analyses
required of the TCLP extract. For wastes containing >Q.5% dry solids
(Sections 7.1/1 or 7.1.2), use the percent solids information, obtained 1n
Section'7.1.1 to determine the optimum sample size (100 gram minimum) for
filtration. Enough solids should be generated by filtration to support
the analyses to be performed on the TCLP extract.
7.2.6 Allow slurries to stand to permit the solid phase to
settle. Wastes that settle slowly may be centrifuged prior to filtration.
Use centrifugatlon only as an aid to filtration. If the waste is
centrifuged, the liquid should be decanted and filtered followed by
filtration of the solid portion of the waste through the same filtration
system.
7.2.7 Quantitatively transfer the waste sample (liquid and solid
phases) to the filter holder (see Section 4.3.2). Spread the waste sample
evenly over the surface of the filter. If filtration of the waste at 4 *C
reduces the amount of expressed liquid over what would be expressed at
room temperature, then allow the sample to warm up to room temperature in
the device before filtering.
NOTE: If waste material (>1% of the- original sample weight) has obviously
adhered to the container used to transfer the sample to . the
filtration apparatus, determine the weight of this residue and
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subtract 1t from the sample weight determined 1n Section 7.2.5, to
determine the weight of the waste sample that will be filtered.
Gradually apply vacuum or gentle pressure of 1-10 ps1, until air or
pressurizing gas moves through the filter. If this point 1s not reached
under 10 ps1, and if no additional liquid has passed through the filter in
any 2 minute interval, slowly Increase the pressure 1n 10 ps1 Increments
to a maximum of 50 psi. After each Incremental Increase of 10 psi, if the
pressurizing gas has not moved through the filter, and if no additional
liquid has passed through the filter in any 2 minute interval, proceed to
the next 10 ps1 Increment. When the pressurizing gas begins to move
..through the filter, or when the liquid flow has ceased at 50 ps1 (I.e.,
.;f1l.tr:at1on does not result in any additional filtrate within a 2 minute
the filtration.
, .•:.-.•!•.•'.'•
•• •• J:~-.- •.
NOTE: Instantaneous application of high pressure can degrade the glass
fiber filter and may cause premature plugging.
7.2.8 The material in the filter holder is defined as the solid
phase of the waste, and the filtrate is defined as the liquid .phase.
Weigh the filtrate. The liquid phase may now be either analyzed (See
Section 7.2.12) or stored at 4 *C until time of analysis.
NOTE: Some wastes, such as oily wastes and some paint wastes, will
obviously contain some material that appears to be a liquid. Even
after applying vacuum or pressure nitration, as outlined 1n
Section 7.2.7, this material may not filter. If this is the case,
the material within the filtration device is defined as a solid and
1s carried through the extraction as a solid. Do not replace the
original filter with a"fresh filter under any circumstances. Use
only one filter.
7.2.9 If the waste contains <0.5% dry solids (see Section
7.1.2), proceed to Section 7.2.13, If the waste contains >0.5% dry solids
(see Section 7.1.1 or 7.1.2), and 1f particle size reduction of the solid
was needed in Section 7.1.3, proceed to Section 7,2.10. If the waste as
received passes a 9.5 mm sieve, quantitatively transfer the solid material
Into the extractor bottle along with the filter used to separate the
initial liquid from the solid phase, and proceed to Section 7.2.11.
7.2.10 Prepare the solid portion of the waste for extraction by
crushing, cutting, or grinding the waste to a surface area or particle
size as described in Section 7.1.3. When the surface area or particle
size has been.appropriately altered, quantitatively transfer the solid
material into an extractor bottle. Include the filter used to separate the
Initial liquid from the solid phase.
NOTE: Sieving of the waste is not normally required. Surface area
requirements are meant for filamentous (e.g.. paper, cloth) and
similar waste materials. Actual measurement of surface area is not
recommended. If sieving is necessary, a Teflon coated sieve should
be used to avoid contamination of the sample.
*
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7.2.11 Determine the amount of .extraction fluid to add to the
extractor vessel as follows:
20 x percent sol Ids (Section 7.1.1) x weight of waste
filtered (Section 7.2.5 or 7.2.7)
Weight of -
extraction fluid 100
Slowly add this amount of appropriate extraction fluid (see Section
7.1.4) to the extractor vessel. Close the extractor bottle tightly (it is
recommended that Teflon tape be used to ensure a tight seal), secure 1n
rotary agitation device, and rotate at 30 ± 2 rpm for 18 + 2 hours.
Ambient temperature (I.e.. temperature of room 1n which extraction takes
place) shall be maintained at 23 ±-Z *C during the extraction period.
NOTE: As agitation continues, pressure may build up within the extractor
bottle.for some types of wastes (e.g.. limed or calcium carbonate
containing waste may evolve gases such as carbon dioxide). To
relieve excess pressure, the extractor bottle may be periodically
opened (e.g.. after 15 minutes, 30 minutes, and 1 hour) and vented
Into a hood.
7.2.12 Following the 18+2 hour extraction, separate the
material 1n the extractor vessel' into its component liquid and solid
phases by filtering through a new glass fiber filter, as outlined in
Section 7.2.7. For final filtration of the TCLP extract, the glass fiber
filter may be changed, 1f necessary, to facilitate filtration. Filter(s)
shall be acid-washed (see Section 4.4) if evaluating the mobility of
'metals..!..
7.2.13 Prepare the TCLP extract as follows:
7.2.13.1 If the waste contained no initial liquid
phase, the filtered liquid material obtained from Section 7.2.12 is
defined as the TCLP extract. Proceed to Section 7.2.14.
7.2.13.2 If compatible (e.g.. multiple phases will not
result on combination), combine the filtered liquid resulting from
Section 7.2.12 with the initial liquid phase of the waste obtained
1n Section 7.2.7. This combined liquid 1s defined as the TCLP
extract. Proceed to Section 7.2.14.
7.2.13.3 If the initial liquid phase of the waste, as
obtained from Section 7.2.7, 1s not or may not be compatible with
the filtered liquid resulting from Section 7.2.12, do not combine
these liquids. Analyze these liquids, collectively defined as the
TCLP extract, and combine the results mathematically, as described
in Section 7.2.14.
7.2.14 Following collection of the TCLP extract, the pH of the
extract should be recorded. Immediately aliquot and preserve the extract
for analysis.; Metals allquots must be acidified with nitric acid to
1311- 13 Revision 0
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pH <2. If precipitation is observed upon, addition of nitric add to a
small aliquot of the extract, then the remaining portion of.the extract
for metals analyses shall not be acidified and the 'extract shall be
analyzed as soon as possible. All other allquots must be stored under
.refrigeration (4 *C) until analyzed. The TCLP extract shall be prepared
and analyzed according to appropriate analytical methods. TCLP extracts to
be analyzed for metals shall be add digested except in those instances
where digestion causes loss of metallic analytes. If an analysis of the
undigested extract shows that the concentration of any regulated metallic
analyte exceeds the regulatory level, then the waste 1s hazardous and
digestion of the extract 1s not necessary. However, data on undigested
extracts alone cannot be used to demonstrate that the waste 1s not
hazardous. li the Individual phases are to be analyzed separately,
determine the volume of the individual phases (to ± 0,5%), conduct the
appropriate analyses, and combine the results mathematically by using a
simple volume-weighted average:
(V,) {C,} + (V2) (C2)
Final Analyte Concentration -
V, + V2
where:
V, • The volume of the first phase (L).
CT « The concentration of the analyte of concern 1n the first phase (mg/L).
V2 - The volume of the second phase (L).
C2 - The concentration of the analyte of concern 1n the second phase
...(mg/L),..
7.2.15 Compare the analyte concentrations in the TCLP extract
with the levels identified 1n the appropriate regulations. Refer to
Section 8.0 for quality assurance requirements.
7.3 Procedure When Volatile* are Involved
Use the ZHE device to obtain TCLP extract for analysis of volatile
compounds only. Extract resulting from the use of the ZHE shall not be used to
evaluate the mobility of nonvolatile analytes (e.g.. metals, pesticides, etc.)-
The ZHE device has approximately a 500 mL internal capacity. The ZHE can
thus accommodate a maximum of 25 grams of solid (defined as that fraction of a
sample from which no additional liquid may be forced out by an applied pressure
of 50 ps1), due to the need to add an amount of extraction fluid equal to 20
times the weight of the solid phase.
Charge the ZHE with sample only once and do not open the device until the
final extract (of the solid) has been collected. Repeated filling of the ZHE to
obtain 25 grams of solid 1s not permitted.
Do not allow the waste, the initial liquid phase, or the extract to be
exposed to the atmosphere for any more time than 1s absolutely necessary. Any
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manipulation of these materials should be done when cold (4 §C) to minimize loss
of volatiles.
7.3.1 Pre-we1gh the (evacuated) filtrate collection container
(See Section 4.6) and set aside. If using a TEDLAR* bag, express all
liquid from the ZHE device Into the bag, whether for the Initial or final
liquid/solid separation, and take an aliquot from the liquid in the bag
for analysis. "The containers listed In Section 4.6 are recommended for
use under the conditions stated 1n Sections 4.6.1 - 4.6.3.
7.3.2 Place the ZHE piston within the body of the ZHE (it may be
helpful first to moisten the piston 0-r1ngs slightly with extraction
fluid). Adjust the piston within the ZHE body to a height that will
minimize the distance the piston will have to move once the ZHE 1s charged
with sample (based upon sample size requirements determined from Section
7.3, Section 7.1.1 and/or 7.1.2). Secure the gas Inlet/outlet flanae
(bottom flange) onto the ZHE body in accordance with the manufacturer's
Instructions. Secure the glass fiber filter between the support screens
and set aside. Set liquid Inlet/outlet flange (top flange) aside.
7.3.3 If the waste 1s 100% solid (see Section 7.1.1), weigh out
a subsample (25 gram maximum) of the waste, record weight, and proceed to
Section 7.3.5.
7.3.4 If the waste contains < 0.5% dry solids (Section 7.1.2),
the liquid portion of waste, after filtration, is defined as the TCLP
extract. Filter enough of the sample so that the amount of filtered
liquid will support all of the volatile analyses required. For wastes
containing > 0.5% dry solids (Sections 7.1.1 and/or 7.1.2), use the
percent sol Ids Information obtained in Section 7.1.1 to determine the
optimum sample size to charge into the ZHE. The recommended sample size
is as follows:
7.3.4.1 For wastes containing < 5% solids (see Section
7.1.1), weigh out a 500 gram subsample of waste and record the
weight.
7.3.4.2 For wastes containing > 5% solids (see Section
7.1.1), determine the amount of waste to "charge into the ZHE as
f ol1ows:
25
Weight of waste to charge ZHE - x 100
percent solids (Section 7.1.1)
Weigh out a subsample of the waste of the appropriate size and
record the weight.
7.3.5 If particle size reduction of the solid portion of the
waste was required 1n Section 7.1.3, proceed to Section 7.3.6. If
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particle size reduction was not required -1n Section 7.1.3, proceed to
Section 7.3.7, • . -
7.3.6 Prepare the waste for extraction by crushing, cutting, or
grinding the solid portion of the waste to a surface area or particle size
as described in Section 7.1.3. Wastes and appropriate reduction equipment
should be refrigerated, if possible, to 4 °C prior to particle size
reduction. The means used to effect particle size reduction must not
generate heat in and of Itself. If reduction of the solid phase of the
waste Is necessary, exposure of the waste to the atmosphere should be
avoided to the extent possible.
NOTE: Sieving of the waste is not recommended due to the possibility that
•• = volatile* may be lost. The use of an appropriately graduated ruler
is recommended as an acceptable alternative. Surface area
requirements are meant for filamentous (e.g.. paper, cloth) and
similar waste materials. Actual measurement of surface area is not
recommended.
When the surface area or particle size has been appropriately
altered, proceed to Section 7.3.7.
7.3.7 Waste slurries need not be allowed to stand to permit the
solid phase to settle. Do not centrifuge wastes prior to filtration.
7.3.8. Quantitatively transfer the entire sample (liquid and
solid phases) quickly to the ZHE. Secure the filter and support screens
onto the top flange of the device and secure the top flange to the ZHE
body 1n accordance with the manufacturer's instructions. Tighten all ZHE
fittings and place the device in the vertical position (gas Inlet/outlet
flange on the bottom). Do not attach the extract collection device to the
top plate.
NOTE: If waste material (>lJi of original sample weight) has obviously
adhered to the container used to transfer the sample to the ZHE,
determine the weight of this residue and subtract it from the
sample weight determined in Section 7.3.4 to determine the weight
of the waste sample that will be filtered.
Attach a gas line to the gas Inlet/outlet valve (bottom flange)
and, with the liquid inlet/outlet valve (top flange) open, begin applying
gentle pressure of 1-10 ps1 (or more if necessary) to force all headspace
slowly out of the ZHE device into a hood. At the first appearance of
liquid from the liquid Inlet/outlet valve, quickly close the valve and
discontinue pressure. If filtration of the waste at. 4 'C reduces the
amount of expressed liquid over what would be expressed at room tempera-
ture, then allow the sample to warm up to room temperature in the device
before filtering. If the waste is 100% solid (see Section 7.1'.l), slowly
increase the pressure to a maximum of 50 psi to force most of the
headspace out of the device and proceed to Section 7.3.12.
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7.3.9 Attach the evacuated pre-weighed filtrate collection
container to the liquid Inlet/outlet valve and open the valve. Begin
applying gentle pressure of 1-10 psi to force the Vlquid phase of the
sample Into the filtrate collection container. If no additional liquid
has passed through the filter 1n any 2 minute Interval, slowly increase
the pressure in 10 ps1 increments to a maximum of 50 psi. After each
Incremental Increase of 10 psi, 1f no additional liquid'has passed through
the filter 1n any 2 minute interval, proceed to the next 10 psi increment.
When liquid flow has ceased such that continued pressure filtration at 50
psi does not result in any additional filtrate within a 2 minute period,
stop the filtration. Close the liquid Inlet/outlet valve, discontinue
pressure to the piston, and disconnect and weigh the filtrate collection
container.
NOTE: Instantaneous application of high pressure can degrade the glass
fiber filter and may cause premature plugging.
7.3.10 The material in the 2HE 1s defined as the solid phase of
the waste and the filtrate 1s defined as the liquid phase.
NOTE: Some wastes, such as oily wastes and some paint wastes, will
obviously contain some material that appears to be a liquid. Even
after applying pressure filtration, this material will not filter.
If this 1s the case, the material within the filtration device is
defined as a solid and 1s carried through the TCLP extraction as a
solid.
If the original waste-contained <0.5% dry solids (see Section
7~.1.2), this filtrate 1s defined as the TCLP extract and is analyzed
directly. Proceed to Section 7.3.15.
7.3.11 The liquid phase may now be either analyzed immediately
(See Sections 7.3.13 through 7.3.15) or stored at 4 'C under minimal
headspace conditions until time of analysis. Determine the weight of
extraction fluid #1 to add to the ZHE as follows:
20 x percent solids (Section 7.1.1) x weight
of waste filtered (Section 7.3.4 or 7.3,8)
Weight of extraction fluid -
100
7.3.12 The following Sections detail how to add the appropriate
amount of extraction fluid to the solid material within the ZHE and
agitation of the ZHE vessel. Extraction fluid #1 1s used in all cases
(See Section 5.7).
7.3.12.1 With the ZHE 1n the vertical position, attach
a line from the extraction fluid reservoir, to the liquid In-
let/outlet valve. The line used shall contain frash extraction
fluid and should be preflushed with fluid to eliminate any air
pockets in the line. Release gas pressure on the ZHE piston (from
the gasr Inlet/outlet valve), open the liquid Inlet/outlet valve,
1311-17 Revision 0
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and begin transferring extraction .fluid {by pumping or similar
means) into the ZHE. Continue pumping extraction fluid into the
ZHE until the appropriate amount of fluid has been introduced into
the device.
7.3.12.2 After the extraction fluid has been added,
immediately close the liquid inlet/outlet valve and disconnect the
extraction fluid line. Check the ZHE to ensure that all valves are
in their closed positions. Manually rotate the device in an
end-over-end fashion 2 or 3 times: Reposition the ZHE in the
vertical position with the liquid Inlet/outlet valve on top.
Pressurize the ZHE to 5-10 psi (if necessary) and slowly open the
liquid inlet/outlet valve to bleed out any headspace (into a hood)
that may have been introduced due to the addition of extraction
fluid. This bleeding shall be done quickly and shall be stopped at
the first appearance of liquid from the valve. Re-pressurize the
ZHE with 5-10 ps1 and check all ZHE fittings to ensure that they
are closed.
7.3.12.3 Place the ZHE in the rotary agitation appara-
tus {1f it 1s not already there) and rotate at 30 + 2 rpm for 18 ±
2 hours. Ambient temperature (L,e.. temperature of room in which
extraction occurs) shall be maintained at 23 ± 2 'C during agita-
tion.
7.3.13 Following the 18+2 hour agitation period, check the
pressure behind the ZHE piston by quickly opening and closing the gas
Inlet/outlet valve and noting the escape of gas. If the pressure has not
been maintained M .e.. no gas release observed), the device is leaking.
Check the ZHE for leaking as specified in Section 4.2.1, and perform the
extraction again with a new sample of waste. If the pressure within the
device has been maintained, the material in the extractor vessel is once
again separated into its component liquid and solid phases. If the waste
contained an initial liquid phase, the liquid may be filtered directly
into the same filtrate collection container M .e.. TEDLAR* bag) holding the
initial liquid phase of the waste. A separate filtrate collection
container must be used if combining would create multiple phases, or there
1s not enough volume left within the filtrate collection container.
Filter through the glass fiber filter, using the ZHE device as discussed
1n Section 7.3.9. All extract shall be filtered and collected if the
TEDLAR' bag is used, 1f the extract is multlphasic, or if the waste
contained an Initial liquid phase (see Sections 4.6 and 7.3.1).
NOTE: An in-line glass fiber filter may be used to filter the material
within the ZHE if it 1s suspected that the glass fiber filter has
been ruptured.
7.3.14 If the original waste contained no initial liquid phase,
the filtered.liquid material obtained from Section 7.3.13 1s defined as
the TCLP extract. If the waste contained an initial liquid phase, the
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filtered liquid material obtained from Section 7.3.13. and the Initial
liquid phase (Section 7.3,9) are collectively defined as the TCLP extract.
7.3.15 Following collection of the TCLP extract, immediately
prepare the extract for analysis and store with minimal headspace at 4 *C
until analyzed. Analyze the TCLP extract according to the appropriate
analytical methods. If the individual phases are to be analyzed
separately (I.e.. are not m1sc1ble), determine the volume .of .the
Individual phases (to 0.5%), conduct the appropriate analyses, and combine
the results mathematically by using a simple volume-weighted average:
(VO (c,) + (V2) (c2)
Final Analyte
Concentration V,+ V2
where:
V, - The vplume of the first phases (L).
C, - The concentration of the analyte of concern in the first phase (mg/L).
V2 • The volume of the second phase (L).
C2 • The concentration of the analyte of concern in the second phase
(mg/L).
7.3.16 Compare the analyte concentrations in the TCLP extract
with the levels identified in the appropriate regulations. Refer to
Section 8.0 for quality assurance requirements.
8.0 QUALITY ASSURANCE
8.1 A minimum of one blank (using the same extraction fluid as used for
the samples) must be analyzed for every 20 extractions that have been conducted
in an extraction vessel.
8.2 A matrix spike shall be performed for each waste type (e.g.,
wastewater treatment sludge, contaminated soil, etc.) unless the result exceeds
the regulatory level and the data are being used solely to demonstrate that the
waste property exceeds the regulatory level. A minimum of one matrix spike must.
be analyzed for each analytical batch. As a minimum, follow the matrix spike
addition guidance provided 1n each analytical method.
8,2.1 Matrix spikes are to be added after filtration of the TCLP
extract and before preservation. Matrix spikes should not be added prior
to TCLP extraction of the sample.
8.2.2 In most cases, matrix spikes should be added at a
concentration equivalent to the corresponding regulatory level. If. the
analyte concentration is less than one half the regulatory level, the
spike concentration may be as low as one half of the analyte concentra-
tion, but may not be not less than flva times the method detection limit.
In order to avoid differences 1n matrix effects, the matrix spikes must be
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0
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added to the same nominal volume of TCLP extract as that which was
analyzed for the unsplkad sample.
8.2.3 The purpose of the matrix spike is to monitor the
performance of the analytical methods used, and to determine whether
matrix interferences exist. Use of other internal calibration methods,
modification of the analytical methods, .or use of alternate analytical
methods may be needed to accurately measure the analyte concentration in
the TCLP extract when the recovery of the matrix spike is below the
expected analytical method performance.
8.2.4 Matrix spike recoveries are calculated by the following
formula:
XR (Recovery) - 100 (X, - XU)/K
where:
X, - measured value for the spiked sample,
Xu • measured value for the unspiked sample, and
K • known value of the spike in the sample.
8.3 • All quality control measures described in the appropriate analytical
methods shall be followed.
8.4 The use of internal calibration quantitation methods shall be
employed for a metallic contaminant if: (1) Recovery of the contaminant from the
TCLP extract is not at least 50% and the concentration does not exceed the
regulatory level, and (2) The concentration of the contaminant measured in the
extract is within 20% of the appropriate regulatory level.
8.4.1. The method of standard additions shall be employed as the
internal calibration quantitation method for each metallic contaminant.
8.4.2 The method of standard additions requires preparing
calibration standards in the sample matrix rather than reagent water or
blank solution. It requires taking four identical aliquots of the
solution and adding known amounts of standard to three of these aliquots.
The forth aliquot 1s the unknown. Preferably, the first addition should
be prepared so that the resulting concentration is approximately 50% of
the expected concentration of the sample. The second and third additions
should be prepared so that the concentrations are approximately 100% and
150% of the expected concentration of the sample. All four aliquots are
maintained at the same final volume by adding reagent water or a blank
solution, and may need dilution adjustment to maintain the signals in the
linear range of the instrument technique. All four aliquots are analyzed.
8.4.3 Prepare a plot, or subject data to linear regression, of
instrument signals or external-calibration-derived concentrations as the
dependant variable (y-axis) versus concentrations of the additions of
standard as the independent variable (x-axis). Solve for the intercept of
1311- 20 Revision 0
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the abscissa (the independent variable, x-axis) which 1s the concentration
1n the unknown.
8,4,4 Alternately, subtract the Instrumental signal or external-
calibration-derived concentration of the unknown (unsplked) sample from
the Instrumental signals or external-calibration-derived concentrations of
the standard additions, Plot or subject to linear regression of the
corrected Instrument signals or external-calibration-derived concentra-
tions as the dependant variable versus the Independent variable. Derive
concentrations for unknowns using the Internal calibration curve as 1f 1t
were an external calibration curve.
8.5
periods:
Samples must undergo TCLP extraction within the following time
' SAMPLE MAXIMUM HOLDING TIMES [Days]
Volatiles
Semi -volatile*
Mercury
Metals, except
mercury
From:
Field
collection
To:
TCLP
extraction
14
"14
28
180
From:
TCLP
extraction
To:
Preparative
extraction
NA
7
NA
NA
From:
Preparative
extraction
To:
Determinative
analysis
14
40
28
180
Total
elapsed
time
28
61
- 56
360
NA - Not applicable
If sample holding times are exceeded, the values obtained will be considered
minimal concentrations. Exceeding the holding time is not acceptable 1n
establishing that a waste does not exceed the regulatory level. Exceeding the
holding time will not invalidate characterization if the waste exceeds the
regulatory level,
9.0 METHOD PERFORMANCE
9.1 Ruggedness. Two ruggedness studies have been performed to determine
the effect of various perturbations on specific elements of the TCLP protocol.
Ruggedness testing determines the sensitivity of small procedural variations
which might.be expected to occur during routine laboratory application.
9.1.1 Metals - The following conditions were used when leaching
a waste for metals analysis:
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Varying Conditions
Liquid/Solid ratio
Extraction time
Headspace
Buffer #2 acidity
Acid-washed filters
Filter type
Bottle type
19:1 vs. 21:1
16 hours vs. 18 hours .
20% vs. 60%
190 meq vs. 210 meq
yes vs. no
0.7 jim glass fiber vs.
vs. polycarbonate
borosilicate vs. flint
0.45 ^m
glass
Of the seven method variations examined, acidity of the extraction
fluid had the greatest impact on the results. Four of 13 metals from an
API separator sludge/electroplating waste (API/EN) mixture and two of
three metals from an ammonia Hme still bottom waste were extracted at
higher levels by the more acidic buffer. Because of the sensitivity to pH
changes, the method requires that the extraction fluids be prepared so
that the final pH is within ± 0.05 units as specified.
9.1.2 Volatile Organic Compounds - The following conditions were
used when leaching a waste for VOC analysis:
Varying Conditions
Liquid/Solid ratio
Headspace
Buffer #1 acidity
Method of storing extract
Aliquottlnq
Pressure behind piston
19:1 vs. 21:1
0% vs.
60 meq
Syringe
yes vs
0 psi
5%
vs. 80 meq
vs. Tedlar"
. no
vs. 20 ps1
bag
None of the parameters had a significant effect on the results of
the ruggedness.test.
9.2 Precision. Many TCLP precision (reproducibility) studies have been
performed, and have shown that, in general, the precision of the TCLP 1s
comparable to or exceeds that of the EP toxidty test and that method precision
1s adequate. One of the more significant contributions to poor precision appears
to be related to sample homogeneity and inter-laboratory variation (due to the
nature of waste materials).
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9,2.1 Metals - The results of a rnultl-laboratory study are shown
in Table 6, and indicate that a single "analysis of a waste may not be
adequate for waste characterization and Identification requirements.
9.2.2 Semi-Volatile Organic Compounds - The results of two
studies are shown 1n Tables 7 and 8. Single laboratory precision was
excellent with greater than 90 percent of the results exhibiting an RSD
less than 25 percent. Over 85 percent of all individual compounds in the
multi-laboratory study fell in the RSD range of 20 - 1ZO percent. Both
studies concluded that the TCLP provides adequate precision, It was also
determined that the high acetate content of the extraction fluid did not
present problems M.e.. column degradation of the gas chromatograph) for
the analytical conditions used.
9.2.3 Volatile Organic Compounds - Eleven laboratories
participated in a collaborative study of the use of the 2HE with two waste
types which were fortified with a mixture of VOCs. The results of the
collaborative study are shown in Table 9. Precision results for VOCs tend
to occur over a considerable range. However, the range and mean RSD
compared very closely to the same collaborative study metals results 1n
Table 6. Blackburn and Show concluded that at the 95% level of signifi-
cance: 1) recoveries among laboratories were statistically similar, 2)
recoveries did not vary significantly between the two sample types, and 3)
each laboratory showed the same pattern of recovery for each of the two
samples.
10.0 REFERENCES
1. Blackburn, W.B. and Show, I." 'Collaborative Study of the Toxlcity
Characteristics Leaching Procedure (TCLP)." Draft Final Report, Contract No. "68-
03-1958, S-Cubed, November 1986.
2. Kewcomer, L.R., Blackburn, W.B., Kimmfill, T.A. "Performance of the
Toxicity Characteristic Leaching Procedure." Wilson Laboratories, S-Cubed, U.S.
EPA, December 1986.
3. Williams, L.R., Francis, C.W.; Maskarinec, M.P., Taylor D.R., and Rothman,
N. "Single-Laboratory Evaluation of Mobility Procedure for Solid Waste." EHSL,
ORNL, S-Cubed, ENSECO,
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Table 1.
Volatile Analytes1-2-
Compound CAS No.
Acetone
Benzene
n-Butyl alcohol
Carbon dlsulfide
Carbon tetrachlorlde •
Chlorobenzene
Chloroform
l,2-D1chloroethane
l,l-D1chloroethylene .
Ethyl acetate
Ethyl benzene
Ethyl ether
Isobutanol
Methanol
Methylene chloride
Methyl ethyl ketone
Methyl isobutyl ketone
Tetrachloroethylene
Toluene
1 , 1 , 1 , -Tr1 chl oroethane
Trichloroethylene .".' ...
Tr1 chl orof 1 uoromethane
l,l,2-Tr1chloro-l,2,2-trifluoroethane
Vinyl chloride
Xylene
67-64-1
71-43-2
71-36-3
75-15-0
56-23-5
108-90-7
67-66-3
107-06-2
75-35-4
141-78-6
100-41-4
60-29-7
78-83-1
67-56-1
75-09-2
78-93-3
108-10-1
127-18-4
108-88-3
71-55-6
... 79-01*6
75-69-4
75-13-1
75-01-4
1330-20-7
1 When testing for any or all of these analytes, the zero-headspace
extractor vessel shall'be used Instead of the bottle extractor.
2 Benzene, carbon tetrachlorlde, Chlorobenzene, chloroform,
1,2-dichloroethane, I,l-d1chloroethylene, methyl ethyl ketone,
tetrachloroethylene, and vinyl chloride are toxtdty characteristic
constituents.
1311- 24 Revision 0
July 1992
-------
Table 2, _
Suitable Rotary Agitation Apparatus1
Company
Location
Model No.
Analytical Testing and
Consulting Services,
Inc.
Associated Design and
Manufacturing Company
Harrington, PA
(215) 343-4490
Alexandria, VA
(703) 549-5999
Environmental Machine and
Design, Inc.
IRA Machine Shop and
Laboratory
Lars Lande Manufacturing
HUlipore Corp.
Lynchburg, VA
(804) 845-6424
Santurce, PR
(809) 752-4004
Whltmore Lake,
(313) 449-4116
Bedford, HA
(800) 225-3384
HI
4-vessel extractor (DC20S)
8-vessel extractor (DC20)
12-vessel extractor (DC20B)
24-vessel extractor (DC24C)
2-vessel
4-vessel
6-vessel
8-vessel
12-vessel
24-vessel
(3740-2-BRE)
(3740-4-BRE)
(3740-6-BRE)
(3740-8-BRE)
(3740-12-BRE)
(3740-24-BRE)
8-vessel (08-00-00)
4-vessel (04-00-00)
8-vessel (011001)
10-vessel (10VRE)
5-vessel (5VRE)
6-vessel (6VRE)
4-2HE or
4 2-liter bottle
extractor (YT310RAM)
1 Any device that rotates the extraction vessel in an end-over-end fashion at 30
± 2 rpm 1s acceptable.
1311- 25
.Revision 0
July 1992
-------
Table 3.
Suitable Zero-Headspace Extractor Vessels1
Company
Location
Model No.
Analytical Testing i
Consulting Services, Inc.
Associated Design and
Manufacturing Company
Lars Lande Manufacturing2
Mlllipore Corporation
Environmental Machine
and Design, Inc.
Caiman Science
Warrlngton, PA
(215) 343-4490
Alexandria, VA
(703) 549-5999
Whltmore Lake, MI
(313) 449-4116
Bedford, MA
(800) 225-3384
Lynchburg, VA
(804) 845-6424
Ann Arbor, MI
(800) 521-1520
C102, Mechanical
Pressure Device
3745-ZHE, Gas
Pressure Device
ZHE-11, Gas
Pressure Device
YT30090HW, Gas
Pressure Device
VOLA-TOX1, Gas
Pressure Device
15400 Gas Pressure
Device
1 Any device that meets the specifications listed .1n Section 4.2.1 of the method
1s suitable.
2 This device uses a 110 mm filter.
1311- 26
Revision 0
July 1992
-------
Table 4,
Suitable Filter Holders1
Model/
Company
Nucleopore Corporation
Micro Filtration
Systems
Location
Pleasanton, CA
(800) 882-7711
Dublin, CA
(BOO) 334-7132
(415) 828-6010
Catalogue No.
425910
410400
302400
311400
Size
142 mm
47' mm
142 m
47 mm
Millipore Corporation Bedford, MA YT30142HW 142mm
(800) 225-3384 XX1004700 47 mm
1 Any device capable of separating the liquid from the solid phase of the waste
is suitable, providing that 1t 1s chemically compatible with the waste and the
constituents to be analyzed. Plastic devices (not listed above) may be used when
only Inorganic analytes are of concern. The 142 mm size filter holder is
recommended.
1311- 27 Revision 0
July 1992
-------
Table 5.
Suitable Filter Media1
Company
MITHpore Corporation
Nucleopore Corporation
Whatman Laboratory .
Products, Inc.
Micro Filtration
Systems
Gel man Science
Location
Bedford, HA
(800) 225-3384
Pleasanton, CA
(415) 463-2530
Clifton, NO
(201) 773-5800
Dublin, CA
(800) 334-7132
(415) 828-6010
Ann Arbor, HI
(800) 521-1520
' Model
AP40
211625
GFF
GF75
66256 (gOrcm)
66257 (142mm)
Pore
Size
(jum)
0.7
0.7
0.7
0.7
0,7
1 Any filter that meets the specifications 1n Section 4.4 of the Method 1s
suitable.
1311- 28
Revision 0
July 1992
-------
Table 6. Multi-Laboratory TCLP Metals, Precision
Waste
Ammonia
Lime Still
Bottoms
API/EH
Mixture
Fossil
Fuel Fly
Ash
Extraction
Fluid
#1
12
#1
#2
#1
#2
#1
#2
#1
#2
11
#2
#1
n
#1
12
#1
n
Metal
Cadmium
Chromium
Lead
Cadmium
Chromium
Lead
Cadmium
Chromium
Lead
X
0.053
0.023
0.015
0,0032
0.0030
0.0032
0.0046
0.0005
0.0561
0.105
0.0031
0.0124
0.080
0.093
0.017
0.070
0.0087
0.0457
S
0.031
0.017
0.0014
0.0037
0.0027
0.0028
0.0028
0.0004
0.0227
0.018
0.0031
0.0136 .
0.069
0.067
0.014
0.040
0.0074
0.0083
%RSD
60
76 '
93
118
90
87
61
77
40
. 17
100
110
86
72
85
57
85
18
%RSD Range - 17 - 118
Mean XRSD . 74
NOTE:.X » Mean results from 6 - 12 different laboratories
Units - mg/L
Extraction Fluid #1 * pH 4.9
#2 = pH 2.9
1311- 29
Revision 0
July 1992
-------
Table 7.- Single-Laboratory Semi-Volatile?, Precision
Waste
Ammonia
.lime Still .
Bottoms
API/EW
Mixture
Compound
Phenol
2-Methyl phenol
4-Methyl phenol
2, 4-Dimethyl phenol
Naphthalene
•
2-Methylnaphthalene
Dibenzofuran
Acenaphthylene
Fluorene
Phenanthrene
Anthracene
Fluoranthrene
Phenol
2, 4-D1methyl phenol
Naphthalene
2 -Methyl naphthalene
Extraction
Fluid
#1
• n
n
12
#1
#2
#1
n
n
n
n
n
#1
*2
11
n
#1
• #2
#1
#2
#1
#2
#1
#2
#1
#2
#1
#2
#1
12
#1
#2
X
19000
19400
2000
1860
7940
7490
321
307
3920
3827
290
273
187
187
703
663
151
156
241
243
33.2
34.6
25.3
26.0
40.7
19.0
33,0
43.3
185
165
265
200
S
2230
929
297
52.9
1380
200
46.8
45.8
413
176
44.8
19.3
22.7
7.2
89.2
20.1
17.6
2.1
22.7
7.9
6.19
1.55
1.8
1.8
13.5
1.76
9.35
8.61
29.4
24.8
61.2
18.9
%RSD
11.6
4.8
14.9
2.8
17.4
2.7
14.6
14.9
10.5
4.6
15.5
7.1
12.1
3.9
12.7
3.0
11.7
1.3
9.4
3.3
18.6
4.5
7.1
7.1
33.0
9.3
28.3
19.9
15.8
15.0
23.1
9.5
%RSD Range -1-33
Mean KRSD > 12
NOTE:
Units
Extractions were performed in triplicate
All results were at least 2x the detection limit
Extraction Fluid #1 - pH 4.9
#2 » pH 2.9
1311- 30
Revision 0
July 1992
-------
Table 8. Hultl-Laboratory Sem1-V.olatiles, Precision
Waste
Ammonia Lima
Still Bottoms (A)
API/EW
Mixture (B)
Fossil Fuel
Fly Ash (C)
Compound
BNAs
BNAs
BNAs
Extraction
Fluid
#1 '
#2
• 11
n
#1
n
X
10043
10376
1624
2074
. 750
739
S
7680
6552
675
1463
175
342
%RSD
76.5
63.1
41.6
70.5
23.4
46.3
Mean %RSD - 54
NOTE: Units
X « Mean results from 3-10 labs
Extraction Fluid II - pH 4.9
n - pH 2.9 .
&RSD Range for Individual Compounds
A, #1 0 - 113
A, n 28 - 108
B, #1 20 - 156
B, #2 49 - 128
C, II 36 - 143
C, #2 61 - 164
1311- 31
Revision 0
July 1992 .
-------
Table 9. Mult 1-Laboratory (11 Labs) VOCs, Precision
Waste
Mine
Tailings
,
Ammonia
L1me Still
Bottoms
Compound
Vinyl chloride
Methyl ene chloride
Carbon dlsulfide
l,l-D1chloroethene
1,1-Dichloroethane
Chloroform
l,2-D1chloroethane
2-Butanone
1,1,1-Trlchloroethane
Carbon tetrachloride
Trlchloroethene
1,1,2-Trichloroethene
Benzene
1 , 1 » 2 , 2-Tetrachl oroethane
Toluene
Chlorobenzene
Ethyl benzene
Trichlorofluoromethane
Acrylonitrlle
Vinyl chloride
Methylene chloride
Carbon dlsulfide
l,l-D1chloroethene
l,l-D1chloroethane
Chloroform
' l,2-D1chl oroethane
2-Butanone
1,1,1-Trichloroethane
Carbon tetrachloride
Trlchloroethene
1 , 1 , 2-Tr i chl oroethene
Benzene
1,1,2 , 2-Tetrachl oroethane
Toluene
Chlorobenzene.
Ethyl benzene
Trichlorofluoromethane
Acrylon1tr1le
X
6.36
. 12.1
5.57
21,9
31.4
46.6
47.8
43.5
20,9
12.0
24.7
19.6
37.9
34.9 '
29.3
35.6
4.27
3,82
76.7
5.00
14.3
3.37
" 52.1
52.8
64.7
43.1
59.0
53.6
7.10
57.3
6.7
61.3
3.16
69.0
71.8
3.70
4.05
29.4
S
6.36
11.8
2.83
27.7
25.4
29.2
33.6
36.9
20.9
8.2
21.2
10.9
28.7
25.6
11.2
19.3
2,80
4.40
110.8
4.71
13,1
2.07
38. B
25.6
28.4
31.5
39.6
40.9
6.1
.34.2
4.7
26.8
2.1
18.5
12.0
2.2
4.8
34.8
%RSD
100
98
51
127
81
63
70
85
100
68
86
56
76
73
38
54
66
115
144
94
92
61
75
49
44
73
• 67
76
86
60
70
44
66
27
17
58
119
118
%RSD Range - 17 - 144
Mean %RSD - 75
NOTE: Units -
1311- 32
Revision 0
July 1992
-------
Motor
(30± 2 rpm)
Extraction Vessel Holder
Figure 1. Rotary Agitation Apparatus
Top Flange s
Support Screen-
Finer
Support Screen
Bottom Range —^_
UquW Inlet/Outlet Valve
cLj
Pretturtzed Gts •
InJet/OutW Valve
3 j>, .:•;;•, Piston:- ^';; =
Gas
cL:)
Pressure
Gauge
Figure 2. Zero-Headspace Extractor (ZHE)
1311- 33
Revision 0
July 1992
-------
METHOD 1311 -
TOXICITY CHARACTERISTIC LEACHATE PROCEDURE
liquidi fro*
•olid* »Uh 0.4
• 0.8 ua gl»i*
!ib«r Jill«r
talld*
Eitraol •/
ippr«priat« fluid
1] Battl* •>lr«etor
Jor non-vol«til»j
2} ZHE divio. tot
liquid* fro.
olid. «i'.h C.6
0.8 u» dim
fib.r fiU.f
Solid
Mu*L the
•olid b«
silled?
Liquid
p»rticl« til*
le <9.S on
1311- 34
Revision 0
July 1992
-------
METHOD 1311 (CONTINUED)
TOXICITY CHARACTERISTIC LEACHATE PROCEDURE
Star* liquid
• I 4 C
Sis:-
Solid
5ip*i
volia'j i
O.I u»
fib.r .
«l»
/ O.i •
gl»«*
liquid
tstciel »/
liquid ph»»«
of »«*l«
liquid
c
STOP
M*«jur*
liquid ind
e/
conbin* rȤult */
mult of utriot
1311- 35
Revision 0
July 1992
-------
55114
Federal' Rngislcr / Vol. 57, No. 227 / Tiinsday. Novnmbnr 24. 1fl(J2 / Ruins -and Regulations
includes a revision of Air Quality
Control Regulations 750 (NSI'S) and 751
(NESHAP) as adopted by Ihn New
Mexico Environment Improvement
Hoard. AQCRs 750 and 751 incorporate
the Federal NSPS and NESI1AP by
reference through November 15.1991.
The EPA reviewed the NMF.D request.
Air Quality Control Regulations 750 and
751 and all other information submitted
by the NMF.D, including its quest for
implementation of the delegation of .
these programs. The EPA has
determined that the Slute has adequate
authority and effective procedures for
implementing and enforcing the NSPS
and NESHAP programs. Therefore. EPA
is delegating full authority to the Slate
through November 15.1991. for NSPS
and for NESHAP. and authority for the
technical and administrative review of
new or amended NSPS and NF.SI 1AP
promulgated by the EPA after November
15.T991. subject to conditions and
limitations of the original delegation
agreement dated March 15.1985. It is
important to note thai no delegation
authority is granted to the Slate for both
Bcrnalillo County and Indian lands.
Also, no authority is delegated to the
State for 40 CFR part DO, subpart AAA. .
Standards of Performance for New
' Residential Wood I leatcrs, and for 40
CFR part 61 for the radionuclidn
NESHAPs. Specifically the subparls for
which delegation is excluded are
Subparts D.(National Emission Standard
for Radon—222 Emissions from
Underground Uranium Mines). 11
(National Emission Standard for
lUidionuclide Emissions from
Department of Energy Facilities). I
(National Emission Standard for
Radionuclide Emissions from Facilities
Licensed by the NRC and Federal
Facilities not covered by Subpart
Phosphorus Plants). R (National
F.mission Standards for Radon
Emissions from Phosphogypsum Stacks).
T (National Emission Standards for
Radon Emissions from the Disposal of
Uranium Mill Tailings), and W (National
Emission Standard for Radon—222
Emissions from Licensed Uranium Mill
Tailings).
Today's notice informs the public that
the F.PA has delegated full authority to
(he Stale for implementation and '
enforcement of the NSPS and NESHAP
promulgated by the EPA through/
November 15.1991. and authority for
technical and administrative review is
delegated for the new and amended .
standards after that date. All of the.
required information, pursuant lo the
Federal NSPS and NESHAP (40 CFR ' •
part 60 and 40 CFR part 61) by sources
located outside the boundaries of ••
Bcrnalillo County and in areas oufsidc
of Indian lands, should be submitted
directly to the New Mexico Environment
Department. Harold Runnels Building.
Room So. 2100. St. Francis Drive. Santa
I-'e. New Mexico 07503. Albuquerque/
Dcrnalillo County is exempt due lo this
area being granted delegation authority
'under AQCRs 30 NSPS and 31 NESI IAP
to the City of Albuquerque's
Environmental Health Department.
Sources located on Indian lands in [he
Slate of New Mexico should submit
required information lo the EPA Region
G office at the address given in'this
notice! All of the inquiries and requests
concerning implementation and
enforcement of the excluded standards
under 40 CFR part RO. subpart AAA and
40 CKR part 01. subparts 13. 11. I, R. T and
VV. in the Slate of New Mexico should
be directed to Ihc F.PA Region 0 Office.
The Office of Management and Budget
has exempted this information notice
from the requirements of Section 3 of
Executive Order 12291.
This delegation is issued under the
authority of section lll(c) and 112(1)(1)
of the Clean Air Act. as amended (42
U.S.C. 7411(C)and7412(D)).
List of Subjects
<0 CFR Part CO
Air pollution control. Aluminum.
sulfalc planls. Cement industry. Coal. •
Copper. Electric power planls. Fossil-
Fuel steam generators. Glass and glass
products. Grain. Iron. Lead. Metals.
Motor vehicles. Nitric acid plants. Paper
and paper industry. Petroleum
phosphate. Fertilizer. Sewage disposal.
Steel. Sulfuric.acid plants. Waste
treatment and disposal zinc.
40 Cf-'R Part 61
Air pollution control. Asbestos.
Benzene. Beryllium. Hazardous
materials. Mercury. Vinyl chloride.
D;ili-il: November 3.1fK>2.
|oc D. Winkle.
Ac'.iuy Hc};ioiwl f\t!t:iinislrutiir.
|FR Uoc. 9^-20514 Filed 11-23-yj: 8:45 urn]
BILLING CODE 6S60-SO-W
ACTION: Final rule.
40 CFR Parts 261 and 271
IFRL-4536-5!
RIN 2050-AC32
Hazardous Waste Management
System; Identification and Listing of
Hazardous Waste; Toxlclty
Characteristic Revision
AGENCY: Environmental Protection'
Agency. . ...
SUMMARY: The Environmental Protection
Agency (EPA or Agency) is amending its
hazardous waste regulations under
Subtitle C of Ihc Rnsourcn Conservation
and Recovery Act (RCRA) for testing
conducted to evaluate a solid waste for
the Toxicily Characteristic. Specifically,
this rule removes the quality assurance
(QA) requirement found in Mclhod.1311.
Toxicily Characteristic Leaching
Procedure (TCLP). for correcting
measured values for analytical bias
(also referred lo within this rule as spike
recovery correction). However, this rule
retains appropriate QA provisions.
including that matrix spike recoveries be
.calculated and'that the method of.
standard additions be employed as Ihe
quantilalion method for metallic
contumirxints when appropriate a.s
specified in Ihc method.
EFFECTIVE DATE: November 2-5. 1992.
ADDRESSES: The official record for this
rulemaking (Docket No. F-92-TCLC-
FFFFF) is located at the U.S.
Environmental Protection Agency. 401 M
Street. SW, Washington. DC 20400 '
(room M-2427). and is available for
viewing from 9 a.m. to 4 p.m.. Monday
through Friday, excluding Federal
holidays. The public must make an
appointment lo review docket materials
by calling (202) 200-9327. The public
may copy a maximum of 100 pages of
material from any one regulatory docket
a! no cost: additional copies cost S0.15
per page.
FOR FURTHER INFORMATION CONTACT:
For general information, contar:! the '
RCRA Hotline al (BOO) 424-934fi (loll
free) or call (703) 920-9310: or. for
' hearing impaired, call TDD (COO) 553-
7672 or (703) 48f>-3323. For information
concerning the TCLP. contact Kim
Kirklar.d. Office of Solid Waste (05-
331). U.S. Environmental Protection
Agency. 401 M Street. SW.. Washington
DC 20400. (202) 200-1/01.
SUPPLEMENTARY INFORMATION:
I. Authority
This amendm«nl to Ihc hazardous
waste regulations in 40 CFR parts 2GI
and 271 is being promulgated under Ihc
authority of sections 1COC. 2002. 3001.
3002. and 300G of the Solid Waste
Disposal Act of 1976, as amended by the
Resource Conservation and Recovery '
Act of 1976. as amended |42 U.S.C. 6005
G912(a). 6921.6922. and 6926|. .
II. Background \ .-.
• On February 8.1990 (55 FR 4440). the
Agency published a notice of data ...
availability lli.il reopened the comment
-------
Federal Register /,Vol. 57. No. 227 /Tuesday. November 24. 1992 / Rules and Regulations 55115
fperiod for a January 23.1989 notice (54
•'FK3212). which proposed lo update
; SW-WG and to designate specific
. quality control procedures as mandatory
for all testing conducted pursuant to
lublille C.of RCKA. including the TCLP.
The February. 1990 notice issued for
. comment a revised Chapter One of SW-
WBenlilled "Report on Minimum
Criteria to Assure Data Quality" which
included spike recovery correction as
one of the QA requirements for RCRA
subtitle C analyses. In thai notice, the
Agency stated that it believed thai il
was appropriate to correct a measured
concentration for recovery and set out
ils intent lo require that reported values
be corrected for spike recovery. The
purpose of this requirement was to
provide more accurate data in those
situations where, there was a significant
analytical bias in (he data due to low
recoveries of the analytes of interest.
On March 29,1990. (55 FR 11796). EPA
•promulgated a rule lo revise the then
existing Toxicity Characteristic, which
is used to identify those wastes that are
hazardous and thus subject to regulation
under subtitle C of RCRA. The rule
broadened and refined the scope of the
hazardous waste regulatory program
and fulfilled specific statutory mandates
under Ihe Hazardous and Solid Waste
Amendments (HSWA) cf 1984. The
regulatory language of the March 29.
1990 rule replaced the Extraction
Procedure (EP) loxicity test with the '
Toxicity Characteristic Leaching
Procedure (TCLP). The TCLP was
promulgated in appendix II to 40 CFR
part 261 and was designated as FPA
Method 1311. to be incorporated in "Test
Methods of Evaluating Solid Waste
(Chemical/Physical Methods)". SW-846.
The March 29.1990. rule required that
matrix spike recoveries be calculated
and that the method of standard
additions be employed as the
quuntitulion method for metallic
contaminants when appropriate as
specified in the method.
On June 29.1990 (55 FR 2698G). the ..
Agency promulgated a final rule which
made technical corrections to the March
29.1990 final rulet including the .
regulatory language in 40 CFR part 261.
appendix II (Method 1311. the TCLP).
These corrections reorganized Ihe TCLP
in 40 CFR part 261. appendix II. to .
correspond to the current version of
SW-846. In addition, the quality
assurance section of the TCLP was
clarified by adding a requirement for the
spike recovery correction. The spike •
recovery correction requirement was •
added to assure consistency wilh SW-
84G Chapter One requirements which
were proposed in the February 8.1990 .
notice. Since the objectives lo be
achieved through the method of
standard additions were being
addressed through spike recovery
correction, that method no longer was
referenced separately in the QA
provisions of the TCLP. •
. At the time that the TCLP was
promulgated in its current form on June
29.1990. the Agency expected to
promulgate Chapter One of SW-846. as
proposed 'on February 8.'1990. with the
spike recovery correction requirement.
The Agency expected that (he
promulgation of Chapter One would
occur prior to the effective date of the
TC final rule. I lowever. the Agency has
not yet promulgated a rule finalizing
Chapter One. as proposed on February
C, 1990. but based upon comments
received on that chapter, the Agency
has reassessed its position respecting
the matrix spike correction requirement.
III. Response to Comments Regarding
Spike Recovery Correction and Basis for
Amendment lo 40 CFR Part 2G1.
Appendix II ...••-.
Many of the commenters to the '
February 8.1990 nolice indicated that
the requirement for spike recovery
correction should not be mandatory.1 In
particular, a number of commenters
raised questions relative to the practical
aspects of implementation of the
requirement (e.g.. how lo add the spike.
how many compounds must be spiked. '
how many samples must be spiked) as
well as the burdensome nature of
implementation for wastes with matrix
interference problems. Wastes with
matrix interferences often require
dilution in an attempt to reduce or
eliminate Ihe interferences. As a result.
detection limits could be elevated and
one might not be able to determine if a
compound of interest is present below
the regulatory threshold. In addition. • .
interferences may not equally affect the
sample and the spike. CommerMers also
expressed concern about bias correction
when applied to a constituent that is
poorly recovered from a sample matrix.
In the case of zero percent recovery, one
may not be suhe that the laboratory
could have delected the presence of the
analyle if it were present.
The Agency recognizes that spike .
recovery correction is a complex issue
and now believes that there is a need for
further evaluation and more detailed
guidance on the specific implementation
procedures. Therefore, in response to
'public comment received on the . . •
February 8.1990. Federal Register • ,
1 Other comments, together with the Agency's
response thereto, have been pluccd in the official *.
record for this rulcmuking.
notice, the Agency has decided not to
proceed with the proposed spike
recovery correction requirements in its
subtitle C analytical procedures, and is
withdrawing the requirement for bins
correction of analytical spiked samples
from the TCLP. . -
As a result, it is also necessary to
'amend Appendix II of 40 CFR part 261
and remove all text in the existing TCLP
which imposes a requirement for
correcting measured values for
analytical bias. Specifically, in today's
final rule. § 8.2 is revised whereby the
following sentence is deleted: "The bias
determined from the matrix spike
determination shall be used to correct •
the measured values.'(See §5 8.2.4 and
8.2.5.)" In addition, § 8.2.5 is deleted.
which provided a formula for spikt;
recovery correction.
Today's rule withdraws Ihe spike
recovery correction requirement from
the TCLP and. except for technical and
format changes made in the June 29.
1990. rule revising the TCLP (55 FR
26986). returns the QA provisions of Ihe
TCLP to those promulgated on March 29.
1990 (55 FR 1179C). As a result, matrix
spike recoveries must be calculated (as
set forth in revised § 8.2 of the TCLP)
and the method of standard addHions
must be employed .as the quantiliition
method for metallic contaminants when
appropriate as specified in the method
(as set forth in revised § 8.4 of the
TCLP). In addition, (he Agency has
made a technical correction to the
regulatory language in § 8.4 to specify
the.use of initial calibration quantilalion
methods for metallic contaminants. The
Age.ncy feels this technicalcorrection is
appropriate because, at present the ;
method of standard additions is
inapplicable lo organic contaminants.
Wastes identified.as hazardous through
TCLP testing utilizing matrix spike .
recovery correction must be managed as
hazardous wastes, unless und until such
wastes are reevaluated using
recalculations of existing data or the
TCLP test procedure as described in :
today's rule cr otherwise reevaluated
und found lo be non-hazardous.
IV. State Authority
A. Applicability of Rule in Authorized
States • . . . : .
Under section 3006 of RCRA. EPA
may authorize qualified States to
administer and enforce the RCRA
program within the State. (Sec 40 CFR
part 271 for the standards and • .
requirements for authorization.) •:. :
Following authorization. EPA retains •
enforcement authority under sections •
3008. 7003 and 3013 of RCRA. although
-------
55116
Federal Register / Vol. 57. No. 227 / Tuesdny. November 24. 1992 / Rules and Regulation's
authorized Stales have primary .
enforcement responsibility.
Prior to (he Hazardous and Solid
Waste Amendments of 19W (HSWA). a
State with final authorization '- .
administered its hazardous waste
program entirely in lieu of EPA
administering the Federal program in
that State. The Federal requirements no
longer applied in the authorized Slate,
and EPA could not issue permits for any
facilities in the State that the State was
authorized to permit. When new. more
stringent Federal requirements were
promulgated or enacted, the Stale \vas
obliged to enact equivalent authority
within specified time frames. New
Federal requirements did not lake effect
in an authorized State until the State
adopted the requirements as State law.
In contrast, under section 300G(g) of
RCRA, 42 U.S.C. 6926(g). new . • .
requirements and prohibitions imposed
by HSWA take effect in authorized •
Stales a\ the same time that they take '
effect in nonauthorized States. EPA is
directed to'cnrry out those requirements
'and prohibitions in authorized States.
including the issuance of permits, until
the Stale is granted authorization to do
so. While States must still adopt • •
HSWA-related provisions as State law
to-retain final authorization. HSWA
requirements are implemented by EPA
in aulhorizod States in the interim.
Today's rule is being promulgated
pursuant to RCRA section 3001(g). a
provision added by HSWA. and amends
the Toxicity Characteristic Leaching
Procedure (TCLP) in appendix II of 40
CFR part 261. Therefore, the Agency is
adding today's rule to Table 1 in 40 CFR
271.1(j). which identifies the Federal .
program requirements that are
promulgated pursuant to HSWA and
that take effect in all States, regardless .
of their authorization status. Slates may
apply for either interim or final , •
authorization for the HSWA provisions
identified in Table 1. as discussed in the
following section of this preamble.
B. Effect on State Authorizations • •
Pursuant to sections 3001(g] of RCRA,
a provision added by HSWA, EPA is
revising the TCLP (40 CFR part 261.
appendix II). Thus, the revisions to the .
TCLP will take effect in unauthorized
states (i.e., states not authorized to .
implement any portion of the RCRA
program] and all States which have nof
been authorized for the Toxicity
Characteristic (TC) on the effective date.
Today's rule deletes the requirements
imposed in the revised final TCLP- • ' •".
method (see 55 FR 26986. June 29.1990)
for spike recovery correction of ' :• : ;
analytical data. The Toxicity .
Characteristic was promulgated ;' ' ;
pursuant to a HSWA provision and must.
be adopted by Slates that intend to • '.
retain final authorization. However.
today's rule provides for a standard that
is less restrictive than was imposed in
the final TC as promulgated on June 29. •
1990. for hazardous waste
determinations based on spike recovery
adjusted data. Although Stales must
modify their'programs to incorporate the
Toxicity Characteristic, they no longer
are required to include spike recovery
correction in those modifications.
Section 3009 of RCRA provides thalt"
States may impose requirements that
are broader in scope or more stringent
than those imposed under Federal
regulation. For slates that have received
final authorization for programs
requiring spike recovery correction as
part of the TCLP, those states ha've the
option of modifying their programs to
•delete this requirement. •
V. Effective Date . .
HSWA amended section 3010 of
RCRA-to allow rules to become effective
in less than six months when.the
regulated community does not need the
six-month period to come into
compliance; Section 553(d) of the
Administrative Procedures Act requires
publication of a substantive rule not less
than 30 days before its effective date
'unless the rule relieves a restriction or
for other good cause. This rule is
effective November 24.1992 because the
regulated community does not need six
months to come into compliance •
therewith, and it relieves a regulatory
restriction. Those reasons also
constitute good cause for not delaying
the effective date of today's rule. This .
amendment removes the spike recovery
correction requirement from the TCLP
and thus provides greater flexibility to
the regulated community in testing solid
waste for the Toxicity Characteristic.
VI. Regulatory Analyses • . .
A. Regulatory Impact Analysis
Under Executive Order 12291, EPA
must determine whether a regulation is
"major" and, therefore, subject to the '
requirement of a Regulatory Impact
Analysis. This rule removes the spike
recovery correction requirement found
in the TCLP and thus, reduces the '
overall costs and economic impact of
EPA's hazardous waste regulations and
provides greater flexibility .to the
•regulated community in testing and . ' :
• monitoring solid waste. There is no • .
additional economic impact, therefore.
due to today's rule. This rule is not a . '
. major regulation: thus, no Regulatory .
Impact Analysis is required. ."--..'• :
B. Regulatory Flexibility Act -.
Pursuant to the Regulatory Flexibility
Act (5 U.S.C. section 601-012. Public
Law 96-354. September 19,1900).
whenever an agency publishes a
General Notice of Rulcmaking for any
proposed or final rule, it must prepare
and make available for public comment
a regulatory flexibility analysis (RFA)
that describes the impact of the rule on
small entities (i.e., small businesses.
small organizations, and small
governmental jurisdictions). No
regulatory flexibility analysis is
required, however, if the head of the
Agency certifies that the rule will not
. have a significant impact on a
substantial number of small entities
This rule will not have an adverse
economic impact on small entities since '
its effect will be to reduce the overall
costs of EPA's hazardous waste •
regulations and provide greater
flexibility to the regulated community,
including small entities. Therefore, in
accordance with 5 U.S.C. section 605(b).
I hereby certify that this rule will not
have a significant economic impact on a
.substantial number of small entities (as
defined by the Regulatory Flexibility
Act). Thus, the regulation docs not i
require an RFA. ' . .
c. Paperwork Reduction Act
There are no additional reporting.
notification, or recordkeeping provisions
in this rule. Such provisions, were they
included, would be submitted for ' '
approval to the Office of Management'
and Budget (OMB) under the Paperwork
Reduction Act. 44 U.S.C. 3501 el scq. '
List of Subjects
40 CFR Part 261 • .
Hazardous waste. Recycling.
Reporting and recordkeeping
requirements.
40 CFR Part 271
Administrative practice and •
procedure. Confidential business
information. Hazardous materials
transportation. Hazardous waste.
Indians-lands, Intergovernmental
relations, Penalties, Reporting and .
recordkeeping requirements. Water
pollution control. Water supply.
. Da led: November 13,1992. . ;
William K. Rcilly, ...
Administrator. ' . • '*• ...
For the reasons set out in the
preamble, title 40 of the Code of Federal
Regulations is amended as set forth
below. •
-------
Federal Register /Vol. 57, No. 227 / Tuesday. November 24, 1992 / Rules and Regulations 55117
PART 261—IDENTIFICATION AND
LISTING OF HAZARDOUS WASTE
l.The authority citation for part 261
continues to read as follows: .
Authority: 42 U.S.C. 6905. 6912(a). 6921.
6922. a t\d 0938.
. 2, Part 201. appendix II is amended by
revising the test of § 8.0 preceding
table I to read as follows:
Appendix II—Method 1311 Toxicity
Characteristic Leaching Procedure
(TCLP) ...
8.0 Quality Assurance ' •
. 8.1 A minimum of one blank (using the •
tame extraction fluid as used for the
samples) must be analyzed for every 20 .
extractions that have been conducted in on
extraction vessel.
62 . A matrix spike shall be performed for
each waste type (e.g.. wastewater treatment
sludge, contaminated soil, etc.) unless the
result exceeds the regulatory level and the
data are being used solely to demonstrate
that the waste property exceeds the .
regulatory level. A minimum of one matrix •
spike must be analyzed for each analytical' '
batch. As a minimum, follow the matrix spike
addition guidance provided in each analytical
method.
• 82.1 'Matrix spikes are to be added after-
'filtration of the TCLP exlracl and before
preservation. Matrix spikes should not be
added prior to TCLP extraction of the sample.
8.2.2 In most uses, matrix spikes should
be added at a concentration equivalent to the
corresponding regulatory level. If the annlyte
concentration is less than one half the
regulatory level, the spike concentration may
be as low as one half of the enalyte
concentration, but may not be less than five
times the method detection limit. In order to'
avoid differences in matrix effects, the matrix
spikes must bc'added to the same nominal
volume of TCLP extract as that which was
analyzed for the unspiked sample.
8.2.3 The purpose of the matrix spike is to
monitor the performance of the analytical
methods used, and to determine whether -s.
matrix interferences exist. Use of other
internal calibration methods, modification of
the.analytical methods, or use of alternate
analytical methods may be needed to
accurately measure the analyte concentration
of the TCLP extract when the recovery of the
matrix spike is below the expected analytical
method performance.
8.2.4 Matrix spike recoveries arc
calculated by the following formula:
%R (« Recovery) = 100 (X. - XJ/K
• where: . . . . ' ' •
X. = measured value for the spiked sample.
Xu = measured value for the unspiked
sample, and
K = known value of the spike in the sample.
8.3 All quality control measures described
in the appropriate analytical methods shall
be followed. . .
8.4 The use of internal calibration ' ,
quantitation methods shall be employed for a
metallic contaminant if: (I) Recovery of the
contaminant from the TCLP extract is not at
least 50% and the concentration does not
exceed the regulatory level, and (2) The
concentration of the contaminant measured
in the extract is within 20% of the appropriate
regulatory level.
S.i.l The method of standard additions
.shell be employed as the internal calibration
quantitation method for each metallic .
. contaminant. . .•'.••• '• .
8.4.2 The method of standard additions :
requires preparing calibration standards in •
the sample matrix rather than reagent water •'.
or blank solution. It requires taking four
Identical aliquots of the solution and adding •
known amounts of standard to three of these
aliquots. The fourth aliquot is the unknown.
Preferably, the first addition should be . . ..
prepared so that the resulting concentration •
is approximately 50% of the expected
concentration of the sample. The second and
third additions should be prepared so that the
concentrations are approximately 100% and .
150% of the expected concentration of the
sample. All four aliquots are maintained at
the same final volume by adding reagent
water or a blank solution, and may need
: dilution adjustment to maintain the signals in
> the linear range of the instrumental
technique. All four aliquots are analyzed.
8.4.3 Prepare a plot, or subject data to
linear regression, of Instrumental signals or
external-calibration-derived concentrations
as the dependent variable (y-axis) versus
concentrations of the additions of standard
as the independent variable (x-axis). Solve
for the intercept of the abscissa (the
independent variable, x-axis) which is the '
concentration in the unknown.
B-4.4.4 Alternately, subtract the
Instrumental signal or external-calibration-
derived concentration of the unknown
(unspiked) sample from the instrumental
signals or external-calibration-derived
concentrations of the standard additions. Plot
or subject data ;o linear regression of the
corrected instrumental signals or extemal-
calibration-derived concentrations as the :
dependent variable versus the independent-"
variable. Derive concentrations for unknowns
using the internal calibration curve as if it
were an external calibration curve. •. •
8.5 Samples must undergo TCLP
extraction within Ihe'following time periods:
SAMPLE MAXIMUM HOLDING TIMES (DAYS)
Volatile*
Semi-
volabies...
Mercury
Metals.
except
mercury_
From:
field
collec-
tion to:
TCLP
extrac-
tion
14
14
. .' 29
' 180
From:
TCLPex-
tracuon
to:
prepara-
tive
• extrac-
tion
NA
7
NA
NA
From:
pre-
parative
extrac-
tion to:
determi-
native
analysis
14
.40
28
.. 180
TolaS
elapsed
time
28
61
58
360
'• NA=Not apptcabte.
If sample holding times are exceeded,
the values obtained will be considered
minimal concentrations. Exceeding the
holding time is not acceptable.in
establishing that a waste does not
exceed the regulatory level. Exceeding .
the holding time will not invalidate
characterization if the waste exceeds
the regulatory level. . •
PART 271—REQUIREMENTS FOR .
AUTHORIZATION OF STATE . '
HAZARDOUS WASTE PROGRAMS
3. The authority citation for part 271
continues to read as follows: : *
Authority: 42 U.S.C. 6905. 6912(a). and 6928.
4. In § 271.1, paragraph (j). Table 1 is .
amended by adding, the following entry
in chronological order by promulgation
date:
§271.1 Purpose and scope.
•. TABLE 1.—REGULATIONS IMPLEMENTING THE HAZARDOUS AND SOLID WASTE AMENDMENTS OF 1984 -
Promulgation data
Title ol regulation
Federal Register reference
Effective date
November 24.1992.
. ToxJdty Cha/BCtert»tfc Revision 57 FR 55117 publication citation November 24, 1992. ..
(!:R Doc. 92-28320 Filed 11-23-92; 8:45 am]
BILLING COOE 6560-SO-W
-------
TJ
TJ
m
g
x
-------
Appendix II
CCWE List from LDR
Technology-Based Standards by RCRA Waste
Code
CCW List
and
August 18, 1992 Updates to Tables
-------
Environmental Protection Agency
§ 263.41
subpart D levels, the waste is prohibit-
ed from land disposal, and all require-
ments of part 268 are applicable,
except as otherwise specified.
(k) Effective May 8, 1993. D008 lead
materials stored before secondary
smelting are prohibited from land dis-
posal. On or before March 1, 1993, the
owner or operator of each secondary
lead smelting facility shall submit to
EPA the following: A binding contrac-
tual commitment to construct or oth-
erwise provide capacity for storing
such D008 wastes prior to smelting
which complies with all applicable
storage standards; documentation that
the capacity to be provided will be suf-
ficient to manage the entire quantity
of such D008 wastes; and a detailed
schedule for providing such capacity.
Failure by a facility to submit such
documentation shall render such D008
managed by that facility prohibited
from land disposal effective March 1,
1993. In addition, no later than July
27, 1992 the owner or operator of each
facility must place in the facility
record documentation of the manner
and location in which such wastes will
be managed pending completion of
such capacity, demonstrating that
such management capacity will be ade-
quate and complies with all applicable
subtitle C requirements.
[55 FR 22688. June 1. 1990. as amended at
56 FR 3878. Jan. 31. 1991; 57 FR 20770. May
15. 1992; 57 FR 28632. June 26. 1992]
Subpart D—Treatment Standards
§ 263.40 Applicability of treatment stand-
ards.
(a) A restricted waste identified in
§ 268.41 may be land disposed only if
an extract of the waste or of the treat-
ment residue of the waste developed
using the test method in appendix II
of part 261 does not exceed the value
shown in Table CCWE of § 268.41 for
any hazardous constituent listed in
Table CCWE for that waste, with the
following exceptions: D004, D008,
K031, K084, K101. K102, P010. P011.
P012, P036. P038, and U136. These
wastes may be land disposed only if an
extract of the waste or of the treat-
ment residue of the waste developed
using either the test method in 40
CFR part 261, appendix II, or the test
method in appendix IX of this part,
does not exceed the concentrations
shown in Table CCWE of § 268.41 for
any hazardous constituent listed in
Table CCWE for that waste.
(b) A restricted waste for which a
treatment technology is specified
under § 268.42(a) may be land disposed
after it is treated using that specified
technology or an equivalent treatment
method approved by the Administra-
tor under the procedures set forth in
§ 268.42(b).
(c) Except as otherwise specified in
§ 268.43(c), a restricted waste identi-
fied in § 268.43 may be land disposed
only if the constituent concentrations
in the waste or treatment residue of
the waste do not exceed the value
shown in Table CCW of § 268.43 for
any hazardous constituents listed in
Table CCW for that waste.
[52 FR 25790. July 8. 1987. as amended at 55
FR 22689. June 1. 1990; 56 FR 3879. Jan. 31.
1991]
§268.41 Treatment standards expressed as
concentrations in waste extract.
- -(a) Table CCWE identifies the re-
stricted wastes and the concentrations
of their associated constituents which
may not be exceeded by the extract of
a waste or waste treatment residual
developed using the test method in
Appendix I of this part of the allow-
able land disposal of such wastes, with
the exception of wastes D004, D008,
D031, K084, K101. K102. P010. P011.
P012, P036. and U136 and the concen-
trations of their associated constitu-
ents which may not be exceeded by
the extract of a waste or waste treat-
ment residual developed using the test
methods in appendix II of 40 CFR
part 261 for the allowable land dispos-
al of such wastes. (Appendix II of this
part provides Agency gruidance on
treatment methods that have been
shown to achieve the Table CCWE
levels for the respective wastes. Ap-
pendix II of this part is not a regula-
tory requirement but is provided to
assist generators and owners/opera-
tors in their selection of appropriate
treatment methods.) Compliance with
these concentrations is required based
upon grab samples, unless otherwise
noted in the following Table CCW.
791
311-147 O—92-
-26
-------
268.41 TABLE CCWE.—CONSTITUENT CONCENTRATIONS IN WASTE EXTRACT
Wine coda
000*
0007
DOOfl . . ,-, i - .__«__. .. ,
0009 (Lew Mercury
Subcateoory—
less man 260
mg/kg Mercury).
0010
001 1
Commercial
erwmica! name
MA
NA
NA
NA
NA
S««al>o
TatttCCWin
266.43.
TabKCCW in
266.43.
Table CCW in
268.43.
TatteCCW in
268.43.
Table CCW in
268.43.
Table 2 in 266.42
and TabieCCW
in 268.43.
TabieCCW in
268.43.
Table CCW in
268.43.
Regulated hazardous conamuent
Arvmic
C*vrium
C^vornium (Total)
Mercury .
CAS No. tor"
regulated
hazardous
constituent
7440-38-2
7440-39-3
7440-43-9
7440-«7-32
7439-92-1
7439-97-6
7782-49-2
7440-22-4
Wastewaters
Concentration
(mg/l)
NA
NA
NA
NA
NA
NA
NA
NA
Notet
Nonwastewaters
Concentration (mg/
1)
5.0
100
1.0
5.0
5.0
0.20
5.7
5.0
Notes
"
o>
pa
ib.
o
n
TI
JO
r>
•o
KS
F001-F005 »enl
eofvsnts.
F006.
R»7.
F008
F009.
NA
NA..
NA
NA
Tade 2 in 268.42
and Table CCw
in 266.43.
Table CCW in
268.43.
Table CCW in
268.43.
Table CCW in
268.43.
Table CCW in
268.43.
1 .2-0>cf.lOfOOenzene
Etnyi aceuie
Etfiyt etner
Metnyiene chloride . _
Uetr.yl isoburyl ketone — .
Tetrachloroctnyiene
1 1 1-TncnIoroelhane
1.1.2-Tncnlorc- 1^.2-Trdluoretnane
Tnchlorofluoromelhane
YytAn^
Cnromum (Total)
Lead
Hftrl
S9v*r
Cnromum (Total). . „
Lead
Nickel....
Silver ._
Cadmium . . „
Chromium (Total) _
Lead
Nckel
Slver
Cadmium . ..
Cnromium (Total)
Lead
Nickel
Silver _'J
71-36-3
75-15-0
56-23-5
108-90-7
108-94-1
95-50-1
141-76-6
100-41-4
60-29-7
78-83-1
67-56-1
75-9-2
78-93-3
108-10-1
S8-95-3
110-86-1
127-18-4
108-68-3
71-55-6
76-13-1
79-01-6
7S-69-4
7440-43-9
744(M7-32
7439-92-1
7440-02-0
7440-22-4
7440-43-9
7440-47-32
7439-92-1
7440-02-0
7440-22-4
7440-43-9
744CM7-32
7439-92-1
7440-02-0
7440-22-4
7440-43-9
7440-17-32
7439-92-1
7440-02-0
7440-22-4
50
1.05
005
0 15
2 82
0 125
0.65
0.05
0 05
0.05
50
025
0.20
005
005
066
1 12
0.079
1 12
1 05
1.05
0062
0.05
005
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
0.59
5.0
4.81
0.96
0.05
0.75
0.75
0.125
0.75
0.053
0.75
5.0
0.75
0.96
0.75
0.33
0.125
0.33
0.05
0.33
0.41
0.96
0.091
0.96
0.15
0.066
5.2
0.51
OJ2
0.072
0.066
5.2
0.51
0.32
0.072
0.066
5.2
0.51
0.32
0.072
0.066
5.2
0.51
0.32
0.072
m
O
3
3
o
3
83
•
3
-------
Wute cods
F011
F012
F020-«>aand
F026-F028 d-onn
containing
mite* '.
ConvTmtLial
ctwmical name
NA
NA..
NA
NA
NA
See also
Table CCW in
268.43.
Table CCW in
268.43.
Table CCW in
268.43.
NA
Table CCW in
258.43.
Table CCW m
2S3.43
Table CCW m
268.43.
Regulated hazardova corottuont
Cnronxjm (Total)
Cadmium
LeaC « •
Nickel — •
Chromium (Total]
HiCDD-All HexacnlonxJib«nzr>p-daiinj._.
HiCDf -AT Heuchlorc-dibonzofurans
PeCOO-AII Pentachloro-diOeruo-p-d>OHns...
PeCOF-AII Penuchioro-dibeniolurans
TCOO-Ali Tet/acniofO-diberurc-p-c'ionns
TCOF-Aii Teuacnloro-ditwruoturans _ _.
Leai
Nickel
Nickel
Lead
CAS No. tor
hazardous
corutjtuent-
7*40-43-9
7440-47-32
7439-92-1
7440-02-0
7440-22-4
7440-43-9
7440-47-32
7439-92-1
74404)2-0
7440-22-4
7440-47-32
95-95-1
88-06-2
56-90-2
87-66-5
7440-«7-32
7435-92-1
7440-02-0
7440-36-0
7440-38-2
7440-39-3
7440-43-9
7440-47-32
7435-92-1
7433-97-6
[ 7440-02-0
7782-49-2
7440-22-4
7435-92-1
Waatewater)
ConccHttration
(mg/l)
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
<1 PPb
<1 PPb
<1 PPb
<1 PPb
<1 ppb
<1 ppb
<0.05 ppm
<0.05 ppm
<0.01 pom
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
, NA
NA
Notes
Nonwastewalen
Concentration (mg/
1)
0.066
5.2
0.51
0.32
0.072
0.066
5.2
0.51
0.32
0.072
5.2
<1 ppb
<1 PPb
" ,
K022
K028
KM1
taut
Ktvtfi
K040
tcavt
KM!
KOW
K061 (Low Zinc
Subcaligor/—
kij inan 15%
Total Zinc).
NA.
NA
NA .. _.
NA
NA
NA
NA_
NA
NA
NA
NA.. _
NA
NA
NA
NA
Na
NA
ua
NA
Tab* CCW in
268.43.
TabJ« CCW in
258.43.
Table CCW in
268.43.
268.43.
Table CCW in
268.43.
Table CCW in
26843.
Tab* CCW in
268.43.
Table CCW in
263.43.
Tatle CCW in
268.43.
Table CCW in
268.43.
Table CCW in
268.43.
Table CCW in
268.43.
Table CCW in
268.43.
268.43.
Table CCW in
268.43.
Table CCW in
268.43.
Table CCW n
268.43.
Table CCW in
268.43.
Table CCW «
268.43.
Table CCW in
268.43.
Leac
Leac
Leac ._.
Lead
CJVomium (Total)
Leai __
Civonium fToal)
Lead _ „
Chromium (Total)
Lead „.. . .
Qvorruum fTotaf)
Nickel _ _ _„
Nickel -.
Latd ._. .
Nickel
Lead. ._ ...
Chronvum (Total)....
Nickel
Chromium (Total)
Nickel _
Chromium (Total)
Nickel .
Chromium (ToMQ _.,..,
Nickel
Chromium (Total)
Nickel ..
Cadmium .
Chromium (Total)
Lead
Nickel _. _. .. _
7.U CM7-32
743&-92-1
7*40-47-32
7<39-92-1
7KCM7-32
7439-92-1
7440-47-32
7439-92-1
7440-47-32
7439-92-1
7440-47-32
744C-47-32
7439-92-1
7440-47-32
7439-92-1
7440-47-32
7440-02-0
7440-3&-0
7440-47-32
7440-02-0
7440-47-32
7439-92-1
7440-02-0
7440-M-2
7439-92-1
7440-47-32
7440-02-0
7440-47-32
7440-02-0
7440-47-32
7440-02-0
7440-47-32
7440-02-0
7440-(7-32
7440-02-0
7440-43-9
7440-47-32
7439-92-1
7440-02-0
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
0.094
0.37
0.094
0.37
0.094
0.37
0.094
0.37
0.094
0.37
5.2
O.OS4
0.37
0.094
0.37
1.7
0.2
0.23
5.2
0.32
0.073
0.021
0.088
5.6
0.18
1.7
0.20
1.7
0.20
1.7
0.20
1.7
0.20
1.7
0.20
0.14
5.2
0.24
0.32
tn
s
o
3
3
a
•o
^
o
n
02
3
C)
ten
M
O-
-------
Waste codv
K061. High Zinc.
Subeategory.
K069(Caloum
Suttate
Subeategory).
K071
K083
K086
K087
K106 (Low Mercury
Scbcategory—
toss than 260
mg/kg Mercury —
resiaues from
RMERQ.
Commercial
cnwnical name
Electric Are
Furnace OusL
NA
NA _ _.
NA
NA
NA
NA
NA
NA
Scearso
Table CCw m
268.43.
Table 2 in 268.42
and Table CCW
in 268.43.
Table CCW in
268.43.
Table CCW m
268.43.
Table CCW in
268.43.
Table CCW in
268.43.
Table CCW in
268.43.
Table CCW in
266.43.
Table CCW in
268.43.
Table CCW in
268.43.
Table 2 m 268.42
and Table CCW
in 268.43.
Regulated hazardous constituent
Arsenjc -
Banum „
Nickel
Sihrer
2mc -
Nickel
Lead -
Lead
Lead
CAS No. for
regulated
hazardous
constituent
NA"
NA
NA
NA
NA
NA
NA
NA
NA
- NA
NA
NA
NA
NA
7440-43-9
7439-92-1
7439-97-6
7440-02-2
7440-38-2
7440-47-32
7439-92-1
7433-92-1
7440-13-9
7110-47-32
7439-92-1
7440-38-2
7440-38-2
7439-97-6
Wastewaters
Concentration
(mg/l)
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Notes
2.1
0.055
7.6
0.014
0.19
0.33
0.37
0.009
5
.0.16
0.3
0.078
Re-
served
5.3
Nonwaslewaters
0
0.14
0.24
0.025
0.088
S.6
0.094
037
05;
0.066
5.2
0.51
5.6
5.6
0.020
Notes
o
<0
10
m
a
K106 (Low Mercury
Subeategory—
test man 260
mg/kg Uercury—
that are not
residues fiuiii
RMERQ.
K115
P010
POII
P012
P013
P036
P038
P065 (Low Mercury
Subeategory—
Leu man 260
mg/kg Mercury—
residues from
RMERQ.
P065 (Low Mercury
Subeategory—
Less man 260
mg/kg Mercury—
ndnerator
residues (and are
not rescues from
RMERQ).
POM
P074
POS2 (Low Mercury
Subcattgory—
Lets than 260
mg/kg Mercury—
residua from
RMERQ.
NA
NA
Arsenic acxj
A/Mnic pefltcrioe.
Arsenic friocoe
Barium cyanide
OictlloropheryUr.
SIM.
Diethytarsine
Mercury tulrrvnate
Mercury fufmrnaie
Nie*el carbonyl
Nickel cyanide
Phenyl mercury
acetate.
. Table 2 in 268.42
and Table CCW
«i 268.43
Table CCW in
268.43.
Table CCW in
268.43.
Table CCW in
268.43.
TaNeCCWin
268.43.
Table CCW in
268.43.
Table CCW in
268.43.
Tab* CCW ti
Tab* 2 in 268.42
and Table CCw
in 268.43
Table 2 in 268.42
and Table CCW
in 268.43.
f
Table CCW in
268.43.
Table CCW n
268.43
Table 2 in 268.42
and Table CCW
r 26843
Mercury _ _...
NckH
Arsenic _
Arsenc „
Arsenic ™
Arsenc
Mercury..
Mercury
Nickel
Nickel
Mercury. „
7440-38-2
7439-S7-6
7439-97-6
NA
NA
NA
NA
NA
0.025
0.32
5.6
5.6
5.6
52
5.6
5.6
0.20
0.025
0.32
1.32
m
3
e
s
3
o
3
3
r>
-------
268.42
(b) When wastes with differing
realment standards for a constituent
f concern are combined for purposes
f treatment, the treatment residue
lust meet the lowest treatment stand-
rd for the constituent of concern,
xcept that mixtures of high and low
Inc nonwastcwatcr KOG1 are subject
o the treatment standard for high
IncKOSl.
il PR 40642, Nov. 7. 1000; 52 FR 21017.
line 4 1087. as amended at 55 FB 22080.
unc 1. 1000; 50 FR 3870. Jan. 31. 1001: 50
'R 41177, Aug. 10, 1001; 57 FR 8080. Mar. 0,
902)
268.42 Treatment standards expressed us
specified technologies.
(a) The following wastes In para-
raphs (a)(l) and (a>(2> of this section
nd In Table 2 and Table 3 of this see-
on must be treated using the tech-
ology or technologies 'specified In
aragraphs OAS:
ILGM:
OOG:
Venting ol comprosaod gases into an absorbing or (oociing modia (i.o.. wild or liquid)—voniing can be
accomplished through physical roleene utilizing valves/piping; physical penetration ol the container; and/oi
penetration Uvouflh delonalion.
Amalgamation ol liquid, elemental mercury contaminated with radioactive materials utilizing Inorganic roagonls
such at copper, zinc, n'ckol. gold, and sullur that result in a nonliquid, semi-solid amalgam and thereby
reducing potential emissions ol elemental mercury vapors to I ho til,
BtodegradaUon ol otganlce or non-metallic inorganlca (i.e.. dogredablo inorganics that contain the elements ol
phosphorus, nitrogen, and sutlur) in units operated under either aerobic or anaerobic conditions such lhat a
surrogate compound or Indicator parameter hat boon substantially reduced in concentration In iho residuals
(e.g.. Total Organic Cartoon can ollon b« used as an indicator parameter lex Ihe bkxlogradalion ol many
organic constituents that cannot be directly analyzed in weslowalor residues).
Environmental Protection Agency
§ 268.42
TADLE 1.—TECHNOLOGY CODES AND DESCRIPTION OF TECHNOLOGY-BASED STANDARDS—
Continued
Technology
code
Description ol technology-based standards
CARDN:
CHOXO:
CURED:
DEACT:
FSUUS:
IILVIt:
INCIN:
LLEXT:
NEUTM:
NLU8R:
PRECP:
nnEHY;
IICGAS:
RCORR:
RlEAO:
Caibon adsorption (granulated or powdered) ol non-metallic Inorganics, organo-metallica. and/or organic
constituents, operated auch that a surrogate compound or indicator parameter has not undergone
breakthrough (e.g.. Total Organic Cartwn can ollen bo used as an indicator parameter lor the adsorpljon ol
many organic constituents that cannot be directly analyzed in wastewalor residues). Breakthrough occura
when the carbon has become saturated with the constituent (or Indicator parameter) and substantial
change In adsorption rate associated with thai constituent occurs.
Chemical or electrolytic oxidation utilizing Ihe following oxidation reagents (or waste reagents) or combinations
ol reagents: (I) Hypochlorilo (e.g. bleach); (2) chlorine: (3) chlorine dioxide: (4) ozone or UV (ultraviolet
lighl) assisted ozone: (5) peroxides: (6) persullates; (7) perchloratoa; (6) permangantes; and/or (9) other
oxidizing roagonls ol equivalent efficiency, performed In unils operated such thai a eunogalo compound or
indicator parameter has been substantially reduced in concentration in the residual* (e.g.. Total Organic
Cnrbon can often be used as an indicalor parameter for Ihe oxidation ol many organic constituents lhat
cannot be directly analyzed in wastowalor residues). Chemical oxidation specifically includes what is
commonly referred lo as alkaline chlorinalion.
Chemical reduction utilizing tl>e following reducing reagenta (or waste reagents) or combinations ol reagents:
(I) Suilur dioxide; (2) sodium, potassium, or alkali aalts or sullites, bisullitos, metabijullites. and polyethyl-
ene glycols (e.g.. NaPEG and KPEG); (3) sodium hydrosullide; (4) ferrous Mils; and/or (5) other reducing
reagents ol equivalent efficiency, performed In units operated such thai a surrogate compound or indicalor
parameter has boon substantially roducod in concentration in the residuals (e.g.. Total Organic Halogens
can ollen be used as an indicator parameter lor Ihe reduction ol many halogenated organic constituents'
Ihnt cannot bo diroclly analyzed in wastowalor residues). Chemical reduction is commonly used lor the
reduction ol hoxavolont chromium to the trivolont stale.
Oonclivolkxi to remove Iho hazardous characteristics of a waslo duo to is ignilability. corrosrviry, and/or
reactivity.
Fuol substitution in unils operated in accordance with applicable technical operating requirement*.
Vitrification ol high lovol miiod radioactive wastes in unils In compliance with all applicable radioactive
protection requirements under control of the Nuclear Regulatory Commission.
Incineration ol wostos containing organics end mercury in unils operated in accordance with Ihe technical
operating requirements ol 40 CFH pan 264 subpart 0 end part 265 subpart 0. All waslewaler and
nonwastowater residues derived from Ihis process musl then comply wilh the corresponding treatment
standards per waslo coda wilh consideration ol any applicable subcalegorios (e.g.. High or Low Mercury
Suucatoyorios).
Incineration in units operated in accordance wilh Iho technical operating roquiromonls ol 40 CFR part 264
subpart 0 and part 265 subpart 0.
Liquid-liquid oxliaclion (ollon rolurrod to as solvent extraction) ol organics Irom liquid waslos into an
irnmiscililo solvent fur which tho haiardous constituents have a groalur solvent alftnity. resulting In an
oitincl high in oiunnics Hint must undergo either incineration, rouse as a fuel, or other rocovory/rouse and
a rallinato (extracted liquid wasle) proportionately low in organics that musl undergo lurlhor treatment as
spocifind in the standard.
Mncrooncnpsiilntion wilh Builncn conling materials such as polyrnorlc orgonics (e.g. rosins and plastics) or
wilh a jnckol ol iriuil inorganic materials lo substantially reduce surface exposure lo potential leaching
media. Macrooncapsulalion specifically does not include any material (hat would bo classified as a tank or
container according to 40 CFR 200.10. « «
Neutralization wilh Iho following roagonls (or waslo reagents) or combinations ol roagonls: (1) Acids: (2)
bases; or (3) water (including wasiowaters) resulting in a pH greater than 2 but less than 12.3 as measured
in Iho aqueous residuals.
No land disposal based on recycling.
Chemical precipilalion ol metals and other inorganics as insoluble procipitatos ol oxides, hydroxides,
carbonates, sullidos, sullatos. chlorides, llouridos. or phosphates. The following reagents (or wasle
reagents) are lypicolly used olono or in combination: (1) Lime (i.e.. containing oxides and/or hydroxides ol
calcium and/or nmgnosium; (2) couslic (i.e.. sodium and/or polassium hydroxides; (3) soda ash (i.e., sodium
caibunalu): (4) stxlnmi sullulo: (0) ferric sutlolo or lorric chloride; (G) atum; or (7) sodium sullato. Additional
lloculnling. coagulation or similar roagonls/procossas (hat enhance sludge dowatoring characlerislica are
not precluded from uso.
Thermal recovery ol Beryllium.
Rocovory/reuse ol compressed gases including techniques such as reprocessing ol me gases lor reuse/
resale: littering/adsorption ol impurities; remixing lor direct reuse or resale: and use ol Ihe gas as a fuel
source.
Recovery ol acid* or bases utilizing one or more ol Ihe following recovery technologies: (I) Distillation (i.e.
thermal concentration); (2) ion exchange: (3) rosin or solid adsorption; (4) reverse osmosis: and/or (5)
incineration lor the recovery ol acid—Note: Ihis does not preclude the use of other physical phase
separation or concentration techniques auch aa decantatlon, filtration (including uluafill/ation). and centritu-
gation, when used in conjunction wilh Ihe above lislod recovery technologies.
Thermal recovery ol load In secondary lead amollers.
-------
8.42
40CFR Ch. I (7-1-92 Edition)
ABLE 1.—TECHNOLOGY CODES AND DESCRIPTION OF TECHNOLOGY-BASED STANDARDS—
Continued
nology
>de
Description ol technology-based standards
RX:
Retorting o» roasting in a thocmal procossing unit copabto ol volaiiiiring moicury and subsequently coiulonsing
U>e volatilized mercury lor recovery. Tho (Otofting or roosting unit (or facility) must bo subjocl to ono or
more ol the following: (a) a National Emissions Standard (or Heiardous Air Pollutants (NESHAP) lor
mercury; (b) ft Qosl Available Control Technology (BAGI) or a Lowest Achievablo Emission Rato (LAER)
Standard lor mercury Imposed pursuant to a Prevention ot Significant Dolor to f a lion (PSD) permit; or (c) a
slate permit that establishes emission limitation* (within moaning ol section 302 ol the Clean Air Act) lor
morcury. All wastewater and nonwastowaior residues derived from this process must thon comply with the
corresponding treatment standards pet waste code with consideration ol any applicable subcalogorios (e.g..
High or Low Mercury Subcaleoorios).
Recovery ol mo tali or inorganics utilixing one or moro ol tho following direct physical/removo! technologies:
(1) Ion exchange: (2) resin or solid (i.e.. roolilos) adsorption: (3) reverse osmosis; (4) cholalion/solvont
extraction; (S) freeze cry stain a (ion: (6) ullralillration and/or (7) simple precipitation (i.e., crvsioiijation}—
Noto: Thii does not preclude tho use ol other physical phnso soporotion or concontiaton techniques such
as docantation. filtration (including ultra It! (ration}, end contrilugation. when used in conjunction with Iho
above listed recovery technologies.
Recovery ol organic! utilizing one or more ol the following technologies: (1) Distillation; (2) thin film
evaporation: (3) steam stripping; (4) carbon adsorption; (S) critical fluid extraction; (6) liquid-liquid extraction;
(7) prectpi la lion/cry st alii a iton (including Irooio crystallization); or (6) chemical phase separation techniques
(i.e.. addition ol acids, bases, domulsiliors. or similar chemicals):—Note: this does not preclude tho use ol
other physical phase separation techniques such as a docantalion. filtration (including ullraiiilralion). and
centnlugalion. when used in conjunction with Iho above listed recovery technologies.
Thermal recovery ol metals or inorganics from nonwastowaiors in units idonliliod as industrial furnaces
according to 40 CFR 260.10 (1). (6). (7), (It), and (12) under Iho definition of "industrial furnaces".
Rosmelling in high temperature metal recovery units lor Iho purpose ol recovery ol line.
Stabttiialion with the following reagents (or waste reagents) or combinations ol reagents: (1) Portland comonl;
or (2) Ume/pouolans (e.g.. fly ash and cement kiln dust)—tins does not prucludo tfra addition ol reagents
(e.g.. iron salts, silicates, and clays) designed to enhance the set/cure time and/or comprossivo strength.
or to Overall reduce (he teachability ol the metal or inorganic.
Steam stripping ol organic* from liquid wastes utilizing direct application ol Bloom to the wastes oporaloU
such (hat liquid and vapor (low (atos. as well as. temperature and pressure tangos have boon opnmcod.
monitored, and maintained. These operating parameters are dependent upon Iho design parameters of Iho
unit such as, tho number ol separation stages and Iho internal column design. Thus, resulting in a
condensed exl/acl high in organics that mual undergo either incineration, rouse as a fuel, or other
recovery/rouse and an extracted wastewator (hat must undergo further Iroatrnonl as specified in the
standard.
Wet air oxidation performed in units operated such that a surrogate compound or indicator pnromotor has
boon substantially reduced in concentration in the rooiduoli (e.g.. Total Organic Carbon crtn olion bo used
as an indcalor par a mot or lor the oxidation ol many organic constituents that cannot bo ditoctty analyioU in
wastowBter residues).
Controlled roacuon with water lor highly reactive inorganic or organic chnrmcnls with precautionary control*
for protection of workers from potential violent reactions as well as procauliona/y controls lor potential
emissions ol to*ic/ignitable levels ol gases released during Iho reaction.
le 1: When a combination of these technologies (i.e.. a treatment train) is specified as a single treatment standard. Iho
ol application is specified in 8268.42. Table 2 by indicating the live letter technology codo that must bo applied first.
the designation "Ib." (an abbreviation for "followed by"), then tho Irvo letter technology code for the technology that must
>plied next, and so on.
t« 2: When more than one technology (or treatment train) are specified as atio/nativo treatment standards. Iho five letter
otooy codes (or (he treatment (rains) are separated by a semicolon (;) with tho last technology preceded by the word
'. This indicates that any one ol UMS* BOAT technologies or treatment trains can bo used lor compliance with Iho
266.42 TABLE 2.—TECHNOLOGY-BASED STANDARDS DY RCRA WASTE CODE
isle
>de
Gee also
NA _
NA
Waste descriptions
and/or treatment
subcttegory
Ignllable Liquids bated
on 26I.J1(o)(l)-
Waslcwalers.
Ignilable Liquids bnaed
on 201.2l(«)(t)— Low
TOO Ingitable UqukU
Sutealegory— Lest
than 10% total
organic carbon.
CAS No. lor
regulated
hazardous
constituents
NA
NA
loclinology codo
Watlewalors
DEACT
NA
Nonwastowators
NA.
DEACT.
Environmental Protection Agency § 268.42
208.42 TADLE 2.—TECHNOLOGY-BASED STANDARDS ov RCRA WASTE CODE—Continued
Wmlo
code
DOOI
DOOI
DOOI
DOOI
D002
DO02
DOO2
D003
D003
D003
0003
UOOO
DOOO
UOOO
Soo alto
NA
NA
NA
NA
NA
NA
NA
NA...
NA
NA
NA
NA
NA
Tablo CCWE
in 260.41
end TablO
CCW in
266.43.
Wosln do&ciiptions
and/or tioalinont
•ubcaloyoty
Igniloblo Liquids baiod
on 2GI.2l(a)(l)—
High TOO Inglublo
Liquid*
Subcalogory—
Gioalor than or equal
lo 10% lolol oiganic
carbon.
Ignilablo comprosaed
gosos basod on
201.21(8)13).
Ignilablo rooclrvoa
basod oil
201.2l(a)(2).
Oxidizors based on
20l.21(a)(4).
Acid subcaiogory basod
on 26l.22(o)(1).
AlKalino subcaiogory
based on
26l.22(a)(l).
Olhor corrosives basod
on 20l.22(a)(2).
Ronclivo Sullidoa
basod on
2C1. 20(0)16).
Eiplosivos bosod on
2GI.23(a)(G). (7). and
0).
Walof rflnclivos basod
on 201.23(0)12). (3).
and (4).
Oihoi toaciivos basod
on 20l.23(a)(l).
Cnilnmim conloining
bolloiios.
Load nod hallmios
(Noto: This slandnid
only nnphos lo lond
ocid boiioiios lhai
are idonliliod as
RCRA haiordous
woslos and lhal are
not excluded
elsowhoro From
regulation undor Iho
land disposal
rostnclionB ol 40
Crn 206 or
OKdmplod undor
Olhor EPA rouulaliuiis
(9oo 40 Cm 2CC.OO.).
Morculy: (High Moicury
Subcatogory — groator
than or equal lo 260
mg/kg total
Morcury— contains
moicury and organica
(and aro not
Incinerator residues)).
CAS No. tor
rogulnlod
hazardous
consliluonls
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
7440-43-0
7439-02-1
7439-97-0
Technology code
Waslewatoit
NA
NA
NA
DEACT
DEACT
DEACT
DEACT
DEACT but not
Including dilution as a
substitute lor
adequate treatment..
DEACT
NA
DEACT
NA
• .
NA
Nonwajtewatera
FSUDS; nonGS: or
INCIN.
DEACT.'
DEACT.
OEACT.
DEACI.
DEACT.
DEACT.
OEACT but not
including dilution as a
substitute tor
adequate treatment.
DEACT.
DEACT.
OEACT.
R1HRM.
RLEAD.
IMERC: or RMERC.
-------
68>42 40 CFR Ch. I (7-1-92 Edition)
268.42 TABLE 2.—TECHNOLOGY-BASED STANDARDS QY RCRA WASTE CODE—Continued
aslo
otto
)
I
)
l
i
1
1
i
>
<
t
:6
:J
0
14
IS
17
Soo alw
Table CCWE
in 268.41
and Tablo
CCWin
266.43.
Tablo CCW In
208.43.
Table CCW In
268.43.
Table CCW in
268.43.
Table CCW In
268.43.
Table CCW in
268.43.
Table CCW In
268.43.
fablo CCWE
in 266.41
and Table
CCWin
268.43.
Table CCWE
In 268.41
and Tab*
CCW in
260.43.
Table CCWE
in 268.41
and Tablo
CCWin
268.43.
NA
Waslo descriptions
and/or tionlmon!
•ubcatogory
Moicury: (High Mercury
Subcatogory— greater
(Man or equal to 2CO
mg/kQ lota)
Mercury— inorganics
(includtno incinerator
residues and residues
Horn FlMEnQ).
24-D
2-Elhoxyothenol
Distillation bottoms
Irom tho production
ol nilrobonjono by
Itio nitration ol
tMiuono.
Stripping 8UII loiln Irorn
(he production ol
nx>lhyl olhyl pyiidinos.
Contrilugo and
distillation residues
from loruono
dtisocyanalo
pfOduction.
Fillor CDKe from Ilio
lillralion ol
diollirlpHonplioiodillv
loic acid In Uio
production ol ptioialo
Waslowator uoatmonl
tludgot from tho
manufacturing and
processing ol
oxploaivel.
Spent caibon Irom the
treatment ol
wastewaler
containing explosives
Pink/rod water Irom
TNT oporauona.
CAS No. loc
louutnlod
hniordous
constituents
7439-97-0
72-20-8
SO-09-0
J2-4J-J
8 001-35-1
94-75-7
93-72-1
79-46-9
110-00-0
NA
NA
NA
NA
NA
NA
NA
NA
1 ochnology codo
Woslowntors
NA
OIOOG: or INCIN
CAI1UN; or INCIN
WIMOX: or INCIN
OIOOG: or INCIN
CHOXD; DIODG; or
INCIN.
CHOXO: or INCIN
WETOX or CHOXD) Ib
CAflUN: or INCIN.
DIODG- or INCIN
INCIN
unxr ib ssinp it>
CARUN; 01 INCIN.
INCIN
CARUN; or INCIN
CAflUN; or INCIN
UliACr
DEACT
DEACT
NunwaslowolOrs
nMEMC.
NA.
NA.
NA.
NA.
NA.
NA.
NCIN
INCIN.
INCIN.
INCIN.
INCIN.
FSUBS: or INCIN.
FSUUS: or INCIN.
UEACT.
OEACT.
DEACT.
Environmental Protection Agency § 268.42
268.42 TAOLE 2.—TECHNOLOGY-BASED STANDARDS BY RCRA WASTE CODE—Continued
code
K009
KI08
K113
Kl 14
KII5
Kl 10
PO01
POOZ
P003
POOS
POOB
POOO
POI4
P01S
POIO
POI7
S*H> alfto
Tabto CCWE
In 200.4 1
arid Tablo
CCW in
2O6.43.
Tablo CCWG
In 206.4 1
ami Tahlo
CCWin
200.43.
NA
NA
NA
NA
NA
NA
NA ,
NA
NA
NA
NA .. .
NA
NA
NA
NA
NA
Waato doacrtpiiont
aitd/or Iroalinont
tubcaiogory
Emission cont/ol dual/
tludyo (torn
aocottda/y load
•molting: Non-
Calcium Sulla!*
Subcalogory.
WaatowBtor treatment
eludgo from Iho
morcuy coll ptocott
in chkxin*)
ptoOuclion: (High
Morcu>y
SutKalogoty — groolnr
limn 01 oqual to 260
mg/Kg total morcury).
ConOonsod liquid light
onds l/om the
pufiftcalion ol
toluonodinmino In Iho
production of
lofuonodiomino via
hyUiogonalKjn ol
dtiiiiroioiuono.
putilicalton ol
loluonodiamino In tho
production o<
loluonodinmirxi via
hydfogonatioo ol
llinilfOIoluono.
pufiftcialion ol
loluonodiamino in Iho
production of
totuonodiamino via
hydrogonation ol
dinilroioluomo.
Iroin Ihn aorvenl
focovoty colunm in
Iho pioduction of
loluono diisocyanalo
via plwogonAtcn ol
loluonodiamino.
Wa/laiin (>0.3%)
1 -Acotyl-2-lhiouf oa
lAOnatolol.
Airvnonfum picralo
thiol).
OrOfTx>acoton«
CAS No. lor
constjtuonti
NA
NA
NA
NA
61-61-2
501-06-2
107-02-6
20050-73-6
131-74-6
106-66-5
542-86-1
598-31-2
Tochno*.
Waal aw* ion
NA
NA
CARBN- or INCIN
CARBN- or INCIN
* •
(WETOX or CHOXO) ft
CARBN; or INCIN.
(WETOX or CHOXD) ft)
CARBN; or INClN.
CARON; or INCIN.
INCIN.
CARON; or INCIN.
CARBN; or INCIN.
CHOXO; CHREO.
CARBN; BIOOG; or
INCIN.
CARBN; or INCIN.
CAF1BN; or INCIN.
(WETOX or CHOXO) Ib
CAflBN: or INCIN.
ogy codo
Nonwatlewatwt
PLEAD
RMERC
FSUBS: or INCIN.
INCIN.
INCIN.
FSUBS: CHOXO;
CHREO; or INCIN.
INCIN.
-------
,8.42 40 CFR Ch. I (7-1-92 Edition)
!68.42 TABLE 2.—TECHNOLOGY-BASED STANDARDS OY RCRA WASTE CODE—Continued
110
la
\
1
I
I
i
>
6
Sen also
NA
Table CCW in
268.43.
NA
HA
NA
NA
NA
NA
NA
NA
NA
Table CCW In
266.43.
NA . .
NA
NA
Table CCWE
in 208.41
•nd Tablp
CCW in
260.43.
Table CCWE
in 268.4 1
and Table
CCW In
266.43.
NA
Waste descriptions
•nd/or Iroalmonl
•ubcategory
liucino
Chloroacotaldohydo
Mo-Cnlorophonyl)
Iniourea.
3-Chloropropioniuilo
Cyanogen
2-Cycloheiry|.4,6-
dinitrophonol.
O.O-Diolhyl O-pyiozinyl
phosphorothioate.
>othy1.p-nilrophenyl
phosphalo:
Epinoptwino
Diisopropyl
lluorophosphalo
(DFP).
Dimelhoale .'i
alpha. alpha-
Dime Ihylphonolhyla-
mine.
4.6-Dinilro-O-cresOt
sails.
2 4-Dilhiobiuret
Flixxoacolic acid,
sodium sail.
Hexaethylteuaphos-
phato.
Isocyanic acid, ethyl
osier.
Motcury tulmitiolo:
(High Moicury
Subcelugory— yiootor
man of equal 10 2CO
mg/Kg total
Moicury— either
incinerator residues
or residues from
RMERC).
Mercury lulminalo: (All
Nonwaslewaslers
lhal are not
Incinerator residues
or are not residues
Irom RMERC:
regardless of Mercury
Content).
Melhomyl
CAS No. lor
regulated
hazardous
constituents
357-57-3
75-15-0
107-20-O
5344-82-1
542-76-7
100-44-7
4CO-IO-5
506-77-4
131-88-5
287-97-2
311-45-5
51-43-4
55-01-4
00-51-5
39196-18-4
122-09-8
534-52-1
541-53-7
151-5C-4
7702-41-4
640-19-7
62-74-B
757-58-4
624-63-9
020-OC-4
626-66-4
16752-77-5
Tecluiology code
Waatewators
WETOX or CHOXD) IU
CARBN: or INCIN.
NA
(WETOX or CHOXD) Ib
CARBN; or INCIN.
(WETOX or CHOXU) Ib
CAHDN; or INCIN.
WEIOX or CHOXU) Ib
CARON: 01 INCIN.
WEIOX 01 CIIUXU) Ib
CARON; or INCIN.
CIIOXO; WLIOX or
INCIN.
CHOXD: WEIOX or
INCIN.
(WETOX or CHOXD) Ib
CARBN: or INCIN.
CARBN; or INCIN
CARDN; or INCIN
(WETOX or CHOXU) Ib
CARBN; or INCIN.
CARDN; or INCIN
CARBN- or INCIN
(WETOX or CHOXD) Ib
CARBN; or INCIN.
(WETOX or CHOXD) Ib
CARON; or INCIN.
(WETOX or CHOXD) Ib
CARDN; or INCIN.
(WETOX or CHOXO) Ib
CARDN: or INCIN.
(WETOX or CHOXO) Ib
CAIIUN; or INCIN.
NA
(WETOX o« CHOXD) Ib
CARON: or INCIN.
(WETOX or CHOXD) Ib
CARBN; or INCIN.
CARBN; or INCIN
(WEIOX or CHOXD) Ib
CARQN: or INCIN.
NA . .
NA
(WETOX or CHOXD) Ib
CADBN; or INCIN.
Nonwastowalors
NCIN.
NCIN.
NCIN.
NCIN.
NCIN.
NCIN.
CHOXD: WETOX; or
INCIN.
CHOXO; WETOX: or
INCIN.
NCIN.
FSUDS; or INCIN.
FSUDS; or INCIN.
NCIN.
FSUUS; or INCIN.
FSUDS or INCIN.
INCIN.
INCIN.
INCIN.
INCIN.
INCIN.
ADGAS IbNUUIII.
INCIN.
INCIN.
FSUDS; or INCIN.
INCIN.
MMERC.
IMERC.
INCIN.
Environmental Protection Agency
268.42 TABLE 2.—TECHNOLOGY-BASED STANDARDS
§ 268.42
BY RCRA WASTE CODE—Continued .'
Wnslo
code
POO 7
I'OGB
P069
P070
P072
P075
I'OCG
P07B
P061
P082
P004
POOS
POO 7
POOD
P092
I'OU2
P093
POOS
ruin;
PI02
PI05
PIOO
PI08
PII2
PII3
PUS
See also
NA
NA
NA
NA
NA
NA
NA
NA
NA
Taulo CCW in
208.43.
NA
NA
NA
NA
Table CCWE
in 260.41
and Table
CCW in
2GB.43.
1 nlilo CCWE
in 2G0.4I
and Table
CCW in
260.43.
NA
NA
NA
NA
NA
NA
NA
NA
Table CCW in
208.43.
Table CCW in
268.43.
Woslo descriptions
anil/or treatment
subcatogory
Molhyllaclonilrilo
Aldicarb
1 •Naphlhyl-2-lhiouriia
Nilrogon dioxide
N>Nilrosodimothylamino ..
N-
Nilrosomolhylvinyla-
mine.
OclamolhylpyroplK>s*
phoramido.
Endotliall
Phony! mercury
acetate: (High
Mercury
Subcatogory — greater
than or equal to 2GO
mg/kg total
Mercury — oilhor
incinerator residues
or residues Irom
RMERC).
I'hnnyl mercury
aculolo: (All
nonwasiowaiors that
aro not incinerator
residues and aro not
residues Irom
RMCRC: regardless
ol Mercury Content).
Phosgene
Sodium elide
Strychnine and salts
Tolraolhyldilhiopyro-
phosphalo.
Totranitromolhano
Thallium (1) sullale
CAS No. lor
rogulalod
hazardous
constituents
75-55-8
60-34-4
75-06-5
116-06-3
06-06-4
1 54-11-5
10102-43-9
10102-44-0
55-63-0
62-75-9
4549-40-0
152-16-9
20016-12-0
145-73-3
62-38-4
62-30-4
I03-BS-5
75-44-5
7003-SI-2
107-19-7
2G62B-22-8
' 57-24-9
3689-24-5
509-14-8
1314-32-5
7446-18-6
Technology code
Waslewators
(WETOX or CHOXD) Ib
CARQN; or INCIN.
CHOXD; CHRED:
CARDN: OIODG; or
INCIN.
(WETOX or CHOXD) Ib
CARBN: or INCIN.
(WETOX or CHOXD) Ib
CARBN: or INCIN.
(WETOX or CHOXD) Ib
CARDN: or INCIN.
(WETOX or CHOXO) Ib
CARDN; or INCIN.
ADGAS
ADGAS
CHOXD; CHRED;
CARQN; BIODG: or
INCIN.
NA.
(WETOX or CHOXD) Ib
CARBN: OR INCIN.
RMETL: or RTHRM
(WETOX or CHOXO) Ib
CARBN; or INCIN.
NA
NA
».
(WETOX or CHOXD) Ib
CARBN; or INCIN.
(WETOX or CHOXD) Ib
CARDN: or INCIN.
CHOXD; CURED; or
INCIN.
(WETOX or CHOXO) III
CARDN; or INCIN.
CHOXD: CHRED:
CARON; BIODG: or
INCIN.
(WETOX or CHOXD) Ib
CARBN; or INCIN.
CARBN: or INCIN
CHOXD: CHREO:
CARBN: BIODG: or
INCIN.
NA
NA
Nonwaslewalers
INCIN.
FSUDS; CHOXD;
CHRED; or INCIN.
INCIN.
INCIN.
INCIN.
INCIN.
ADGAS.
ADGAS.
FSUBS; CHOXD;
CHRED; 01 INCIN.
INCIN.
INCIN.
FSUBS: or INCIN.
RMETL: or RTHRM.
FSUBS: or INCIN.
RMERC.
IMERC: 01 RM6RC.
INCIN.
INCIN.
CHOXD: CHIICD; or
INCIN.
FSUOS: or INCIN.
FSUBS. CHOXD:
CHRED; or INCIN.
INCIN.
FSUBS; or INCIN.
FSUBS. CHOXD:
CHRED; or INCIN.
RTHRM; or STABL.
HTHRM; or STABL.
-------
1.42 40 CFR Ch. I (7-1-92 Edition)
>8.42 TABLE 2.—TECHNOLOGY-BASED STANDARDS BY RCRA WASTE CODE—Continued
I
/.
S*« Alto
NA
NA
TabtoCCWIn
266.43.
TabtaCCWIn
266.43.
NA
NA
TabUCCWIn
206.43.
NA
NA
NA
NA
NA
NA . .
NA
NA
NA
NA
NA
NA
NA
NA
Tab* CCW In
266.43.
NA
Tabte CCW In
268.43.
NA
NA
NA
NA
NA
TabtoCCWln
266.43.
NA »
Wailo do»criptJon»
and/or treatment
•ubcalegory
Thlot«mic«/t*2iO«
ThricMoromoUiarwlhlol....
Ammonium vanadJie
Vanadium ptntoxkfe
Zinc PhotpWd*
«tO%). '
Ac«tak)«ftyd«
Aofltyl CNorid*
Aoytemid*
Acrylic acid
Eternal chtorid*
Benzenoaulfonyl
chtorid*. -
Doruotrichkxkto
TnchkxoawtaW«hyd«
(CM«
Watlowaloft
(WETOX or CHOXO) Ib
CARBN; or INCIN.
(WETOX o> CHOXO) Ib
OHDN; or INCIN.
NA
NA
CHOXD: CHRED: or
INCIN.
(WETOX Of CHOXO) Ib
CAflUN; or INCIN.
NA
(WETOX or CHOXO) Ib
CAF1DN; or INCIN.
(WETOX or CHOXD) Ib
CARBN: or INCIN.
(WCIOX or CHOXD) rb
CARDN; or INCIN.
(WETOX or CHOXO) Ib
CARBN; or INCIN.
(WETOX or CHOXD) 111
CAFIUN; or INCIN.
(WETOX or CHOXD) Ib
CAF1UN; or INCIN.
(WETOX or CHOXD) Ib
CAIION; or INCIN.
(WETOX or CHOXD) Ib
CARDN; or INCIN.
(WcTOX or CHOXO) Ib
CARBN: or INCIN.
(WETOX or CHOXD) Ib
CARBN; or INCIN.
(WETOX or CHOXD) Ib
CAI1DN; or INCIN.
CHOXD; CHREO:
CARON; DIODG; or
INCIN.
(WinOX or CIIOXO) Ib
CARON; or INCIN.
(WETOX or CHOXD) Ib
CARBN; or INCIN.
(WETOX « CHOXD) Ib
CARQN; of INCIN.
(WETOX or CHOXD) ft)
CARBN; Of INCIN.
NA
(WETOX or CHOXO) Ib
CARBN; or INCIN.
(WETOX Of CHOXD) Ib
CARBN; or INCIN.
(WETOX or CHOXO) (b
CARBN; or INCIN.
(WETOX Of CHOXD) tb
CARBN; or INCIN.
(WETOX of CHOXD) Ib
CARBN: or INCIN.
(WETOX or CHOXD) Ib
CARON; or INCIN.
CARBN: or INCIN
NonwaslowalofB
INCIN.
INCIN.
STABL
STABL
CHOXD: CURED; or
INCIN.
INCIN.
INCIN.
INCIN.
INCIN.
FSUUS; or INCIN.
INCIN.
INCIN.
INCIN.
INCIN.
FSUDS; or INCIN.
INCIN.
INCIN.
INCIN.
FSUOS; CHOXD:
CHREO: or INCIN.
INCIN.
INCIN.
INCIN.
INCIN.
INCIN.
INCIN.
INCIN.
INCIN.
INCIN.
FSUBS; or INCIN.
FSUBS; or INCIN.
FSUBS; or INCIN.
FSUDS; or INCIN.
FSUBS; of INCIN.
Environmental Protection Agency
260.42 TABLE 2.—TECHNOLOGY-BASED
§ 268.42
STANDARDS BY RCRA WASTE CODE—Continued
Waslo
code
U009
U062
U064
U073
U074
U005
U006
U007
U009
UOflO
U09I
UO
-------
8.42 40 CFR Ch. I (7-1-92 Edition)
:68.42 TABLE 2.—TECHNOLOGY-BASED STANDARDS BY RCRA WASTE CODE—Coniinuod
to
&•• «ISO
NA
NA
NA . ...
NA
NA
206.43.
NA
NA
NA
NA I
NA
NA
Table CCWE
In 206.41
and Table
CCWin
266.43.
NA
NA
NA
NA
NA . .
NA
NA
NA
Table CCW n
266.43.
NA
NA
NA
NA
NA
NA
HA
NA
NA
Waaie doacripliont
and/w i/eatmonl
aubcateoory
Furfuftl
Glyod*W«oyd«
Hydrazkw
Hydrogen Sulfti*
Matoic anhydride
Maleic hydrutto
Melphalan
Subc a louory — g» o a ler
than or oqual to 260
mg/kg total Metcury).
Methane thiol
Moinanol
Molhyl ethyl kotono
pofoxkto.
N Molhyl N'-nttio N-
Nilrosoguanidino.
elhanolamlno.
N • NiU o to-N-e tltylui ea
N-NII/OBO-N-
meUtytuioUunt.
Paraktahydo
PtnUchlotoelhan*
1.3-Pwitedtone
Phoephoms aUlid«
CAS No. (or
haiardoui
conetitiMnu
1IO-OO-9
98-O1-I
765-34-4
70-30-4
302-O1-2
7664-39-3
7763-O6-4
303-34-4
108-31-6
123-33-1
109-77-3
140-62-3
7430-97-6
74-93-1
67-56-1
79-22-1
1338-23-4
70-25-7
66-O4-2
130-15-4
134-32-7
91-59-8
79-46-9
1 1 16-54-7
759-73-9
664-93-5
615-53-2
123-63-7
76-01-7
504-60-9
1314-60-3
T*chnolc
Waslrmalort
(WETOX gycode
Nonwaitowalort
FSUBS: Of INCIN.
FSUBS; or INCIN.
FSUBS: or INCIN.
INCIN.
FSUBS: CHOXD:
CHRED; or INCIN.
ADGAS Ib NEUTR' or
NEUTR.
CHOXD: CHRED: or
INCIN.
INCIN.
FSUDS; or INCIN.
INCIN.
INCIN
INCIN.
RMERC
INCIN.
FSUUS: or INCIN.
INCIN
FSUDS- CHOXD
CHRED; or INCIN.
INCIN
INCIN
FSUBS or INCIN
INCIN
INCIN
INCIN
INCIN
INCIN
INCIN
FSUDS' or INCIN
INCIN.
FSUDS; or INCIN.
CHOXD' CHRED' or
INCIN.
Environmental Protection Agency § 268.42
268.42 TADLE 2.—TECHNOLOGY-BASED STANDARDS BY RCRA WASTE CODE—Continued
Waslo
coda
U191
U193
UI94
U200
U201
U202
U206
U213
U214
U2I5
U2IO
U2I7
U2IO
U2I9
U221
U222
U223
U234
U236
U237
U23U
U240
U244
U246
U246
U24U
Soo also
NA
NA
NA
NA
NA
NA ...
NA
NA
NA
Tablo CCW in
26043.
Tablo CCW in
2130.43.
Tablo CCW in
2G0.43.
Tablo CCWin
2GIM3.
NA ..
NA
NA
NA
NA
NA
NA
NA
NA
NA.
NA.
NA
NA
NA
Waste descriptions
and/or Irontmont
subcologory
1.3-Propano sultono
p-Denioquinono
Slroploialocin
Totrahydroluran
Thallium (1) acotato
Thallium (1) caibonnto
Thallium (1) chloiida
o-Toluidino
hydrochlondo.
sym-Trmilrobonrono
2.4.
Dichlorophonoxyaco-
tic (salts and oslois).
Cyanogon biomido
Wailann (.3%) 01 loss
Zinc Phosphide
CAS No. lor
rogulalod
hntaidous
conslituonls
109-O6-8
1120-71-4
107-10-8
106-51-4
50-55-5
106-46-3
1 61-07-2
16683-66-4
109-99-9
563-68-8
6533-73-9
7/91-12-0
10102-45-1
62-55-5
62-56-6
25376-45-8
636-21-5
26471-62-5
99-35-4
72-57-1
66-75-1
51-79-6
•94-75-7
137-26-8
506-68-3
81-81-2
1314-84-7
Technology code
Wastewatora
(WETOX or CHOXD) Ib
CARON: or INCIN.
(WETOX or CHOXO) Ib
CARDN; or INCIN.
(WETOX or CHOXO) Ib
CARBN: or INCIN.
(WETOX or CHOXD) Ib
CARON; or INCIN.
(WETOX or CHOXD) Ib
CARBN: or INCIN.
(WETOX or CHOXO) Ib
CARDN: or INCIN.
(WETOX or CHOXO) Ib
CARDN; or INCIN.
(WETOX 01 CHOXD) Ib
CARBN; or INCIN.
(WETOX or CHOXD) Ib
CARBN: or INCIN.
NA ....
NA
NA
NA
(WETOX or CHOXD) Ib
CARON: or INCIN.
(WETOX or CHOXO) Ib
CARDN: or INCIN.
CARBN; or INCIN
(WETOX or CHOXO) Ib
CARBN; or INCIN.
CARBN' or INCIN
(WETOX or CHOXO) Ib
CARDN; or INCIN.
(WETOX or CHOXO) Ib
CARDN; or INCIN.
(WETOX or CHOXO) Ib
CARON: or INCIN.
(WETOX or CHOXO) Ib
CARDN: or INCIN.
(WETOX or CHOXO) Ib
• »CARON; or INCIN.
(WETOX Of CHOXD) Ib
CARBN: or INCIN.
CHOXD: WETOX; or
INCIN.
(WETOX or CHOXO) Ib
CARON: or INCIN.
CHOXO: CHREO: or
INCIN.
Nonwaslewatorft
INCIN.
INCIN.
INCIN.
FSUBS: Of INCIN.
INCIN.
FSUBS: or INCIN.
INCIN.
INCIN.
FSUBS: Of INCIN.
RTHRM; or STABL.
RTHRM; Of STABL.
RTHRM; or STABL.
RTHRM; or STADL.
INCIN.
INCIN.
FSUBS; or INCIN.
INCIN.
FSUBS: or INCIN.
INCIN.
INCIN.
INCIN.
INCIN.
INCIN.
INCIN.
CHOXO; WETOX: or
INCIN.
FSUBS: or INCIN.
CHOXD; CURED: Of
INCIN.
1 CAS Number givon (or potent compound only.
1 This wssio codo exists in gnsoous lorm and is nol caloyotiiod as waslewaler or nonwastowator forms.
Note: NA moons Nol Applicable).
-------
268.42
40 CFR Ch. I (7-1-92 Edition)
Environmental Protection Agency
(b) Any person may submit an appli-
cation to the Administrator demon-
strating that an alternative treatment
method can achieve a measure of per-
formance equivalent to that achieva-
ble by methods specified in para-
graphs (a), (c), and (d) of this section.
The applicant must submit informa-
tion demonstrating that his treatment
method Is in compliance with federal.
state, and local requirements and is
protective of human health and the
environment. On the basis of such In-
formation and any other available In-
formation, the Administrator may ap-
prove the use of the alternative treat-
ment method if he finds that the al-
ternative treatment method provides a
measure of performance equivalent to
that achieved by methods specified in
paragraphs (a), (c). and (d) of this sec-
tion. Any approval must be staled in
writing and may contain such provi-
sions and conditions as the Adminis-
trator deems appropriate. The person
to whom such approval Is Issued must
comply with all limitations contained
In such a determination.
(c) As an alternative to the other-
wise applicable subpart D treatment
standards, lab packs arc eligible for
land disposal provided the following
requirements arc met:
(1) The lab packs comply with the
applicable provisions of 40 CFR
204.310 and 40 CFR 2G0.31G;
(2) All hazardous wastes contained
in such lab packs are specified In ap-
pendix IV or appendix V to part 268;
§ 268.43
(3) The lab packs are Incinerated In
accordance with the requirements of
40 CFR part 264, subpart O or 40 CPR
part 265, subpart O; and
(4) Any incinerator residues from lab
packs containing D004. D005. D006.
D007. D008. D010, and D011 arc treat-
ed In compliance with the applicable
treatment standards specified for such
wastes in subpart D of this part.
(d) Radioactive hazardous mixed
wastes with treatment standards speci-
fied in Table 3 of this section are not
subject to any treatment standards
specified In § 268.41. § 208.43. or Table
2 of this section. Radioactive hazard-
ous mixed wastes not subject to treat-
ment standards In Table 3 of this sec-
tion remain subject to all applicable
treatment standards specified in
§ 268.41, § 268.43, and Table 2 of this
section.
(51 PR 40642. Nov. 7. 198G. as amended al 5'.
Ftt 25790. July 8. 1987; 55 I'll 22G92. June 1
1990; 50 PR 3884. Jan. 31. 1991; 57 PH 8089
Mar. 8. 1992]
S 2C8.43 Treatment stundurds cxprcHHcd ai
waste concentrations.
(a) Table CCW identifies the re
stricted wastes and the concentration.-
of their associated hazardous constitu-
ents which may not be exceeded bj
the waste or treatment residual (noi
an extract of such waste or residual
for the allowable land disposal of such
waste or residual. Compliance wit!
these concentrations Is required bascc
upon grab samples, unless otherwise
noted Jp the following Table CCW.
-------
Wait* code .
DC03 (Be4trtve
CyanidesSub- •
category baaed on
• »1.23
a.
5'
F008 _
F009
F010
F011
FOI2
F019
NA _
NA _
NA
NA _....
NA
NA
TaMe CCWE in 258.41..
Table CCWE in 268.41..
NA
Table CCWE m 268.41..
Table CCWE m 26841..
Table CCWE in 268.41..
Cyandes (Total)
Cyanides (Amenable)
Had ...
Nickel . . .
Cyanides (Total)
Cyanides (Amenable)
Lead
Cyanides (Total)
Cyanides (Amenable)
Cyaniees (Total)
Cyanides (Amenable)
C.iromium (Total)
Lead
Nickel
Cyanides (Total) _
Cyanides (Amenable)
Chromium (Total)
Lead
Nickel
Cyanides (Total)
Cyanides (Amenable)
Chromium (Total)
57-12-5
57-12-5
7440-47-32
7439-92-1
7440-02-0
57-12-5
57-12-5
7440-47-32
7439-92-1
744O-02-0
57-12-5
57-12-5
57-12-5
57-12-5
7440-47-32
7439-92-1
7440-02-0
57-12-5
57-12-5
7440-47-32
7439-92-1
7440-02-0
57-12-5
57-12-5
7440-47-32
1.9
0.1
0.32
0.04
0.44
1.9
0.1
0.32
0.04
0.44
1.9
0.1
1.9
0.1
0.32
0.04
0.44
1.9
0.1
0.32
0.04
0.44
1.2
0.86
0.32
590 I.
30
NA
NA
NA
590
30
NA
NA
NA
1.5
NA
110
9.1
NA
NA
NA
110
9.1
NA
NA
NA
590
30
o
en
a
3
to
0
CO
-------
I ABLE ^w.—owna
K>
WlStt G00O
oat
F025 {Uctrt Ends
Succatefoy).
CommarcJaJ chemiLaJ
narrn
Ml
NA _.. .
Sxalso
Table CCWE n 268 41
and Tab* 2 in
268.42 (Note: F024
organic »tandan3t
must be fraatad v\a
incineration (1NQN)).
NA
Regulatajd hazardous
constiujefll
2-CNoro-l ,3-butadMne ...
1.1-Oicnloroethane
1 ,2-DicWorootnane -
\ ,2'DicNcropropana
OV1.3-
OicMoropropene.
tranj-1.3-
Dtchloropropene.
pnmaiate.
Hexacfiioroamane —
Cnrornium (Total)
Nickal
Chloroform
U-Oicnlorosmane.-
l.'.-Dcntoroetflylene......
Wetnylana chlonoe
Carson letracnionde
1.1^-Trchloroemarw —
Trich(oro«thy*ef>e
Viryl chJorids
CAS number
tor rvo^aated
hazardous
coosttujent
126-W-8
107-O4-1
75-34-3
107-06-2
78-87-5
10061-01-5
10061-02-6
117-81-7
67-72-1
7440-47-32
7440-02-0
67-66-3
107-05-2
75-35-4
75-9-2
56-23-5
79-OO-5
79-01-6
75-01-4
Was*
_
0.28
0.28
0.014
0.014
o!oi4
0.014
0.014
0.036
0.036
0.35
0.47
0.046
0.21
0.025
0.069
0.057
O.OS4
0.054
0.27
Nratam
Note*
C)
C)
C)
.1')
(»)
C)
C)
(>)
C)
. .
(M
C)
C)
(>)
C)
C)
(•)
C)
Nonwasi
Concwttoboo
(mg/kfl)
0.28
0^8
0.014
0.014
0.014
0.014
0.014
1.8
1.8
NA
NA
6.2
6.2
6.2
31
6.2
6.2
5.6
33
mraters
Notes
(>)
C)
(1)
(1)
C)
C)
C)
C)
._
(M
C)
(!)
C)
C)
C)
C)
C)
o
n
•n
JO
n
•^
I
•lo
O
a
W25 (Seem Rners or
Aei and Dcs«anu
Sueuiegory).
F039..
NA
Table CCWE in 268.41 ..
•
Cnlorolorm
Metnylene chlorxae
Careen teuacniofide
l.1.2-Tricnioroeinane
Thcfiioroeinyfene
Vinyl cnlonde
Heiacniorobenzene
Heiacniorobuiadiene
Hewcnoroeinane
Aceione
Acenaphtnaiene
Acenaonuiene
Aceionttrile
Acetophenone
2-Acetytamino(luo
(•
('
('
('
('
('
(•
('
(!
('
('
('
('
('
('
('
('
['
.., I1
('
('
C)
6.2
31
6.2
6.2
5.6
33
37
28
30
150
3.4
4.0
NA
9.7
140
NA
84
0.066
NA
14
4.0
NA
0.92
0.92
0.92
0.92
0.92
1.8
1.8
0.066
0.066
0.066
0.066
36
8.2
3.4
3.4
1.5
8.2
15
15
15
(M r^l
1 ' 3
C) <
C) 0
3
o 3
a
C> ^
o £.
(') t»
o a
a
o r.
(') O
(M 3
\ i
n\ ^
I J ^
Cfi
MI a
«-i 2
^
C)
C)
_ _ „.
Ml
\ I
C)
C)
01
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C) ._.
C) ""
(') g
as
C) *
CJ
-------
268.43 TABLE CCW.—CONSTITUENT CONCENTRATIONS IN WASTES—Continued
Wait* code
name
Sm also
constiluent
•ther.
n-Butyl alcohol .....
Butyl benzyl pnmalaie....
2-«ec-Butyi-4.6-
oinrtropnenol.
Canon tetrachlonde —
Casbon disulMe -
Otordane
p-CNoroeniline
CNorooenzene
Chlorooenzilale
2-Cniorc-1.3-ouUd>er>e...
CntarodAfomometnane..
Cnioroetnane .....
bn(2-Cnkxoetnoiy)
methane.
bi»l2-Cnioroemyi) etner..
Chloroform
bis(2-Chloroisopropyl)
etner.
p-Cfitorc-rn-cresoi
Cnkvomethane (Metnyl
c.-.kxide).
2-Cnloronaphmaiene
2-Chlorophenol
3-CWoropropyl«ne
Qvysene
c-Cresol
Creioi (m- and p-
bcmers).
Cyclohexanone
l.2-Dibromo-3-
ehkxopropane.
1.2-Dibromoetnane
(Etnylene dibromide).
Dibromomemane
2.4-
Oc.ikxophenory-
acetic aod (2. 4.0).
o.o'-OOO _
p.3''CDO z
CAS number
hazardous
constituent
101-55-3
71-36-3
85-68-7
88-85-7
56-23-5
75-15-0
57-74-9
106-47-8
108-90-7
510-15-6
126-99-8
124-48-1
75-00-3
111-91-1
111-44-4
67-66-3
39638-32-9
59-50-7
74-87-3
91-8-7
95-57-6
107-05-1
218-01-9
95-48-7
1 06-94- 1
66-12-8
106-93-4
74-95-3
94-75-7
53-19-0
72-54-8
Wane
Concentration
- (mg/l)
0 055
5.6
0.017
0.066
0.057
0.014
0.0033
0.4«
0.057
0.10
0.057
0.057
0.27
0.036
0.033
0.046
0.055
0.018
0.19
0.055
0.044
0.036
0.059
0.11
0.77
0.36
0.11
0.028
0.11
0.72
0.023
0.023
waten
Notn
(*)
)
(>)
(i)
o
C)
(*)
(*>
/t\
(')
lt\
<•>
(«)
(•>
(')
/It
(')
(*)
C)
(*)
C)
C)
(>)
(I)
" (')
FlOl'MU
ConoBi IL a Uon
(mg/kg)
2.6
7.8
2-5
5.6
NA
0.13
18
5.7
NA
NA
15
6.0
12
72
5.6
72
14
33
5.6
5.7
28
8.2
5.6
3.2
NA
15
15
15
10
0.087
0.087
Lowmten
Mom
(l\
1
C)
(1)
C)
(i)
(i)
(>)
C)
C)
(>)
C)
C)
(M
(I)
(M
' 1
(t)
C)
(')
(M
(M
* i
(')
(>)
(>)
(')
C)
C)
(O
u
JO
n
op'. ODE
p B'-DDE
0 3'. DOT
p p'.QOT
Oberj(a.n) antmacene..
Dibcnzo(a.e) pyrenc ......
m-Dicmoroberzene
c-Dic.-.iorobeniene.....
c-D>chlorooen2ene
Dicrilorodilluorometh-
ane.
1.1-Dichloroe tnane
1.2-DiChloroetnane
1.1-Oicnioroemylene
trans- 1.2-
Dichloroetnylene.
2.4-Ocniorophenol
2.6-Dichlorophenoi
1 7-OchloroproBane
os-1.3-
DKhloropropene.
trar.s-1.3-
dcnioropropene.
Oieidrin
Dieihyl phtnalate.-
2.4- Dimethyl phenol
Dimethyl phthalate
Di-rvbutyl phtnalate
1.4-Diniuobenzene
4.6-DinJtrc-c-cresol
2.4-Omiuophenol
2.4*Dinitrotoluene
2.6-Diniuotoluene
Di-n-octyl phtnalate
Di-n-propylniuosoamine .
Dtphenylamine
i^-Diphenyl hydrazine...
Diphenyl rtuosamine._..
i. 4-Oioxane
Disulloton
Enoosullan 1
Enoosullan 11 — _..
Enoosullan sullate
Endrin aldehyde...
Etryl acetate „...
Ethyl cyanide
Ethyl benzene
ethvi etner
3424-62-6
72-55-9
789-02-6
50-J9-3
53-70-3
192-65-4
541-73-1
95-50-1
106-46-7
75-71-8
75-34-3
107-06-2
75-35-<
120-83-2
87-65-0
78-87-5
10061-01-5
10061-02-6
60-57-1
84-66-2
105-67-9
131-11-3
84-74-2
100-25-4
534-52-1
51-28-5
121-14-2
606-20-2
117-84-0
621-64-7
122-39-4
122-66-7
621-64-7
123-91-1
298-04-4
939-98-8
33213-6-5
1031-07-8
72-20-8
7421-93-4
141-78-6
107-12-0
100-41-4
0.031
O.C31
0.0039
0.0039
0.055
0.061
0.036
0.088
0.090
0.23
0.059
0.21
0.025
0.054
0.044
0.044
0.85
0.036
0.036
0.017
0.20
0.036
0.047
0.057
0.32
0.28
0.12
0.32
O.S5
0.017
0.40
O.S2
0.067
0.40
0.12
0.017
0.023
0.029
0.029
0.0028
0.025
0.34
0.24
0.057
0.12
C)
(])
C)
\ .,.
C)
ft\
C)
C)
C)
C)
(')
(>)
(>)
(*)
C)
C)
(»)
C)
C)
(*)
C)
(•}
*)
I*
c
{«
[•
{•
(I
I*
(«
(«
(•
(•
(«
(1
(1
(1
>)
l\
,.
1)
>)
11
')
0.087
0.087
0.087
0.087
8.2
NA
6.2
6.2
6.2
7.2
7.2
7.2
33
33
14
14
18
18
18
0.13
28
14
28
28
2.3
160
160
140
28
28
14
NA
NA
NA
170
6.2
0.066
0.13
0.13
0.13
0.13
33
360
6.0
160
o 5*
C) <
* ' ^
C) ~
'. 1
3
o 2
O o
ci —
C) T>
o
o r
o S
i1' ?
C) §
C) ^
(') *
C) 3
C) "
C)
\\
\
')
')
')
>)
')
>)
')
1)
l)
')
— ,-
')
1
c
c
c
(1
«»
IJ g»
') OB
>) ^
') W
-------
268.43 TABLE CCW.—CONSTITUENT CONCENTRATIONS IN WASTES—Continued
Waste code
name
Soeabo
conswueni
twtf-Ethylheiyl)
phmaiate.
EtTtyl meitacrytete -
Efftytene oxide
Famphur
Fluoranmeno
Fluorene..
Fkjorotnchkxomethane ..
Heptachlof
Heptachior epox«oo
Hexacfttorobeniene.-
K0iacMorooutjid*ofX)
Hei acftlor ocyctopenia-
diene.
turans.
dionns.
H«x*?cnioroethan«
Hexacftioroproperw
lnoenoO.2.3-
tdlpyrene.
Metnacrylonitrile ..._
Me:ranol
Meuiorychlor _...
3-Meihylcnolanihrene....
M-Methyfene-bis.(2-
chloroaniline).
Me:nytenc chlonde
Meinyl ethyl ketone
Metnyl isotwryl ketorw ..
Meirtyl memacrylate
metnansulfonate.
Metr.yi pa/athion _...
Naontnaiene
CAS number
hazardous
consttuent
117-81-7
97-63-2
75-21-8
52-85-7
206-44-0
86-73-7
75-69-4
76-U-8
1024-57-3
118-74-1
87-68-3
77-47-4
67-72-1
1888-71-7
193-39-5
74-88-4
78-83-1
465-73-6
120-56-1
143-50-6
126-98-7
67-56-1
91-80-5
72-43-5
56-49-5
101-14-4
75-09-2
78-93-3
1CS-10-I
80-62-6
66-27-3
238-00-0
91-20-3
Wasle-
Concantratcn
-<9/n
0-28
0.14
0.12
0.017
0.068
0.059
. 0.020
0.0012
0.016
0.055
0.055
0.057
0000063
0000063
0.055
0.035
0.0055
0.19
5.6
0.021
0.061
0.00 11
0.24
5.6
0.081
0.25
0.0055
0.50
0.069
0-28
0.14
0.14
0018
0.014
0.059
tfllen
Notn
0
0
(')
(')
•(«)
(•)
(')
(')
(')
(')
0
C)
(')
(')
C)
(')
0
(')
•)
•)
')
')
')
')
')
')
C
('
(•
('
<'
('
('
['
(•
tJQlfKtt
Conovntribon
(mg/kg)
28
160
NA
15
8.2
4.0
33
0.066
0.066
37
28
3.6
0001
0001
28
28
8.2
65
170
0.066
2.6
0.13
64
NA
1.5
0.18
15
35
33
36
33
160
NA
4.6
3.1
mratan
Notes
C)
C)
')
')
')
')
')
')
')
')
')
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
')
C)
C)
C)
C)
C)
')
W7>
M
CO
t
o
n
~n
JO
n
m
e.
3
2-Naoritftylaniine
p-NitfOaniline
NrtroMnzene
5-Nitro-o-toluidine
4-Nitropnenoi •
N-Niuosodiethytamine ....
N-
Nitrosodimemyia-
mine.
N-Nitioso-*-tv
butylamine.
N-Noosometnyl-
einylamine.
N-Ni'jc&omofphoiine
N-Niaosopipendine
N-Nitrosopyrrolidine
ParaUuon
PenucMoroberuene —
Penucriiorodiberuo-
furans.
Pemachlofodibenzo-p-
dioiins.
PenlachloronitrcDerv
zene.
PeniacMorophenol
PrvenaCBlin
Ptwnanthrene
Pnenoi .....
Pmnalic anhydride
Pronamide. — .
pyTeno
Pyridine
Safroie
Save. (2.4.S-TP)...
24.5-T
1^.4.5.-
Teuachlorobenzene.
Tetracrilofodibonzo-
turans.
Teuachiorodibenz>p-
dioxtns.
1.1.1.2-
Tetrachlofoethane.
1.1.2.2-
TetracMoroeinane.
Tetrachloroethyiene
2.3.4.6-
TetrachKxopfienol.
Toluene
91-59-8
100-01-6
98-95-3
99-55-6
100-02-7
55-18-5
62-75-9
924-16-3
105SS-95-6
59-89-2
100-75-4
930-55-2
56-38-2
608-93-5
„...
82-68-8
87-66-5
62-44-2
85-01-8
108-95-2
298-02-2
85-H-9
23950-56-5
129-00-0
110-86-1
94-59-7
93-72-1
93-76-5
95-94-3
630-20-6
79-34-6
127-18-4
58-90-2
108-88-3
0.52
0.029
0.068
0.32
0.12
0.40
0.40
0.40
0.40
0.40
0.013
0.013
0.014
0.055
0.000063
0.000063
0.055
0.089
0.081
0.059
0.039
0.021
0.069
0.093
0.067
0.014
0.081
0.72
0.72
0.055
0.000063
0.000063
0.057
0.057
0.056
0.030
0.080
C)
C)
I1)
C)
C)
(=)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C
{')
(')
C
C
(•
(•
C
II
C
ft
C)
I'll
C)
C)
1=)
C)
t1)
(*!
C)
NA !
29 |
14
28
29
28
NA
17
2.3
2.3
35
35
4.6
37
0.001
0.001
4.8
7.4
16
3.1
6.2
4.6
NA
1.5
8.2
16
22
7.9
7.9
19
0.001
0.001
42
42
5.6
37
28
1')
C)
01
C)
I1)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
03
a
3
CO3
KJ
C*
CO
i>.
w
-------
268.43 TABLE CCW.—CONSTITUENT CONCENTRATIONS IN WASTES—Continued
Waste code
K001
K002
Commercial cnenScal
name
NA
NA...._ - . ._
SM the
Title CCWE in 266.41.
Table CCWE « 268.41..
Regulated hazardous
MjiuLIUenl
Toxapnene
1 ,2.4-Tncfwrobeiuene..
1.1.1-Trichtoroeihane
1 .1 .2-Triehioroemane ....
TricMoroetnylene
2.4.S-Tnchlorophenol_..
2.4.6-Tricnlorophenol_._
1 .2.3-Trienloropnjpane ..
1.i.2.Trichloro-1.2.2-
bifluoro-ethane.
Tns(2.3-d>t>romoprDpyl)
pnosphati.
Vinyl chloride
Xytano(s)
Fluoride
Sulfide
Antimony
Binum ... .
Chromium (Total)
Copper _.
Lnc.._ _
NCMI ...
Selenium
Sirver _
Thallium
Zinc
Pentacntoropnonol
Fy.ru _..
Toluene
Xylenes (Total)
Lead
Chromium (Total)
Luc
CAS number
lor regulated
hazardous
constituent
6001-35-1
120-82-1
71-55-6
78-00-5
7»-01-6
SS-95-1
88-06-2
B6-1S-I
76-13-1
126-72-7
7S-01-4
57-12-5
16964-48-8
6496-25-8
7440-36-0
7440-38-2
7440-39-3
7440-41-7
7440-43-9
7440-47-32
74X0-50-8
7439-92-1
7439.97-6
7440-02-0
7782-49-2
7440-22-4
7440-28-0
7440-62-2
7440-66-6
91-20-3
87-86-5
85-01-8
12S-OO-0
108-88-3
7439-92-1
7440-47-32
7439-92-:
Waalewaterj
ConceiTtration
•(mg/O
0.0095
0.055
0.054
0.054
0.054
0.18
0.035
0.85
0.057
0.11
0.27
0.32
1.2
35
14
1.9
1.4
1.2
0.82
0.20
0.37
1.3
0.28
0.15
0.55
0.82
0.29
1.4
0.042
1.0
0.031
0.16
0.031
0.02S
0.02B
0.032
0.037
0.9
3.4
Notes
:
Nonwastewaters
Concentration
(mg/kg)
1.3
19
5.6
5.6
5.6
37
37
. 28
28
NA
33
28
1.8
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
1.5
7.4
1.5
1.5
28
33
NA
NA
NA
Notn
C)
')
')
')
')
')
C)
C)
C)
C)
C)
I'.'
-
C)
C)
C)
CI
C)
CI
... .
CO3
0>
to
'*.
ft
-n
jo
ft
o
3
K005
K006
KOCft
K009 ,
K010
K013 — ._— - —..
K01 * „- ._._.-..
NA
NA
NA
NA __ _ _.,
NA _
NA
NA
NA _
NA
NA „...
NA ...
f^A _..
NA -.
Table CCWE m 2S3.*i ..
Taol«CCWEin2Sa-4i..
Table CCWE in 268.41..
TaWt CCWE in 268.4 U
Table CCWE in 268.4 1_
Table CCWE in 268.41 ..
NA
NA
NA
NA
f
•
Table CCWE in 268.41.
NA
Ovomium (Total) '
Civonium (Total)
Lead
^vomiuni (Total) —
Cyanides ffoial)
Cri/omium (Total)
__«>j{]
Chromium (Total) _...
Lead.-
Cyanides fTotal) — —
Chromium fTotal)
L*ad.- - ~
Chloroform
Chloroform _. .......... ._......
Aceionitnle
Acrylonitnle _..-
Ac.*ylamide _ -»
Cyanide (Total)......
Acetonitnle -
Aoytonitrile
Acryiamide
Benzene
Cyanide (Total)
Acetonrtrile
Acrytonjtrile — -
Benz e n 0 . ........... _«.__. -
Cyanide (Total)
Antnracene .
Berual Cnloride
Sum ol Benzo(b)
fluoranlnene
and Beruo(k)
fluoiantnene.
Pnenanthrene
Toluene
Chromium (Total)
Nickel
Heiacnlorobenzene
Hexachlorobutadiene. —
Hexachlonxyelocenta-
diene.
HexacMoroethane
Tetracfiloroetnene
1 i-OicNoropropan*
1 J.3-Tncnhxo(xopane ._
7439-92-1
7440-<7-32
7439-92-1
7440-47-32
7439-92-1
7439-92-1
67-66-3
107-13-1
79-06-1
71-43-2
75-05-8
107-13-1
79-06-1
71-43-2
S7-12-5
75-05-fl
107-13-1
79-06-1
71-43-2
57-12-5
120-12-7
98-87-3
207-08-9
es-oi-e
108-68-3
116-74-1
87-68-3
77-47-4
67-72-1
127-18-4
78-87-5
96-18-4
0 9
3 4
0 9
3.4
0.9
0.9
3.4
3.4
0.1
0 1
38
006
19
0.02
38
0.06
19
0.02
21
38
0.06
19
0.02
21
1.0
0.28
0.29
0.27
0.15
0 32
0.033
0.007
0.007
0.033
0.007
0.85
0.85
C)
(*)
(t)
C)
C)
3.4
(')
(')
lt\
(')
...«. 1 _»..
"
1')
C)
C)
C)
C)
ri
(M
NA
NA
NA
NA
NA
NA
(•)
C)
C) '
NA
NA
(«)
NA
NA
6.0
6.0
1.8
1.4
23
0.03
57
1.8
1.4
23
0.03
57
1.8
1.4
23
0.03
57
3.4
6.2
3.4
3.4
6.0
NA
NA
28
5.6
5.6
28
60
18
23
t ^
<§
NA
NA
(,,
I1)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
m
O
3
3
a
£
^
o
B
n
5'
to
e
3
n
«^
UK
M
O>
pa
t**
-------
268.43 TABLE CCW.—CONSirruENT CONCENTRATIONS IN WASTES—Continued
Wast* cod*
^01B
ltrit$
K050 __
K021 _.
Cut 1 • l'l*l L4J LTmUdJ
mm*
MA
NA
NA
MA
S*at)K>
MA
MA
NA.
Table CCWE in 268 41 .,
oonslim*fTt
Chlorometrttn*
1.1-OicttorDethartt
1 j-Oichloroetnane
HexAcfttorobuUdierM —
HeucNoroetnane
PmuchkxoeBwte
1,1.1-Trichterecthane^.
B«t(2-cMorD6ttiy>}ether
CfatorobonzonG .._—.._...
CNofOfOfm _..
U-OcrtofO«thane
RufXfKMt
HflxacWoroethane
NwftmaJerw
Phenan throne
1.245-
ToVBCftlOTOC4K12ene.
T«7acnioroetfiene
1 .2.4-Trichloroe«njene._
1.1.1 -Trichtoroethane
1 ,2-Dchloroetrtane
1.1.2.2-
T«trachloro*tnane.
Tetracftkxoemene
Chloroform
Carbon totracrJonde
CAS numoer
hazardous
constituent
75-00-3
74-87-3
75-34-3
107-06-2
87-64-3
67-72-1
76-01-7
71-55-6
111 44 .4
106-90-7
67-66-3
106-46-7
107-06-2
66-73-7
67-72-1
S1-20-3
as-ot-8
&5-W-3
127-16-4
120-82-1
71-55-6
107-06-2
79-J4-6
127-18-«
67-66-3
56-23-5
7*iO-36-0
Wu)«
Concontrtbon
- (ms/I)
0.007
0.007
0.007
0.007
0.007
NA
0.007
0.007
0.007
0.006
0.007
0.008
0.007
0.007
0.033
0.007
0.007
0.017
0.007
0.023
0.007
0.007
0.007
0.007
0.0^6
0.057
0.60
nun
Nona
(')
(')
(')
I1)
(')
('
('
(i
('
('
(>
('
('
0
('
('
C
('
('
('
('
(')
(')
(')
C)
(')
Nonwu.
Concentration
(mg/kg)
60
NA
6.0
e.o
5.6
28
5.6
6.0
56
6.0
6.0
NA
6.0
NA
28
5.6
5.6
NA
6.0
19
6.0
6.0
5.6
6.0
6.2
6.2
NA
owaten
Noun
(')
(')
(')
(')
(i)
(')
(')
(')
(')
I1)
(')
(')
(')
(')
(')
(')
(')
(i
('
('
C
('
(')
KJ
0>
pa
CJ
O
n
-n
10
.,.
s
(')
-•-••
0.034
19
NA
NA
13
12
NA
NA
28
26
60
6.0
5.6
28
5.6
5.6
5.6
6.0
6.0
6.0
NA
NA
NA
NA
60
60
6.0
6.0
6.0
NA
NA
5.6
28
19
26
5.6
14
Environmental Pro
M
9
TM n
0
(') ^
a
a
'•I s
o
.,.
i-i
S «
(') 5.
(') 00
-------
s
o
Wuucrte
K031
K032 —
K033
K034
K035
K036
K037
K038
K040
K041
K042
K043
Commercial chxncaa
nanx
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
Se« also
Table CCWE in 268.41..
NA
NA
NA .
NA
NA
NA
NA
NA
NA
NA
NA _
R*gulatad haianXxt
constrtxwfil
Ti
1 .2.4.Trichtorob«m«na...
ATM CMC
HaucMoropentAdene ...
CNortano
Heptachkx _
H«puchky «poxid«
HQxacMoroqrdopenta-
dw;ne.
He xa cMorocyctope nia-
dien«.
Acufi &ph thfl rtfi
A^itnrBccrvo
Benz(a)aniftracene
Bcn20(a)pvr*ne
ChrysonQ
Dtbenz(a.h)anmra-cena ..
Fluor anmene
Ruofonc
lno«no( 1 .2.3-cd)pyrene ..
Cresols (m- and p-
isomers).
Naphthalene
O-CfCSOl
Phenanthrerw
Pftenol
Pyrer>6
DisuKolon
Disultoion
Toluene
Phoraie
Phoraie
T^aph*>n«»
U.4.5-
Tetracnlorobenzene.
o-Oicnlorobenzene
p-D*chioroben2ene
Pentachlwobenzena...-.
1 .2.4-Tnehlorobenzene..
2.4-DichHxopherxji
2.6-Dichl(x cphenol .._
2.4.5-Tnc.ilorophonol.....
CASnumb«r
to> regulated
hazanlou)
consbtuenl
127-18-«
120-82-1
7440-38-2
77-47-«
57-74-9
76-44-«
1024-57-3
77-47-4
77-47-4
83-32-9
120-12-7
56-55-3
50-32-8
218-01-9
53-70-3
206-44-0
8S-73-7
193-39-5
91-20-3
95-48-7
85-01-8
108-95-2
129-00-0
298-04-4
298-04-4
1C8-88-3
298-02-2
298-02-2
8001-35-1
95-94-3
95-50-1
106-46-7
608-93-5
120-S2-1
120-83-2
87-65-0
95-95-4
Wanevaiera
Concentration
(mg/l)
0.007
0.023
0.79
0.057
0.0033
0.0012
0.016
0.057
0.057
NA
NA
0.059
NA
0.059
NA
0.068
NA
NA
0.77
0.059
0.11
0.059
0.039
0.067
0.025
0.025
0.080
0.025
0.025
0.0095
0.055
0.088
0.090
0.055
0.055
0.049
0.013
0.016
Note*
(')
(')
C)
0
(')
. 0
(')
(')
CI
(')
(')
(')
(')
(')
(')
('
('
('
('
('
('
('
(•
('
('
(•
('
(')
(')
(')
Nonwaitewaterj
Concarmabon
(mg/kj)
8.0
18
NA
2.4
0.2C
0.066
0.066
2.4
2.4
3.4
3.4
3.4
3.4
3.4
3.4
3.4
3.4
3.4
NA
3.4
NA
3.4
NA
8-2
0.1
0.1
28
0.1
0.1
2.6
4 4
4.4
4.4
4.4
4.4
0.38
0.34
8.2
Note*
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
'I
'1
:;
:;
')
')
')
')
')
CD
U
o
r>
r>
m
O.
o
3
K046..
K048..
X
s5
-3
NA..
NA..
Table CCWE in 268 41 ..
Table CCWE in 268.41..
*
2.4.6-Trichkxopnenol-....
TetrachiorDpno* no(3
fTotal).
Pentaehlorophenol
Tetrachkxoemene ._
Hexachlorodibenzo-p-
dtoxins.
Hexachlorodibenzo-
furans.
PentachlofOdibenzo*p-
daxins.
Pe.-vlachlorodibenzo-
turans.
TetracfitorodJOenzo-p-
dioxins.
Tetrachiorodibenzo-
turans.
Lead
Benzene
Benzolatpyrene
Bis(2-etny1heryl)
pntnalate.
Chrysene..- — ......
O-rvbutyl pnmalate
Etnyibenzene
Fluorene
Naphthalene
Phenantnrene
PHeool
Pyrene .„ »
Toluene - „
Xylene(s)
Cyanides (Total)
Chtomiun (Total)
Lead
88-06-2
87-ee-s
79-01-6
7439-92-1
71-43-2
50-32-8
117-81-7
218-01-9
84-74-2
100-41-4
86-73-7
91-2O-3
85-01-8
108-95-2
1 29-00 -O
108-88-3
57-1 2-S
7440-47-32
7439-92-1
0.039
0.018
0.022
0.006
0.001
0.001
0.001
0.001
0.001
0.001
0.037
0.011
0.047
0.043
0.043
0.06
0.011
0.005
0.033
0.039
0.047
0.045
0.011
0.011
0.028
0.2
0.037
7.8
0.68
1.9
1.7
0.001
) 0.001
0.001
) 0.001
) 0.001
) 0.001
NA
) . 1«
) 12
7.3
) 15
) 3.6
) 14
NA
42
34
3.6
36
14
32
1.8
NA
NA
(') F
0 <
(') §
(') 1
o g
a
(') £
o ?
e
o y
r.
o |
(1) >
CD
(') 3
(') x
(') ^
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
O>
CD
-------
Wuiecode
KO-*9
KBSO
ConvnercaJ chentcftl
name
"» ,
NA
See irto
TaWeCCWE in 268.41.
TaflleCCWE in 268.41.
Regulated hazardous
conatrluont
Antrvafwne
Benzene
Benjofalpyrene....:;
Bo<2-etnyineiyt)
phtfulate.
Ca/fton disutfide ............
Qvywne
Ethytbeniene
Nagntttalene
Pnenantrvene
Pnenol - -
Prrene..- -
ToJ^ene
Xytene(s)
Cyanides (Total)
Chromium (Total) —
BerccXalPyrene —
Phenol -
Cyanides (Totall
Chromium (Total)
1 *»4
CAS number
lot regulated
hazaroous
constituent
120-12-7
71-43-2
50-32-8
117-81-7
75-15-0
2218-01-9
105-67-9
100-41-4
91-20-3
85-01-8
108-95-2
129-00-0
108-88-3
57-12-5
7440-47-32
7439-82-1
50-32-8
108-95-2
57-12-5
7440-47-32
7434-33-1
Wutmrltara
Conc0i IU Ebon
(mg/l)
0.039
0.011
0.047
0.043
0.011
0.043
0.033
0.011
0.033
0.039
0.047
0.045
0.011
0.011
0.028
0.2
0.037
0.047
0.047
0.028
0.2
0.037
Notes
(')
(')
(')
(')
(')
• (')
(')
(')
(')
I1)
I1)
(')
(')
(')
(')
....
(M
(')
(')
Nonwaxtewaien
Concentration
(mg/kg)
28
14
12
7.3
NA
15
NA
14
42
34
3.6
36
14
22
1.8
NA
NA
12
3.6
I.S
NA
NA
Notes
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
n
-n
jo
KOS2-
..J Taole CCWE in 253.41..
NA
Table COVE in 268.41
Table CCWE in 268.41,
Accnapriteno .___._.„
ArtiVBCono ,,..,..,....,..
8enzo(a»- anmraccne
Ben20(a)pyrene
Bis(2-cthyihe«yl)
pmnalate.
C.fcjy5aftc
Di-rvburyt phtnalaie
E^ylbenzene
Fluofence
Na?nu\alene.._ .
Pherwntn/cne —
Prenol . ..-
Pyrene _
Tciusne „ „.._..._..._..
Xyten«(sl ...-
Cyanides (Total) _
Lead
Benzone
8enzoU)Pyrene
o^/esol _.
2.4-Dimetnylpnenol
Etnyloenzeno
Naphthalene
Phenanihrene
Phenol
Cyanides CTolaQ
Cnromiuni (Total)
Benzene
Betuoialpyrene
Nacntnaiene
Phenol . .__
Cyanides (Total)
Cadnvum .....——.—._....
Chromium (Total)
Lead
Nickel
2C8-96-8
120-12-7
71-43-2
50-32-8
117-81-7
75-15-0
2218-31-09
105-67-9
100-41-4
86-73-7
91-20-3
85-01-8
108-95-2
129-OO-0
108-E8-3
57-12-5
7440-47-32
7439-92-1
71-43-2
50-32-8
95-48-7
106-44-5
105-67-9
100-41-4
91-20-3
85-01-8
108-95-2
108-88-3
57-12-5
7440-17-32
7439-92-1
71-43-2
50-32-8
91-20-3
108-95-2
57-12-5
7440-43-9
7440-47-32
7439-92-1
7440-02-0
0.05
0.039
0.011
0.043
0.047
0.043
0.043
0.06
0.011
O.OS
0.033
0.039
0.047
0.045
0.011
0.011
0.028
0.2
0.037
0.011
0.047
0.011
0.011
0.033
0.011
0.033
0.039
0.047
0.011
0.011
0.026
02
0.037
0.17
0.035
0.028
0.042
1.9
1.61
0.32
0.51
0.44
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
(')
<11
rl
<")
Cl
NA
28
14
20
12
7.3
15
3.6
14
NA
42
34
3.6
36
14
22
1.8
NA
NA
14
12
6.2
6.2
NA
14
42
34
3.6
14
22
1.8
NA
NA
0.071
3.6
3.4
3.4
1.2
NA
NA
NA
NA
m
(') <
(') — •
(') 0
3
CI ^
n °
—
£
(') -o
o **
PI a
fl
(') 5"
(') 3
(') >
c) to
/n 9
m 3
( i n
(M *<
(»)
(*)
')
')
i)
')
')
')
')
')
')
„..„_
C)
(')
C)
(')
— „
». .._ r- „.„, C*93
o»
CO
JU
-------
co
CO
o
Waste code
KOM
K069
K071
K073 _
K083
K084
K085 _
Commercial cfiernical
name
NA
NA
NA „
NA.
NA _._
NA _
NA
See also
Table CCWE h 268 41
Table CCWE ri 268 41
and Table 2 in
268.42.
Table CCWE In 268.41..
NA
Table CCWE «i 268 41
NA - _ _
NA _ _ .. ..
constituent
Nckut
Lead _
Mercury
Carbon tetrachloride.
Hezachloroetnane —
TetracMoroetnane
1 , 1 . 1 -TricMoroatnana ..':.
dpnenytamne
Dtpnenytnitrosamtne
Sum of Diphenytamne
and
Qphenytnitrosamine.
Nitrobenzene
Cydohexanona
Nickel
CMorOberUine
c-Ochlorobenzene
nvDtcftlorobenzene
p-DefMorobenzene
1 ^.4-Tnenlorooenzeoe._
1.2.4.5-
Tetrachloroberuene.
Pentachlorobenzene -
HenefUoroDenzene
Aroclor 1016
A/oclor 1221
Arcctor 1232....- -
A/odor 1242 -....
Arcctor 1248
CASrumoer
hazardous
7440-47-32
7439-92-1
7440-02-0
7440-43-9
7439-92-1
7438-97-6
56-23-5
67-66-3
67-72-1
127-1B-<
71-55-6
71-43-2
82-53-3
22-39-1
66-30-6
98-95-3
1C4-95-2
104-94-1
7440-02-0
744O-34-2
71-43-2
104-90-7
95-50-1
541-73-1
106-46-7
120-82-1
95-94-3
608-93-5
118-74-1
12674-11-2
11104-28-2
11141-16-5
53469-21-9
12672-2&-6
Waal*
Concentration
(mg/l)
0.32
0.04
0.44
1.8
0.51
0.030
0057
0.046
0.055
0.056
0.054
0 14
0.81
0.52
0.40
NA
0.068
0.039
0.36
0.47
0.79
0.14
0.057
0.088
0.036
0.090
0.055
0.055
0.055
0.055
0.013
0.014
0.013
0.017
0.013
ntan
Notas
:
C)
C)
o
C)
C)
C)
C)
C)
C)
C)
H
C)
C)
(1)
Normal
Concentration
NA
NA
NA
NA
NA
NA
62
6.2
30
6.2
6.2
NA
NA
14
14
56
NA
NA
NA
4 4
4.4
4.4
4.4
4.4
4.4
4.4
4.4
4.4
0.92
0.92
0.92
0 92
0.92
lewaters
Notas
C)
C)
C)
C)
Ml
C)
C)
(I)
(1)
C)
C)
C)
C)
C)
C)
u
>)
o
n
«*
•c
O
-.
KW7
NA
phihaU:e
Dxtnyl pntralaie
Dim«inyl pninjliie
Dt-tvbutyl pntnatate
Emyi ac*u:«
ElnylMrutn*
M«thylen« cwonae
Nipfitniieno
Nitrooen2tn«
Tokjtn*
1.1.1-Tnchl)
I1)
C)
C)
C)
C)
C)
C)
3.4
0071
3.4
3.4
3.4
3.4
3.4
0.65
0.07
NA
28
28
5.6
5.6
m
3
o
a
89
e
a
C47>
to
-------
Want code
K097
K099
Convrwrotl tfwnical
iwne
NA
NA .
NA
NA
NA
S*» also
NA
NA
NA - ..
NA
TtbtoCCWE in 266.41
NA
FUguiaiod hazirfoa
constituent
1.1.2-Trichionjetnane —
HexacNoroemane
Penuchioroeinane
t.i.1.2-
Tenchloro«tnane.
1.1Z2-
Tetracnloroemane.
Tetracnlof oethei M ..........
1 .1 ,2-Tricnloroethane —
Tricnloroetnene
Tncnkxoetnytene
1 ,3-Ocnlorrjo«n2ene
Pentacnloroetnane
1.2.4-TncMorobenzene..
Hexacrtlorocyctop«nu-
o>ene.
^JOrdATkQ ..._...«_.___._
HepucWof
Hfloiactikx apoxioe
Tc^^ofwo* — — •
2.*-
Dichtoroprwnoxyac*-
be aod.
HaxachkxobOenzo-p-
Ooivu.
H« ucNorodiboniofur-
tns.
PerMcWofObenzahr-
ins.
C^drrwT1
r^vnmin iTatfth
Lo«i
0-Nrtroarv!ina
Aj>*Ytrvc
CAS number
htZ4Vdom
COnvtituont
127-18-<
7S-00-5
7»-OI-6
67-72-1
76-01-7
£30-20-6
7»-34-6
127-18-4
7«-00-5
79-01-6
79-01-6
541-73-1
76-01-7
12O-42-1
77-47-4
57-74-9
76-44-8
1024-57-3
8001-35-1
94-75-7
7440-43-9
7439-32-1
7440-38-2
Wutcwatera
Cortowntr ebon
(mg/I)
0.056
0.054
0.054
0.055
0.055
0.057
0.057
0.056
0.054
0.054
0.054
0.036
0.055
0.055
0.057
0.0033
0.0012
0.016
0.0095
1.0
0.001
0.001
0.001
0.00 1
0.001
0.001
1.6
0.32
0.51
0.27
1 0.79
Not**
C)
C)
0
o
C)
C)
C)
C)
C)
C)
C)
C)
._
Nonwutewiiara
Concentration
(mo/kg)
6.0
6.0
5.6
28
5.6
5.6
5.6
6.0
6.0
5.6
5.6
5.6
5.6
19
2.4
0.26
0.066
0.066
2.6
1.0
0.001
0.001
0.001
0.001
0.001
0.001
NA
NA
NA
14
NA
Nous
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C
C
C
C
C
C
i:
C)
C)
C)
C)
C)
C)
1
1 " «•)
po
CJ
.C.
o
O
•n
O
•o
K)
m
o"
3
K102
-.
K1Q4
Kf05
K10$
P010
ann
PO1?
P0?4
PO*WI
on-iT
NA
NA
NA..
NA
KJA
NA
AVfnq
Arsenic ic"d
ArwjniG rj^n*c*^fl
A/seruc tnoxjde
Banum cyan^e
2.aoc.8uTyi-4 6-
dnitrocnenol
(Dinoseb).
Carbon douMSde
p-C*ICrpirtlin«
Cooper cyanide
Cyanides (soluble salts
and complies.
Dicnlorophenytarsine. •
nuiAifi
TaWe CCWE in 268.41.
NA
NA
NA
Table CCWE in 268.41
and Table 2 in
268.42.,
Table CQVE «i 268 41 ..
NA
Table CCWE in 268.41 .
Table CCWE in 268.41 .
Table CCWE in 268.41 ..
Table CCWE in 268.41 ..
MA
NA
Table 2 in 268.42
NA
Nf
NA
Table CCWE in 268.41.
NA
Cadmium
Lead
Mercury
Ar^n^
Cadmium
Lead
Mercury
Aniline
&en26rte
2.4-Dmitroonenol
Pnenoi
Aniline -,
Benzene —
2.4-Oinitrophenol
Nitrobenzene
Prtenol
Cyanides (Total)
p^nlfln^
Cnlorobenzene
o-D«chlorobenzene
p-r>cnlorobenzena
2.4.5-Tncnioropnenol —
2.4.6-Tnchloropnenol....
2-Cnlorophenol
Phenol
Mercury.
N>chlH
AJdnn ._
A/wnic
A/senic
Ar^nlc , ...
Cyanides (Total) —
Cyanides (Amenable) —
2-sec-Butyf-4.6-
dinitrophenol
(Dinoseb).
Cyanrrj45 (Tot^rj
Cyanides (Amenable) —
Carbon disuifide —
pCnioroaniiine . ._
Cyanides (Total).. ._
Cyanides (Amenable)
Cyanides (Total) _
Cyanides (Amenable)..
Anenic
Oeidrin
7440-43-9
7439-92-1
7439-97-6
7440-38-2
7440-43-9
7439-92-1
7439-97-6
62-53-3
71-4 3-J
51-28-5
98-95-3
108-95-2
62-53-3
71-43-2
51-28-5
98-95-3
108-95-2
57-12-5
71-43-2
108-90-7
85-50-1
106-46-7
95-95-4
88-06-2
95-57-8
108-95-2
7439-97-6
7440-02-0
309-00-2
7440-38-2
7440-38-2
7440-38-2
57-12-5
57-12-5
88-85-7
57-12-5
57-12-5
75-15-0
106-47-8
57-12-5
57-12-5
57-12-5
57-12-5
7440-38-2
60-57-1
0-2*
0.17
0.082
0.028
0.79
0.24
0.17
0.062
4.5
0.15
0.61
0.073
1.4
4.5
0.15
O.S1
0.073
1.4
2.7
0.14
0.057
0.068
0.090
0.18
0.035
0.044
0.039
0.030
0.47
0.021
0.79
0.79
0.79
1.9
0.1
0.066
1.9
0.1
0.014
0.46
1.9
0.1
1.9
0.1
0.79
0.017
C)
I'l
NA
NA
NA
13
NA
NA
NA
NA
5.6
6.0
5.6
5.6
5.6
5.6
6.0
S.6
5.6
5.6
1.8
4.4
4.4
4.4
4.4
4.4
4.4
4.4
4.4
NA
NA
0.066
NA
NA
NA
110
9.1
2.5
110
9.1
NA
16
110
B.I
110
e.i
NA
0.13
C)
C)
C)
O
3
3
e
3
<0
•
3
A
0>
a
w
-------
268.43 TABLE CCW.—CONSTITUENT CONCENTRATIONS IN WASTES—Continued •
Waste code
POM
PQ39
PO47
P0*8
P050
PfKl
PQ56
P059
P060
P063
P071
P073
P074
P077
PM3
POM
P092 _.
P094
P097
P098
P099
PlQi
Pica . . T_.._
Commercial cherrucal
name
Dietriyiarsine
2.4-CXnmopnenol
Endnn .„
Mercury fulminate
Nickel caoonyi....- -
Nickel cyai£e
c-Niuoamiine
N-Nitrosoometn-
PhenytmefCLtry aceu:e ..
Phorale
Potassium ytvef
cyanide
Ettiyt cyanioe
(Ptooanenivil*).
Selenourea _
See also
Table CCWE in 268.41.
NA
NA
NA
NA
Table 2 in 268 42
NA
NA
NA . „_
Table CCWE in 268 41
and Table 2 in
268.42.
NA _ _..
Table CCWE in 25841..
Table CCA'E «i 26841..
NA
Table 2 in 268 42
NA . . _
Table CCWE in 265 41
and Table 2 in
268.42.
NA ......
NA
NA
Table CCWE in 26541.
NA
Table CCWE in 265.41.
Regulated hazardous
constituent
Arsenic -.._
Oisurloton
4.6"t>nitrc-o-ctesol
2.4.r>nitrophenol
Endo&uHan 1
Endosuttan II _
EndosuHan sullate
Endnn .......
Endnn akfchyd* -.....".
Fluonde _
Hep'jchkx
Heotacnior eoowde
lsod«s (Amenable) .-
Cyaruoes (Amenable)....
Silver
CAS number
for regulated
hazardous
constituent
7440-38-2
296-04-4
534-52-1
51-26-5
839-96-8
33213-6-5
1031-07-8.
72-20-8
7421-93-4
16964-46-8
76-*4-8
1024-57-3
465-73-6
57-12-5
57-12-5
7439-97-6
298-00-0
7440-02-0
57-12-5
57-12-5
7*40-02-0
100-01-6
62-75-9
56-38-2
7439-97-6
298-C2-2
52-8 S-7
57-12-5
57-12-5
57-12-5
57-12-5
7*40-22-4
Etnyi cyanide 1 107-12-0
(PropanennnLe).
Selenium J 7782-49- 2
Wastewaten
Concentration
(mg/l)
0.79
0.017
0.28
0.12
0.023
0.029
0.029
0.0028
0.025
35
0.0012
0.016
0.021
1.9
0.10
0.030
0.025
0.32
1.9
0.10
0.44
0.028
0.40
0.025
0.030
0.025
0.025
1.9
0.10
1.9
0.1
0.29
0.24
1.0
Nctn
0
. O
0
0
<|>
-
8
— —
O
Nonwastewaten
Concentration
O-
n
P104
Pi 06
*>110
Pi 14 .
PUS
Pllfl
P120 ., , ,
P121 -_,,-, .
P123 m ,
U002 - , , --
y(X>4
U005 _——..— ..-..—
U0 12 „ ^..n^
U018
» U019
Jl UW«^ —
U02S -_..
U07* , ,,
W3l -
U03? . ,
U036
Sivtf cytmO«
Sodium cy»r*d«
Te&tetnyl («i AMtylammcfluo.- 1 ne ....
Anil.o«
Banz(a)anmric«ne
Burafl1^*
rnetrvant.
Bis(2ver -
Cyanides (Total)
Cyanid« (Amenable)-..
lusd
Thallium
Selenium — .
Tnallium....— _—.-_.—...
Vanadium
Vanadium
Cyanides Total)
Cyanides (Amenable)
Toxaphena
Acetone.-
Acetomtnle
Acetopnenone
2-AcetytarnnoHuorene....
Acrylonthle
Aniline
Banzlalantnracene
Beruo(a)pyr>ne —
Bu(2-chloroetnoxy)
metnane.
Bis(2-chioro«tnyl) ether..
Bb(2)
(')
(•)
C)
(•)
(«)
(•)
0
110
9.1
NA
110
9.1
NA
NA
NA
NA
NA
NA
110
9.1
1.3
160
0.17
8.7
140
84
14
8.2
36
13
7.2
7.2
13.
28
15
15
2.6
NA
0.13
S.7
NA
1*
NA
33
5.6
33
g
•^
e
3
*~ "" "" 3
3
— 3
•—"—•—"""" *0
^
•
»
o
3
(') ^
(') 83
•
ii\ 3
' ' n
(')
(')
(')
(')
(')
(')
(')
(')
(M
0
(')
(')
(')
(')
(')
, *cn
(') e>
(') 00
-------
268.43 TABLE CCW.—CONSTITUENT CONCENTRATIONS IN WASTES—Continued
co
CO
Ci
. Waiueodo
UC44
•UOSO
U051
UC*9
U057
U060
U063
U066
U067
I.IOfilJ
U068-
y070 -
U071
i_W72
0075
1)076
U078 -...
U07?
UOQO
U081
CofTtfrwroaJ ctwrtcal
name
?-ChlO'9P'V"*0'
Creaotl (CrnyK tod) ...
C>tiohexanone
nnn
nny
r>beraoD>cnloroo«n2ene
m-Dicnioroeerjene
Oc*ilc»o*fluorometn-
ane.
1.1-Dictilc«oer-*ne
1.1-DicJiioroeriy*«rw ......
1.2-Oc«0'oenytef>e...
Memyieoe e-Joroe
2.4-DicMorconenol
See alao
NA
NA. .
Table CCWE in 268.41.
NA
Table 2 in 268.42
NA .
NA
NA
NA
NA ...
NA
NA
NA
NA
NA
NA
NA
NA .. . . ...
NA . _.
NA ....
NA ... ... .
Regulated haaretoua
constituent
2benzoc*orro-emane
(Ethyfene dibromide).
Oioromomemane
O-n-butyl r^.tnalate
c-Dtchlorobenzene....
m-Dchiorobeniene
p-DtcMorobenzene. —
DcnlorodinuororTtetn-
ane.
1.1-Dicnioroethane
1 i-Dicnloroe thane
1.1-DieMoroethylene
trans-l.2-
Dtchloroethylene.
Methyiene chloride
2.4-D«Silorconenol
CAS number
lor rafulated
hazardous
oomtKuent
B5-57-8
218-01-9
81-20-3
87-86-5
85-01-8
129-00-0
108-64-3
7439-92-1
B5-t8-7
106-94-1
53-19-0
72-54-8
789-02-6
50-29-3
53-19-0
72-54-8
3424-92-6
72-E5-9
53-70-3
96-12-8
106-S3-4
74-35-3
84-74-2
95-50-1
541-73-1
104-48-7
75-71-8
75-34-3
107-06-2
75-35-4
156-60-5
75-09-2
12C-83-2
Wanewaters
ConceMiuabon
(mg/l)
0.044
0.059
0.031
0.18
0.031
0.028
0.028
0.032
0.037
0.11
0.77
0.36
0.023
0.023
0.0039
0.0039
0.023
0.023
0.031
0.031
0.055
0.11
0.028
0.11
0.54
0.088
0.036
0.090
0.23
0.059
0.21
0.025
0.054
0.089
0.044
Notes
C)
C)
C)
CI
o
C)
C)
C)
C)
C)
C)
C)
C)
C)
CI
C)
C)
C)
C)
C)
C)
C)
C)
C)
NWTwasKrwltoO
Concentrabon
(mg/ks)
5.7
8.2
1.5
7.4
1.5
1.5
28
33
NA
5.6
3.2
NA
0.087
0.087
0.087
0.087
0.087
0.087
0.087
0.087
8.2
15
15
l£
28
6.2
6.2
6.2
7.2
7.2
12
33
33
33
14
Noun
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
c
C)
ten
M
0>
00
jp>
W
o
r>
n
•o
K)
M
U082 1
U088
U093 — ..._
U105 -....
U107
U 1 08
U111 ... ....
U 1 1 2 _
Ul 1 7
Ul t8
Ul21
Ul 27 „...
U128 _
U131 „
2.6-D
benzene.
2.4-Dinitroiciyene
Di-n-ocryl pfimalate _ ....
V4-D>oxa;*
t>n-propytrjtrcso*mine .
Ethyl acetate
Ethyl ether
Ethyl meinacrytate
Tnchlofcoonollixxo-
methane.
Hexachlorooenien*
Hexachlorcoutad«ne —
tiene.
Hexachloroetf\ane
c.dlpyrefte.
tod o TipO*m 'y*
MethacjVo«tnle
NA
NA_. .. ._ _
NA .,
Table 2 in 268.42
NA
NA «
NA _
NA
NA
NA
NA
NA..._
NA
NA
NA
NA
NA
g
m
NA._
NA
Table 2 in 268.42
Table CCWE in 268.41..
NA
NA . . _
NA
NA
NA „
Table CCWE in 268.41 _
Table CCWE in 268.41 ..
Table CCWE in 268.41 _
Table CCWE in 268.41
•nd Table 2 in
268.42.
NA
2.6-Dicnlorophenol
1 ,2-Dicnioropropane
OS- 1.3-
Dichloropropylene.
uans-1.3-
Dicnitxopropylene.
Oelhyl phlnalate
P-
Dirnethylaminoazo-
benzene.
2.4-Oimelhylphenol
Dimethyl phttialate
2.4-DtniVotoluene ..._
2.6-Oinitrptohiene
Di-n-cctyl phtnalale
1.4-Dioxane..... .—.._..._.
Dt-n-propylnrtrosoarrune .
Ethyl acetate
Etnyl ether —
Ethyl meihacrylale
Fluorantnene
Trichloromonoftuoro-
metrtane.
HeiacWwoberaene
Hexachlorobutadiene
aipna-BHC -...
beta-BHC
Della-BHC
gamma-BHC (Undone)...
Hezachlorocyclopema-
d«ne.
HeiacMorrjethane
u0"**
tndeno(U.3-
c.ajpyrene.
lodometnane — —
Isobutyl alcohol ..«
~°M ro e
Lead .
o
Mercury
Metnaoylonitriie
87-65-0
78-87-5
10061-01-5
10061-02-6
84-66-2
60-1 1-7
105-67-9
131-11-3
121-14-2
606-20-2
117-84-0
123-91-1
621-64-7
141-78-6
60-29-7
97-63-2
206-»4-0
7S-69-4
118-74-1
87-68-3
319-84-6
319-85-7
319-86-8
58-89-9
77-47-7
67-72-1
16964-48-8
7440-38-2
193-39-5
74-88-4
78-83-1
120-58-1
143-50-^
7439-92-1
7439-92-1
7439-92-1
7439-97-6
126-98-7
0.044
0.85
0.036
0.036
0.54
0 13
0.036
0.54
0.32
0.55
0.54
0.12
0.40
0.34
0.12
0.14
0.068
0.020
0.055
0.055
0.00014
0.00014
0.023
0.0017
0.057
0.055
35
0.79
0.0055
0.19
5.6
0.081
0.0011
0.040
0.040
0.040
0.030
0.24
C C
C)
C)
C)
C)
C)
(i)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
t1)
C)
C)
C)
14
18
18
18
28
NA
14
28
140
28
28
170
14
33
160
160
8.2
33
37
28
0.66
0.66
0.66
0.66
3.6
28
NA
NA
8.2
65
170
2.6
0.13
NA
NA
NA
NA
84
u*
o P
C) \
c> 5-
0
o 1
3
a
C) §
Q
^
i1' S
o 2.
C) *
o -
C) 0
C) =
(') >
o ca
(') o
o 2
C) •<
C)
I1)
I1)
C)
C)
C)
C)
C)
C)
^
C)
C)
(')
C)
C)
— -
ten
„. M
< I 0-
-------
oo
CO
co
Wait* code
II1M
Ul?a
yi§i
"'» ,
U165
U 1 68
U169
U170 , ,
U172
U1 74
U1 79 _
|J1 SO __ _
U181
U163_ -
U1B5
U187
U188
U190
U19J
U196 ......
U203
U204 _ — -_
UM5
M*"
U208
UXQ
U?10
U'n
U?i4
U2 1 5
U216
UJ17
U3M
mine
4.4'-Merhf(eoebis<2-
cnlorctnlne).
Metnyl emyl ketone
U«thyt iueutyl ketone ..
Metnyl menacrylaie
Napntnalene .
2-Napntry.anino
NwoOeotne
4-Nitmpfw.^l
N-Nitrcvx>«nyi«min« ....
N-Nrtrcsoopen&ne
N-NitrosoeyTToiidine
S-Nitro-o-unpdne
Pentacfttoronrroberv
zene.
Pnenacein
Pnonnj
(meiwrK is
Pntna!« aotf).
Pronance
Satrote
Selenium cicxio'e
Setenium suffice .
1.245-
TetracMcrooeruene.
1.1.1.2-
TetracMoroemane.
1.1 2.2-
TetracMcroemane.
TetracftioroeJwyteoe
Ca/t»o tejacniorioe
Thal)(um{l)acfiiAte
ThalUurTt(l) cs,-5onate —
TnaiiiuiTXiJcnlorioe
Thallium(l)rj7ale _
Tnt-n.
S«*«lta
MA
KIA
HA
MA
NA
TtNe 2 in 268.42
NA
NA
MA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA.._
Table CCWE in 268 «1
Table CCWE In 268 41
NA
NA
NA
NA _.
NA
Table 2 in 268 42
Table 2 in 268.42
Table 2 in 268.42
Table 2 'm 268.42
NA . ._
Constituent
4 4'44«thy*«nebia(2-
chtorotri&w).
Welnyt bobutyl ketone
Naptttna)en0 ,
2-Napnthy1«mine
Niu utMnzvnG - -•
4^i1ropn«no1
butytamine.
n-Nirraso0«tnyl«mine ....
n-Nlvo90pipendina
n-Nitrojopyrrolidine
5-Nrtro-o-tohjidine
PanucMaronnrotien-
nne.
Pnenacatin
(measured u
Pntnaiic acid).
Salrole.-
1^,4 5-
Tevacnlorobenzene.
1.1.1J-
TencMoroelhana.
1 1.2.2-
TetracMoroelhane.
Thallium
Thallium
TXfllliym...
Tci-~i
CASnuntwr
htunxxn
constituent
101-14—4
78-83-3
108-10-1
80-62-6
81-20-3
91-59-8
98-85-3
100-02-7
824-16-3
55-18-5
100-75-4
800-55-2
W-SS-8
608-93-5
62-68-8
62-U-2
108-95-2
05-U4 0
23850-58-5
110-86-1
94-59-7
7782-49-2
7782-49-2
85-94-3
630- 20-6
79-34-5
127-18-*
56-23-5
7440-28-0
7440-2S-0
7440-28-0
744O-2B-0
108-88-3
Wilt*
Conc*nv«tion
(mj/l)
050
0.28
0 14
0 14
0058
0.52
0.068
0 12
040
0.40
0.013
0.013
0.32
0.055
0.061
0 039
0 54
OM3
0.081
1 0
1 0
0.057
0057
0056
0057
0 14
0.14
0.14
0.14
0.080
•ntm
Notes
(i\
(')
(')
f*l
C)
0
C)
(')
(')
. ...
m
m
/i\
o
o
o
ci
Nonwaj
Coficfliiuaijud
(mg/hQ)
35
NA
14
28
35
35
28
4.8
16
22
NA
42
NA
NA
NA
9R
teoftion
Notn
(')
(')
(M
(M
(')
(>)
(')
(l)
..«.._..»..«..„.....
'" ~
(')
..._
m
o
n
•n
90
m
a.
o
a
U225
U227 ~
U22B
U235
U2O
(Sromcionr.).
1.1.2-Tncr.ioroeP^ne —
2.4.-
Dicrilotocrenoryace-
casec upon combustion in fuel suoswuwn units operabng in accordance wrth applicable techmcaJ recwements. A faoUty may certify compliance >
witn mew treatment sunCarSs accsfttng to provisions in 40 CFR Section 268.7.
1 Based on analysis ol compcs-'e samples.
1 As analyzed using SW-646 Menod 9010 of 9012: sample size 10 onwn: dsbllation tone: one hour ana fifteen minutes.
«B«seved.
Note: NA means Not Applicable.
CO
!u
w
-------
§ 268.44
40 CFR Ch. I (7-1-92 Edition) ' Environmental Protection Agency
No Land Disposal (or:
K005 Nonwaslcwalcrs generated by the
process described In IHc waste listing de-
scription, and disposed after June 8. 1000.
and nol generated In the course of treat-
Inn waslewalcr forms of these wastes.
(Based on No Generation)
K001 Nonwaslewalers generated by the
process described In the waste listing de-
scription, and disposed after June B. 1080.
and not generated In the course of treat-
ing waslewatcr forms of these wastes.
(Based on No Generation)
K021 Nonwoslewatcr forms of these
wastes generated-by the process described
In the waste listing description and dis-
posed after August 17. 1008. and not gen-
erated In the course of treating
waslcwalcr forms of these wastes (Dosed
on No Generation)
K025 Nonwastewalcr forms of these
wastes generated by the process described
In the waste listing description and dis-
posed after August 17. 1988. and not gen-
erated In the course of treating
waslcwatcr forms of these wastes (Dosed
on No Generation)
. K030 Nonwastewalcr forms of these
wastes generated by the process described
In the waste listing description and dis-
posed after August 17. 1080, and not gun-
crated In the course of treating
waslewaler forms of these wastes (Based
on No Generation)
K044 (Dosed on Reactivity)
K045 (Based on Reactivity)
K047 (Dosed on Reactivity)
KOQO Nonwostcwatcr forms of these
wastes generated by the process described
In the waste listing description itnd dis-
posed after August 17. 108(1, and not gen-
erated In the course of treating
wastcwaler forms of these wastes (Based
on No Generation)
K081 Nonwaslcwalcrs—High Zinc Subcalc-
gory (greater than or equal to 15% total
zinc) (Dosed on Recycling): effective 8/0/
00
KOOO Non-Calcium Sulfalc Subcatcgory—
Nonwaslcwatcr forms of these wastes gen-
erated by the process described In the
waste listing description and disposed
after August 17, 1UIIU, and not generated
In the course of treating waslcwater forms
of these wastes (Dosed on Recycling)
K100 Nonwaslcwatcr forms of those
wastes generated by the process described
In the waste listing description and dis-
posed afler August 17. 1088, and nol gen-
erated In the course of treating
waslewaler forms of these wastes (Dased
on No Generation)
(b) When wastes wllli differing
treatment standards (or a constituent
of concern arc combined (or purposes
o( treatment, the treatment residue
must meet the lowest treatment stand-
ard for the constituent of concern.
(c) Notwithstanding the prohibitions
specified In paragraph (a) of this sec-
tion, treatment and disposal facilities
may demonstrate (and certify pursu-
ant to | 200.1(b)(5)) compliance with
the treatment standards for organic
constituents specified by a footnote In
Table CCW In this section, provided
the following conditions arc satisfied:
(1) The treatment standards for the
organic constituents were established
bused on Incineration in units operat-
ed In accordance with the technical re-
quirements of 40 CFR part 204, sub-
part O, or part 205, subpart O, or
based on combustion in fuel substitu-
tion units operating In accordance
with applicable technical require-
ments;
(2) The treatment or disposal facility
has used the methods referenced in
paragraph (c)( 1) of this .section to
treat the organic constituents; and
CJ) The treatment or disposal facility
has been unable to detect the organic
constituents despite using its best
good-faith efforts as defined by appli-
cable Agency guidance or standards.
Until such guidance or standards are
developed, the treatment or disposal
facility may demonstrate such good-
faith efforts by achieving detection
limits for the regulated organic con-
stituents that do not exceed an order
of magnitude of the treatment stand-
ards specified In this section.
153 Fll 3121U. Aug. 17. 1000. as amended al
54 PR 20049. June 23. 1009; 55 FK 22701,
June 1, 1000: 58 FR 3802, Jan. 31. 10011
H ZGH.'M Variance from a treatment Htinnl-
urd.
(a) Where the treatment standard Is
expressed its a concentration In a
waste or waste extract and a waste
cannot be treated to the specified
level, or where the treatment technol-
ogy Is not appropriate to the waste,
the generator or treatment facility
may petition the Administrator for a
variance from the treatment standard.
The petitioner must demonstrate that
because the physical or chemical prop-
erties of the waste differs significantly
from wastes analyzed In developing
the treatment standard, the waste
cannot be treated to specified levels or
by the specified methods.
(b) Each petition must be submitted
In accordance with the procedures In
§ 200.20.
(c) Each petition must include the
following statement signed by the pe-
titioner or an authorized representa-
tive:
I certify under penalty of law thai I have
personally examined and am familiar with
the Information submitted In this petition
and all attached documents, and that, based
on my Inquiry of those Individuals Immedi-
ately responsible for obtaining the Informa-
tion, 1 believe that the submitted Informa-
tion Is true, accurate, and complete. I am
aware that these arc significant penalties
for submitting false Information. Including
the possibility of fine and Imprisonment.
(d) After receiving a petition for
variance from a treatment standard,
the Administrator may request any ad-
ditional information or samples which
he may require to evaluate the peti-
tion. Additional copies of the complete
petition may be requested as needed to
send to affected states and Regional
Offices.
(c) The Administrator will give
public notice In the FEDERAL REGISTER
of the Intent to approve or deny a pe-
tition and provide an opportunity for
public comment. The final decision on
a variance from a treatment standard
will be published In the FEDERAL UEG-
ISTKII.
(f) A generator, treatment facility,
or disposal facility that is managing a
waste covered by a variance from the
treatment standards must comply with
the waste analysis requirements for re-
stricted wastes found under § 268.7.
(g) During the petition review proc-
ess, the applicant Is required to
comply with all restrictions on land
disposal under this part once the ef-
fective date for the waste has been
reached.
§ 268.44
(h) Where the treatment standard Is
expressed as a concentration In' a
waste or waste extract and a waste
generated under conditions specific to
only one site cannot be treated to the
specified level, or where the treatment
technology Is not appropriate to the
waste, the generator or treatment fa-
cility may apply to the Administrator,
or his delegated representative, for a
site-specific variance from a treatment
standard. The applicant for a site-spe-
cific variance must demonstrate that
because the physical or chemical prop-
erties of the waste differs significantly
from the waste analyzed In developing
the treatment standard, the waste
cannot be treated to specified levels or
by the specified methods.
(I) Each application for a site-specif-
ic variance from a treatment standard
must include the Information in
82G0.20(b)U)-(4):
(j) After receiving an application for
a site-specific variance from a treat-
ment standard, the Assistant Adminis-
trator, or his delegated representative,
may request any additional Informa-
tion or samples which may be required
to evaluate the application.
(k) A generator, treatment facility,
or disposal facility that Is managing a
waste covered by a site-specific vari-
ance from a treatment standard must
comply with the waste analysis re-
quirements for restricted wastes found
under 5 2G8.7.
(1) During the application review
process, the applicant for a site-specif-
ic varlarjce must comply with all re-
strictions -on land disposal under this
part once the effective date for the
waste has been reached.
(m)—(n) [Reserved]
(o) The following facilities are ex-
cluded from the treatment standard
under 5 208.43(a). Table CCW. and are
subject to the following constituent
concentrations:
-------
§268.44
40 CFR Ch. I (7-1-92 Edition)
Environmental Protection Agency
§
3.
CO
a
uj
o
in
a
a
w
z
U)
1
a
O
a
UO
UJ
en
3
m
III? Ell
; i !s i i
o o —
t* * •<• fD CM 3 1
>r)O'«r>4 c6 u> ri p -4
.C
« 2 s a
c
n M 5 «>
aa- 510
EJogK |
W'l
< Of- •*. Q i;
I 1 I * 1 5
JLJLJL^JL s
i^i..ji.i
s
[51 FR 40042. Nov. 7. 1000; 52 FR 21017.
June 4. 1007. as amended at 53 FR 31221.
Aug. 17, 1BUU; 54 Fit 30072. Sept. 0. 1000: 50
FR 12355. Mar. 25. 1001]
Subpart E—Prohibitions on Storage
fi 2GH.50 Prohibitions on utornge of re-
stricted WUHlCB.
(a) Except as provided in this sec-
tion, the storage of hazardous wastes
restricted from land disposal under
subpnrt C of this part of R.CRA sec-
tion 3004 is prohibited, unless the fol-
lowing conditions arc met:
(1) A generator stores such wastes In
tanks or containers on-slte solely for
the purpose of the accumulation of
such quantities of hazardous waste as
necessary to facilitate proper recovery,
treatment, or disposal and the genera-
tor complies with the requirements In
§ 2G2.34 of this chapter. (A generator
who Is In existence on the effective
tlatc of a regulation under this part
and who must store hazardous wastes
for longer than 90 days due to the reg-
ulations under this Part becomes an
owner/operator of a storage facility
and must obtain a RCRA permit. Such
a facility may qualify for interim
status upon compliance with the regu-
lations governing interim status under
40 CFR -21Q.10).
(2) An owner/operator of a hazard-
ous waste treatment, storage, or dis-
posal facility stores such wastes In
tanks or containers solely for the pur-
pose of the accumulation of such'
quantities of hazardous waste as nec-
essary to facilitate proper recovery.
treatment, or disposal and:
(i) Each container is clearly marked
to identify its contents and the date
each period of accumulation begins;
(il) Each tank is clearly marked with
a description of Its contents, the quan-
tity of each hazardous waste received.
and the date each period of accumula-
tion begins, or such Information for
each tank is recorded and maintained
In the operating record at that facility.
Regardless of whether the tank Itself
Is marked, an owner/operator must
comply with the operating record re-
quirements specified in S 2G4.73 or
5 200.13.
(3) A transporter stores man
shipments of such wastes at a ti
facility for 10 days or less.
(b) An owner/operator of a
mcnt. storage or disposal faclll
store such wastes for up to or
unless the Agency can demo
that such storage was not sol
the purpose of accumulation c
quantities of hazardous waste
necessary to facilitate proper re
treatment, or disposal.
(c) A owner/operator of a tre:
storage or disposal facility ma
such wastes beyond one year; hi
the owner/operator bears the
of proving that such storage wa
for the purpose of accumula
such quantities of hazardous u
are necessary to facilitate pro
covery. treatment, or disposal.
(d) If a generator's waste Is
from a prohibition on the type
disposal utilized for the waste
ample, because of an approve
by-case extension under 5 268.5
proved 5 208.G petition, or a r
capacity variance under subp
the prohibition In paragraph
this section does not apply dui
period of such exemption.
(e) The prohibition In paragi
of this section does not apply
ardous wastes that meet the trc
standards specified under §§
208.42, and 260.43 or the tr(
standards specified under the v
In § 2G8.44. or. where trcatmcn
ards have not been specified, is
•pllance with the applicable
tlons specified In § 268.32 or
section 3004.
(f) Liquid hazardous wastes <
Ing polychlorlnalcd blphcnyls
at concentrations greater t
equal to 50 ppm must be stored
clllty that meets the rcqulrcn
40 CFR 7Gl.G5(b) and must
moved from storage and treatc
posed as required by this par
one year of the date when sucl
are first placed Into storage. 1
visions of paragraph (c) of thl;
do not apply to such PCB wa.1
hlbltcd under S 2G8.32 of this p
(51 FR 40042. Nov. 7. 1080: 52 J
June 4. 1087. as amended at 52 I
July 8. 1087: 54 FR 36072, Sept. 6, I
842
0/10
-------
Pt. 268, App. I
40 CFR Ch. I (7-1-92 Edition)
Environmental Protection Agency
Pt. 26B, App.
APPENDIX I TO PART 2GB—TOXICITY CHARACTERISTIC LEACHING PROCEDURE
(TCLP)
NOTE: The TCLP Is published In appendix II of part 201.
[56 FR 11876, Mar. 29. 19901
APPENDIX II TO PART 268—TREATMENT STANDARDS (As CONCENTRATIONS IN THE TREATMENT
RESIDUAL EXTRACT)
(Not*: The technologies shown are tho basis of tho nonimoni standards. Thoy wo noi required to bo used In mooting lite
troalmonl standards)
Conslllulonts of FOOI-FOO5 Spool
Solvent Waalts
Wasio Testability Gioups Fa FOOI-FOOS Sponl Sofvonl Wastes (mg/l)
WatlowalM
005
5.00
1.05
0.05
0.15
2.82
0.125
0.65
005
005
0.05
500
0.25
0.20
0.05
0.05
0.66
1.12
0.079
1.12
1.05
1.05
0.062
005
005
Technology Oasis *
SS
SS
SS
B . ... '
BSAC
AC
SS
(J4AC
SS ...
U ....
SS
SS
SS
JJ
SS
SS
SS&AC
B1AC
B
U&AC
SS
SS
OAAC
u
AC
Waslowalor
Gonoiatod by
Phaimacoulical
Plant •
12.7
All OHIO! '
0.50
5.00
481
0.90
0.05
0.75
0.75
0.125
0.75
0.053
0.75
500
0.75
QUO
075
0.33
0.125
0.33
0.05
033
0.41
090
0.091
000
0.15
1 In aom« instances olhef technologies achieved soinowhal lower lionlmonl values but waste chDfacloiijntkm dntn wore
Insuflicienl to idontify separate tiostatxltly groups. Hotof to UK> BOAT background document lor a detailed explanation ol Itto
determination ol tfto treatmenl standards. ,
SS« steam suipping
B-biological lionlmonl
AC-activated carbon
• Wasiewatera generated by pharmaceutical plants must bo treatoO to th« standards grvon lex all other wastewatera oicopt
in the case ol rrtethyteno chtorioo.
• The tteaumnl standards In this uealability group arn based on incineration.
(61 FR 40053. Nov. 7. 19801
APPENDIX 111 TO PAIIT 20U—LIST OK
IlALOGENATED OllCANIC COMPOUNDS
REGULATED UNDER 5 200.32
In determining the concentration of
HOCs In a hazardous waste (or purposes ot
the t 268.32 land disposal prohibition. EPA
has defined the HOCs that must be Includ-
ed In the calculation as any compounds
luwliiK a curbon-linloKi'H buiul which art:
listed In this npin'tidlx (arc t 2(11).2). Apprii-
dlx III to purl 208 consists of the followltiR
compounds:
Volatile!
Bromodlchloromethane
Dromomclhane
Carbon Tctrachlorldc
Chlorobcnzcne
2-C'hloro-1.3-butndlcnc
Chlorodlbromoinethane
Chlnroclhanc
2-Chloruclhyl vinyl ether
Chloroform
Chloroinclhanc
3-Chloropropcnc
1.2-Dlbromo-3-chloropropanc
1.2-Ulbromomc thane
Dlbromomelhanc
Truns-1.4-Dlchloro-2-bulenc
Dlclilorodlfluoromclhane
1.1-Dlchloroclhnnc
1.2-Dlchloroclhane
1.1-Dlchlorocthylcnc
Trans-1.2-Dlchloroethciic
1.2-Dlchloropropixnc
Trans-1,3-Olchloropropcnc
cls-1.3-Dlchloropropcnc
lodotnclhanc
Mcthylcnc chloride
1.1.1.2-Tctrachlorocthanc
1,1.2.2-Tctrachloroclhanc
Tctrftchlorocthcne
Trlbromomcthnnc
1.1.1-Trlchloroelhiinc
1.1,2-Trlchloroclho.ne
Trlchloroethcnc
Trlchloromonofluoroinclhaiic
1.2.3-Trlchloropropnnc
Vinyl chloride
Semivolalila
Dls(2-chloroethoxy)cthanc
Dls(2-chloroclhyl)cthcr
Dls(2-chlorolsopropyl) ether
P-Chloroanlllne
Chlorobcnzllatc
p-Chloro-m-cresol
2-Chloronnphlhnlcnc
2-Chlorophcnol
3-Chloroproplonltrlle
m-Dlchlorobcnzcnu
o-Dlchlorobcnzcnc
P-Dlchlorobcnzenc
3,3'-Dlchlorobcnzldlne
2,4-Dlchlorophenol
2.0-Olchlorophcnol
Hexachlorobcnzene
llcxnchlorobulndlcnc
llexnchlorocyclopcntadlcnc
llrxnchlurocthnnc
UexiiclilurouroDlicnc
llcxnchluropropcnc
4,4'-Mclhylcncbls(2-cliluroanlllnc)
Pviilachlorobcnzcnc
Pcnlachloroethanc
Pcnlachloronltrobcnzcne
Pentachlorophenol
Pronamlde
1.2.4,5-Tctrachlorobcnzcnc
2.3.4,0-Tclrachlorophenol
1.2.4-Trlchlorobcii7.cnc
2.4,!>.Trlchlorophcnol
2.4.0-Trlchlorophcnol
Trls(2.3-dlbromopropyl)phosphale
Organoc/ilorinc Pesticides
Aldrln
alpha-BHC
bcta-DIIC
delta DHC
gamma-BHC
Chlordanc
ODD
DDE
DDT
Dlcldrln
Endosulfan I
Endosulfan II
Endrln
Endrln aldehyde
Hcptachlor
Hcplachlor cpoxldc
Isodrln
Kcpone
Mcthoxyclor
Toxaphcne
Phenoxuacclic Acid Herbicides
2.4-Dlchlorophcnoxyacctlc acid
Sllvcx
2.4.5-T
PCBi
Aroclor 1010
Aroclor 1221
Aroclor 1232
Aroclor 1242
Aroclor 1246
Aroclor 1254
Aroclor 1260
PCOs not otherwise specified
Dioiiii3 and Furans
Hexochlorodlbcnzo-p-dloxlns
Hcxachlorodlbcnzofuran
Pcnlachlorodlbcnzo-p-dloxlns
Pcntachlorodibcnzofuran
Tetrachlorodlbenzo-p-dloxlns;
TeUrachlorodlbenzofuran
2.3,7.8-Tetrachlorodlbcnzo-p-dloxln
[52 FR 25791. July 8. 1987]
APPENDIX IV TO PART 68—
OnCANOMETALLIC LAB PACKS
Hazardous waste with the following
Hazardous Waste Code No. may be plat
an "organometalllc" or "appendix I'
pack:"
POOl. P002. P003. P004. POOS. P006.
P008. P009. P013. POM. PO15. P016.
P018. P020. P021. P022. P023. P024.
P027. P02B. P029. P030. P031. P033.
P036. P037, P03B. P039. P040. P041,
-------
37270 Federal Register / Vol. 57, No. 160 / Tuesday, August 18, 1992 / Rules and Regulations
post-closure, and financial
responsibility, such a containment :
building is then considered to be a :
landfill, and the owner or operator must
meet all of the requirements for landfills
specified in subparts G and H of this
part.
§§265.1103—265.1110 [Reserved]
PART 268-LAND DISPOSAL
RESTRICTIONS
26. The authority citation for part 268
continues to read as follows:
Authority: 42 U.S.C. 6905, 6912(a). 6921. and
6924.
27. In § 268.2 paragraph (g) is revised
and paragraph (h) added to read as
follows:
§ 268.2 Definitions applicable In this part.
• • • • •
(g) Debris means solid material
exceeding a 60 nun particle size that is
intended for disposal and that is: A
manufactured object; or plant or animal
matter or natural geologic material.
However, the following materials are
not debris: Any material for which a
specific treatment standard is provided
in subpart D, part 268; Process residuals
such as smelter slag and residues from
the treatment of waste, wastewater,
sludges, or air emission residues; and
Intact containers of hazardous waste
that are not ruptured and that retain at
least 75% of their original volume. A
mixture of debris that has not been
treated to the standards provided by
§ 268.45 and other material is subject to
regulation as debris if the mixture is
comprised primarily of debris, by
volume, based on visual inspection.
(h) Hazardous debris means debris
that contains a hazardous waste listed
in subpart D of part 2B1 of this chapter,
or that exhibits a characteristic of
hazardous waste identified in subpart C
of part 261 of this chapter.
28. Section 268.5 is amended by
adding "; or" in place of the semicolon
at the end of paragraph (h)(2)(ii), by
redesignating paragraph (h)(2)(v) as
paragraph (h)(2)(vi), by revising
paragraph (h)(2)(iv) and by adding new
paragraph (h)(2)(v) to read as follows:
§ 265.5 Procedure* for case-by-cas*
extensions to an tftscttv* dat*.*,
• • « • •
(h)' • •
I?]'''
(iv) The surface impoundment, if
permitted, is in compliance with the
requirements of subpart F of part 264
and § 264.221 (c). (d) and (e) of this
chapter or
(v) The surface impoundment. If newly
subject to RCRA section 3005{j)(l) due
to the promulgation of additional listings
or characteristics for the identification
of hazardous waste, is in compliance
with the requirements of subpart F of
part 265 of this chapter within 12 months
after the promulgation of additional
listings or characteristics of hazardous
waste, and with the requirements of
§ 265.221 (a), (c) and (d) of this chapter
within 48 months after the promulgation
of additional listings or characteristics
of hazardous waste. If a national
capacity variance is granted, during the
period the variance is in effect, the
surface impoundment, if newly subject
to RCRA section 3005p)(l) due to the
promulgation of additional listings or
characteristics of hazardous waste, is in
compliance with the requirements of
subpart F of part 265 of this chapter
within 12 months after the promulgation
of additional listings or characteristics
of hazardous waste, and with the
requirements of § 265.221 (a), (c) and (d)
of this chapter within 48 months after
the promulgation of additional listings or
characteristics of hazardous waste; or
• A • • •
29. Section 268.7 is amended by
revising paragraphs (a)(l)(iii). (a)(l)(iv),
(a](2) introductory text (a)(3)(iv),
|a)(3)(v), (a)(4) introductory text. (b)(4)
introductory text, and (b)(5)
introductory text, and by adding
paragraphs (a)(l)(v), (a)(3}(vi). and (d) to
read as follows:
§ 263.7 Waste analysis and recordkeeplng.
(a) * ' *
(I)'*'
(iii) The manifest number associated
with the shipment of waste;
(iv) For hazardous debris, the
contaminants subject to treatment as
provided by § 268.45(b) and the
following statement: "This hazardous
debris is subject to the alternative
treatment standards of 40 CFR 268.45";
and
(v) Waste analysis data, where
available.
(2) If a generator determines that he is
managing a restricted waste under this
Part, and determines that the waste can
be land disposed without further
treatment, with each shipment of waste
he must submit, to the treatment,
storage, or land disposal facility, a
notice and a certification stating that the
waste meets the applicable treatment
standards set forth in subpart D of this
part and the applicable prohibition
levels set forth in } 268.32 or RCRA
section 3004(d). Generators of hazardous
debris that is excluded from the .
definition of hazardous waste under
§ 261.3(e)(2) of this chapter (i.e.. debris
that the Director has determined does
not contain hazardous waste), however.
are not subject to these notification and
certification requirements.
• • • • •
(3)* ' '
(iv) Waste analysis data, where
available;
(v) For hazardous debris, the
contaminants subject to treatment as
provided by § 268.45(b) and the
following statement: "This hazardous
debris is subject to the alternative
treatment standards of 40 CFR 268.45":
and
(vi) The date the waste is subject to
the prohibitions.
(4) If a generator is managing
prohibited waste in tanks, containers, or
containment buildings regulated under
40 CFR 262.34. and is treating such
waste in such tanks, containers, or
containment buildings to meet
applicable treatment standards under
subpart D of this part, the generator
must develop and follow a written
waste analysis plan which describes the
procedures the generator will carry out
to comply with the treatment standards.
(Generators treating hazardous debris
under the alternative treatment
standards of Table 1, J 268.45, however,
are not subject to these waste analysis
requirements.) The plan must be kept on
site in the generator's records, and the
following requirements must be met
* • * • •
(b) * * '
(4) A notice must be sent with each
waste shipment to the land disposal
facility which includes the following
information, except that debris excluded
from the definition of hazardous waste
under § 261.3(e) of this chapter (i.e.,
debris treated by an extraction or
destruction technology provided by
Table 1. § 268.45. and debris that the
Director has determined does not
contain hazardous waste) is subject to
the notification and certification
requirements of paragraph (d) of this
section rather than these notification
requirements:
• • . • • •
(5) The treatment facility must submit
a certification with each shipment of
waste or treatment residue of a
restricted waste to the land disposal
facility stating that the waste or
treatment residue has been treated in
compliance with the applicable
performance standards specified in
subpart D of this part and the applicable
prohibitions set forth in § 268-32 or
RCRA section 3004(d). Debris excluded
from the definition of hazardous waste
under § 261.3(e) of this chapter (i.e..
debris treated by an extraction or
destruction technology provided by
-------
Federal Register / Vol. 57. No. 160 / Tuesday. August 18. 1992 / Rules and Regulations 37271
Table 1. 5 268.45, and debris that the
Director has determined does not
contain hazardous waste), however, is
subject to the notification and
certification requirements of paragraph
(d) of this section rather than the
certification requirements of this
paragraph (b){5).
t • • • . •
(d) Generators or treaters who first
claim that hazardous debris is excluded
from the definition of hazardous waste
under § 2613(e) of this chapter (i.e.,
debris treated by an extraction or
destruction technology provided by
Table 1. § 268.45, and debris that the
Director has determined does not
contain hazardous waste) are subject to
the following notification and
certification requirements:
(1) A one-time notification must be
submitted to the Director or authorized
State including the following
information:
(i) The name and address of the
Subtitle D facility receiving the treated
debris;
(ii) A description of the hazardous
debris as initially generated including
the applicable EPA Hazardous Waste
Number(s); and
(iii) For debris excluded under
5 261.3(e)(l) of this chapter, the • •
technology from Table 1, § 266.45, used
to treat the debris.
(2) The notification must be updated if
the debris is shipped to a different
facility, and, for debris excluded under
§ 261.2(e)(l) of this chapter, if a different
type of debris is treated or if a different
technology is used to treat the debris.
(3) For debris excluded under
§ 251.3(e)(l) of this chapter, the owner
or operator of the treatment facility must
document and certify compliance with
the treatment standards of Table 1. .
§ 258.45. as follows:
(i) Records must be kept of all
inspections, evaluations, and analyses
of treated debris that are made to
determine compliance with the
treatment standards;
(ii) Records must be kept of any data
or information the treater obtains during
treatment of the debris that identifies
key operating parameters of the
treatment unit; and
(iii) For each shipment of treated
debris, a certification of compliance
with the treatment standards must be
signed by an authorized representative
and placed in the facility's files. The
certification must state the following: "I
certify under penalty of law that the
debris has been treated in accordance
with the requirements of 40 CFR 268.45.1
arr. aware that there are significant
penalties for making a false
certification, including the possibility of
fine and imprisonment."
• • « • •
30. In 5 288.9,.paragraph (d) is .revised
to read as follows:
J 263.9 Special rule* refardng wastes
that exhtou a characteristic.
• • • t ..-. •
(d) Wastes that exhibit a
characteristic are also subject to § 268.7
requirements, except that once the .
waste is no longer hazardous, a one-
time notification and certification must
be placed in the generators or treaters
files and sent to the EPA region or
authorized state. The notification and
certification that is placed in the
generators or treaters files must be
updated if the process or operation
generating the waste changes and/or if
the subtitle D facility receiving the
waste changes. However, the generator
or treater need only notify the EPA
region or an authorized state on an
annual basis if such changes occur. Such
notification and certification should be
sent to the EPA region or authorized
state by the end of the calendar year.
but no later that December 31.
(1) The notification must include the
following information:
(i) Name and address of the Subtitle D
facility receiving the waste shipment;
(ii) A description of the waste as
initially generated, including the
applicable EPA Hazardous Waste
Number(s) and treatability group(s);
(iii) The treatment standards
applicable to the waste at the point of
generation.
(2) The certification must be signed by
an authorized representative and must
state the language found in $ 268.7(b)(5).
31. Section 288.14 is added to subpart
B of part 268 to read as follows:
§268.14 Surface Impoundment
exemptions.
(a) This section defines additional
circumstances under which an
otherwise prohibited waste may
continue to be placed in a surface
impoundment
(b) Wastes which are newry identified
or listed under section 3001 after
November 8,1984, and stored in a
surface impoundment that is newly
subject to subtitle C of RCRA as a result
of the additional identification or listing,
may continue to be stored in the surface
impoundment for 48 months after the .
promulgation of the additional listing or
characteristic, not withstanding that the
waste is otherwise prohibited from land
disposal, provided that the surface
impoundment is in compliance with the
requirements of subpart F of part 265 of
this chapter within 12 months after
promulgation of the oew listing or
characteristic.
(c) Wastes which ere newry identified
or listed under section 3001 after
November 8,1984, and treated in a
surface.impoundment that is newly
subject to subtitle C of RCRA as a result
of the additional identification or listing,
may continue to be treated in that
surface impoundment, not withstanding
that the waste is otherwise prohibited
from land disposal, provided that
surface impoundment is in compliance
with the requirements of subpart F of
part 2S5 of this chapter within 12 months
after the promulgation of the new listing
or characteristic. In addition, if the
surface impoundment continues to treat
hazardous waste after 48 r.onths from
promulgation of the additional listing or
characteristic, it must then be in
compliance with { 288.4.
32. Section 268.38 is added to subpart
C of part 268 to read as follows:
§268.36 Waste specific proWbrtlons—
newly Hated wastes.
ta) Effective November 9.1992, the
wastes specified in 40 CFR 281.32 as
EPA Hazardous Waste Numbers K107.
K108, K109, KllO, Kill, K112. K117,
K118, K123, K124.-K125. K126. K131.
K132, and K136; and the wastes
specified in 40 CFR 261.33(f) as EPA
Hazardous Waste numbers U328. U353,
and U359 are prohibited from lar.d
disposal.
(b) Effective June 30.1993, the wastes
specified in 40 CFR 261.31 as EPA
Hazardous Waste Numbers F037 and
F038 that are not generated from surface
impoundment cleanouls or closures are
prohibited from land disposal.
(c) Effective June 30.19S4. the wastes
specified in 40 CFR 261.31 as EPA
Hazardous Waste Numbers F037 and
F038 that are generated from surface
impoundment cleanouts or closures are
prohibited from land disposal.
(d) Effective June 30.1994. radioactive
wastes that are mixed with hazardous
wastes specified-in 40 CFR 261.31 as
EPA Hazardous Waste Numbers F037
and F038; the wastes specified in 40 CFR
261.32 as EPA Hazardous Waste
Numbers K107, K108, K109, KllO. Kill.
K112. K117. K118, K123, K124, K125.
K126 K131. K132, and K136; or the
wastes specified in 40 CFR 26l.33(fj as
EPA Hazardous Waste Numbers U328.
U353, and U359 are prohibited from land
' disposal.
(e) Effective June 30.1994, debris
contaminated with hazardous wastes
specified in 40 CFR 261.31 as EPA
• Hazardous Waste Numbers F037 and
F038: the wastes specified in 40 CFR
261.32 as EPA Hazardous Waste
-------
37272 Federal Register / Vol. 57, No. 160 / Tuesday." August 18. 1992 / Rules and Regulations
Numbers K107. K108. K109. KllO. Kill.
K112. K117. K118. K123. K124. K125.
K126 K131. K132. and K136; or the :
wastes specified in 40 CFR 261.33(f) as
EPA Hazardous Waste Numbers U32S.
U3S3. and U359: and which is not
contaminated with any other waste
already subject to a prohibition are .
prohibited from land disposal.
(f) Between June 30.1992 and June 30.
1993, the wastes included in paragraph
(b) of this section may be disposed of in
a landfill, only if such unit is in -i
compliance with the requirements
specified in § 268.5(h)(2). and may be
generated in and disposed of in a
surface impoundment only if such unit is
in compliance with either § 268.5(h)(2) or
5 268.14. .
(g) Between June 30,1992 and June 30.
1S94, the wastes included in paragraphs
(d) and (e) of this section may be
disposed of in a landfill only if such unit
is in compliance with the requirements
specified in § 268.5(h)(2). and may be
generated in and disposed of in a
surface impoundment only if such unit is
in compliance with either § 2S6.5(h)(2) or
§ 268.14.
(h) The requirements of paragraphs
(a), (b), (c), (d). and (e) of this section do
r.ot apply if:
(1) The wastes meet the applicable
standards specified in subpart D of this
part
(2) Persons have been granted an
exemption from a prohibition pursuant
to a petition under § 268.0. with respect
to those wastes and units covered by
the petition;
(3) The wastes meet the applicable
alternate standards established
pursuant to a petition granted under
5 268.44:
(4) Persons have been granted an
extension to the effective date of a
prohibition pursuant to § 268.5, with
respect to the wastes covered by the
extension.
(i) To determine whether a hazardous
waste identified in this section exceeds
the applicable treatment standards
specified in §§ 268.41 and 268.43. the
initial generator must test a
representative sample of the waste
extract or the entire waste, depending
on whether the treatment standards are
expressed as concentrations in the
waste extract or the waste, or the
generator may use knowledge of the
waste. If the waste contains constituents
in excess of the applicable levels in
subpart D of this part, the waste is
prohibited from land disposal, and all
requirements of part 268 are applicable.
except as otherwise specified.
33. In 5 268.40, paragraph (b) is
revised and paragraph (d) is added to
read as follows: -
§ 268.40 Applicability of treatment
standards.
» * • • •
. (b) A restricted waste for which a
treatment technology is specified under
§ 268.42(a) or hazardous debris for
which a treatment technology is
specified under § 268.45 may be land
disposed after it is treated using that
specified technology or an equivalent
treatment method approved by the
Administrator under the procedures set
forth in § 268.42(b).
• • * • •
(d) If a treatment standard has been
established in §§ 268.41 through 268.43
for a hazardous waste that is itself
hazardous debris, the waste is subject to
those standards rather than the
standards for hazardous debris under
§ 268.45.
34. In § 268.41. paragraph (a) text
preceding table is revised, and Table •
CCWE is amended by revising the eatry
for "F001-F005 spent solvents." by
removing the entries for "K061 {Low
Zinc Subcategory—less than \5~o Total
Zinc)" and "K061 (High Zinc
Subcategory—greater than 15^ Total
Zinc)—Effective until August 7, 1991, by
adding entries for "F037". "F038". and
"K061", and by adding paragraph (c] to
read as follows:
§268.41 Treatment standards expressed
as concentrations In waste extract.
(a) Table CCWE identifies the
restricted wastes and the concentrations
- of their associated constituents which
may not be exceeded in the extract of a
waste or waste treatment residual
extracted using the test method in
appendix I of this par: for the allowable
land disposal of such wastes.
Compliance with these concentrations is
required based upon grab samples.
268.41 TABLE CCWE.—CONSTITUENT CONCENTRATIONS IN WASTE EXTRACT
Waste cade
F001-F005 spent solvents
F037
F038...- .
K061
-
Coroner-
ch^C3J See also Regulated hazardous consbtueni
name
NA Tay*» CC'^v in 268 43 Car^o" d^urfidA
Mettianol
NA Table CCW ta 268 43 Chromium (TotaJ)
. . NA - Table CCW in 268 43 Chrormjm (Total) _ „ _
. . .
Arsenic '
Barium.
1 ~ . BerytHum
Cadmium _
Chromium (Total) ..
Lead .„- „-.,, , . .-
. Mercury ___
Nickel
Selenium :.
Silver
hazardous
constituent
75-15-0
108-94-1
67-56-1
7440-47-32
7440-02-0
7440-47-32
744O-02-0
7440-36-0
7440-38-2
7440-39-3
7440-41-7
7440-43-9
7440-47-32
7439-92-1
7439-97-6
7440-02-0
7782-49-2
7440-22-4
7440-66-6
Wastewalers I
Cooc&nta- f.
NA..... _...
NA
NA
NA
NA _'
NA
NA..
NA _
NA
NA ."
NA .
NA
NA
NA
NA
NA
NA
NA
NA
NA.
^Jorv
Jotes
4.8
0.75
0.75
1.7
0.20
1.7
0.20
2.1
0.055
- 7.6
0.014
0.19
0.33
0.37
0.009
5
0.16
. 0.3
0.078
5.3
-------
Federal Register / Vol. 57, No. 160 / Tuesday, August 18, 1992 / Rules and Regulations
(c) The treatment standards for the
constituents in F001-F005 which are
listed in Table CCWE only apply to
wastes which contain one, two, or all
three of these constituents. If the waste
contains any of these three constituents
along with any of the other 26
constituents found in F001-F005, then
only the treatment standards in § 268.43
Table CCW are required.
35-36. In { 268.42. Table 2 of
paragraph (a) rs amended by adding
K123, K124. K125, K126, U323, U353. and
U359 in alphanumerical order and
paragraphs (b) and (d) are revised to
read as follows: •
entries for K107. K108, K109. KllO, K112, •
§ 268.42 Treatment standards expressed
n *p«ctfied technologies.
268.42 TABLE 2.—TECHNOLOGY-BASED STANDARDS BY RCRA WASTE CODE
Waste
code
See aiso
Waste descriptions and/or treatment subcalegpry
CAS No.
lor
regaled
hazardous
consmu-
Technology code
Wastewsters
Nonwastewaters
NA_..
K107_ Column bottoms from product separation from tne produc-
tion ol 1.1-dffnetrylriydraiine (UDMH) from carboxvtic
acid hydraades.
K108 Condensed column overheads from product separation NA
and condensed reactor vent gases from the producbon
01 l.l-dimernylhydraane (UOMH) from cartoxytic ecid
hyorazides.
K109— _ Spent filter cartridges from product purrficstjon from the NA
production o< l.l-dime9>yinydrazJr>e (UDMH) »rom cv-
boxytic acid hydrazkjes.
K110- Condensed column overheads from intermediate sepere- NA.._ —
tion from Bie production of 1.1-dimethy»iy3ra23ne
(UDMH) from carboxyfc: acid hydrazides.
K112 Reaction by-product water from me drying column in (he NA....
production ol toluenediamine via hycVogenabon o* tfni-
tjotokierve.
INCIN: or CHOXD fb. CARBN: or INCIN.
BIOOG it CARBN.
INCIN; or CHOXD fb. CAR9N; or INCIN.
BIOOG ft CARBN.
INCIN; or CHOXD fb. CAHBN; or INCIN.
BIOOG m CARBN.
INCIN: or CHOXD fb. CAHBN: or INC:N.
BIOOG ft CARBN.
INCIN; or CHOXD fb, CARBN; or INCIN.
BIODG fb CARBN.
K123 Process waslewater (inducing supemates. filtrates, and NA_
wasnwaiers) from trie production of etnytenebisditNocw-
bamic acid and its sarts.
K'.24 _ Reactor vent scrubber water from the production of efliy- MA
tenebisdithiccarbamic acid and te salts.
K125 — — Filtration, evaporation, and cararrfugation solids from »w NA
production of ethyienebisditniocarbamic acid and its
salts.
K126 — - Bagrxx-se dusl and floor s»eepmgs in milling and sacfcag- NA
ing operations Iron (he production or tormutotion ot
etnylene beditriiocarbamic acid and its salts.
INCIN; or CHOXD fb (ElOOG or INCIN.
CAnBN). ' '
INCIN; or CHOXD ft (BlODG rx INCIN.
CAREN).
INCIN; or CHOXD to (BIODG or KIN.
CARB.NT
INCIN; or CHOXD fb (BlODG or INCIN.
CARBN).
U32S o-toruidine...
... 85-53-1..
U353 p-toluidine _ _ 106-»9-0..
U3S9 ZOToxy^tharol. _ _ 110-60-5..
INCIN; or CHOXO ft). (BKDDG or
CARBN): or BIODG ft CARBN.
INCIN; or CHOXD ft. (BIODG Or
CARBN): or BIOOG ft CAR8N.
INCIN; or CHOXD ft. (BIODG or
CARBN); or BIODG ft CARBN.
INC.'N: or Thermal
Destruccon.
INCIN; or Thermal
Destruction.
INCIN; or FSUBS.
(b) Any person may submit an
application to the Administrator
demonstrating that an alternative
treatment method can achieve a
measure of performance equivalent to
that achieved by methods specified in
paragraphs (a), (c). and (d) of this
section for wastes or specified in Table
1 of § 268.45 for hazardous debris. The
applicant must submit information
demonstrating that his treatment method
is in compliance with federal. sta*te, and
local requirements and is protective of
human health and the environment. On
the basis of such information and any
other available information, the
Administrator may approve the use of
the alternative treatment method if he
finds that the alternative treatment
method provides a measure of
performance equivalent to that achieved
by methods specified in paragraphs (a),
(c). and (d) of this section for wastes or
in Table 1 of J 268.45 for hazardous
debris. Any approval must be stated in
writing and may contain such provisions
and conditions as the Administrator
deems appropriate. The person to whom
such approval is issued must comply
with all limitations contained in such a
determination.
• • * • •
(d) Radioactive hazardous mixed
wastes with treatment standards
specified in Table 3 of this section are
not subject to any treatment standards
specified in |§ 268.41 or 268.43, or Table
2 of this section. Radioactive hazardous
mixed wastes not subject to treatment
standards in Table 3 of this section
remain subject to all applicable
treatment standards specified in
§§ 268.41. 268.43, and Table 2 of this
section. Hazardous debris containing
radioactive waste is not subject to the
treatment standards specified in Table 3
of this section but is subject to the
treatment standards specified in
§ 268.45.
'37. In § 268.43(a) Table CCW is
amended by revising the entries for
F001-F005 spent solvents, K015. K016,
K018. K019, K020, K023, K024. K028.
K030. K043, K048. K049, K050. KOS1.
K052, K087, K093. K094. U028, U069,
U088, U102. U107. and U190, by
removing the entry for 1)042, and by
-------
37274 Federal Register / Vol. 57. No. 160 / Tuesday.-August IB. 1992 / Rules and Regulations
adding the entries for F037, F038, K117. § 268.43 Treatment standards expressed
K118, K131. K132. and K136 in as waste concentrations, '•
alphanumerical order to read as follows: (a) * * *
268.43.—TABLE CCW.—CONSTITUENT CONCENTRATIONS IN WASTES
c
Waste exle Commercial Sae -i.,, Regulated hazardous fo
cooe chemical name ^^ .. constituent t
c
F001-F005 spent NA _ __ _ __.. Acetone ._
solvents.
Benzene - .
n-3uty! alcohol -
Carbon tetrachioride _
Chlorobenzene... .
o-cresol - ....
o-Oichlorobenrene
Ethyl acetate —
Ethyl ether _.
Isobutyl alcohol
Metnylene chloride
Methyl ethyl ketone.-
Methyl isobutyl ketone
Nitrobenzene .
Pyridine-. - _
Tetrachtoroetrrylene .....
Toluene '.
1.1.1 -Tnchtoroethane _
1 .1 ,2-Tricfiloroeeiane
Trichloroeihylene _.
1.1,2-Trichtoro- 1.2.2-
trifluoromethane.
Trichlcfomono-
fluoromethane.
Xytenes (total)
F037 ..._ .- NA Table CCWE in Acenaphmene
268.41.
Anthracene _
Benzene
Benzo(a)arithraceoe -...
Benzo(a)pyrene
Bis(2-ethy1he«yl) phthalate ...
Chrysene ....
Di-n-butyl phthalate _.
Ethylbenzene
Naphthalene —
Phenol _
Pyrene
Toluene-
Cyanides (Total)
Chromium (Total)
Lead .
F038 NA _ Table CCWE in Benzene .
263.41.
Benzo(a)pyrene...S _ -
Bis<2-ethylhexyO phtrialate...
Chrysene
Di-n-butyl phtnalate
Ethylbenzene _'.
Ftuofeoe ...... _...,.,
Naphthalene ^
Phenol
Pyrgne
To'uflfV .
Cyanide* fToial)
Chromium (Total)
KOI? ;.,, NA ' T?hl" Cf^WE in Anrhr;y.Ana
268.41. .
*S number
Wastewaters Nonwastewalers
azardous Concentration
onstituent (mg/l)
67-64-1
71-J3-2
71-36-3
56-23-5
108-90-7 '
95-50-1
141-7-6
100-^)1-4
60-29-7
78-83-1
75-9-2
78-93-3
108-10-1
98-95-3
110-86-1
127-18-4
108-88-3
71-55-6
79-CO-5
79-01-6
76-13-1 .
75-69-4
208-96-8
120-12-7
71-43-2
50-32-8
117-81-7
75-15-0
218-01-9
105-67-9
100-41-4
86-73-7
.91 -20-3
85-01-8
108-95-2
129-00-0
108-88-3
57-12-5
7440-47-32
7439-92-1
71-43-2
.50-32-8
117-81-7
218-01-9
84-74-2
100-41-4
86-73-7
91-20-3
85-01-e
108-B5-2
129-00-0
108-88-3
57-12-5
7440-47-32
7439-92-1
120-12-7
98-87-3
0.28
0.070
5.6
0.057
0.057
0.77
0.11
0.088
0.34
0.057
0.12
5.6
0.089
0.28
0.14
0.068
0.014
0.056
O.C8
0.054
0.030
0.054
O.C57
0.02
0.32
0.059
0.059
0.14
0.059
0.061
0.28
0.059
0.057
0.057
0.059
0.059
0.059
0.039
0.067
0.08
0.32
0.028
0.2
0.037
0.14
0.061
0.28
- ' 0.059
0.057
0.057
0.059
0.059
0.059
0.039
0.067
0.080
0.32
0.028
OS
0.037
0.059
0.28
u iae Concentra-
"Oles ton (mg/l)
160
3.7
2.6
5.6
5.7
3.2
5.5
6.2
33
6.0
•. 160
170
33
36
33
14
16
5.6
28
5.6
7.6
5.6
28
33
28
=) NA
C) 28
') 14
') 20
«) 12
') 7.3
') 15
') 3.6
(=) 14
J) NA
('} 42
(') 34
(') 3.6
(') 36
(') 14
(3) 22
C) 1.8
NA
NA
{*) 14
(') 12
') 7.3
') 15
') 3.6
«) 14
') NA
') 42
') 34
') 3.6
«) 36
H 14
(.) 22
C) 18
NA
NA
3.4
6.2
Notes
C)
C)
C)
C)
C)
C)
C)
C)
C)
c
C)
C)
C)
n
C)
c
c
c
c
c
c
c
C1)
-------
Federal Register / Vol. 57. No. "160 / Tuesday. August 18. 1992 / Rules and Regulations 37275
. 268.43.— TABLE CCW.— CONSTITUENT CONCENTRATIONS IN WASTES— Continued
Waste code
K016
K018
K019 _ .. •
K020
KOJ3 ......
K02<
K023......
"030
••330
Commercial . ,. . Regulated hazardous
chemical name aee arao constituent
Sum o( Benzofb) ftuoran-
thene and BenzofX) fluo-
ranthene. •
Phenanthrene
Toluene ':
Chromium (Total)
Nickel
NA..._ _ _ _ ._ Hexachtorobenzene ..
HexacNorobutadene
Hexachtoroeydoperrta •
diene.
Hexachtoroethane
Tetrachkxoethene ._ _
• * • •
..... NA _ _ _ . .. Chtoroethane -
Otoromemane ...
1 , 1 -Dehtoroethane
1,2-Dichtoroethane
Hexachtorobenzene
Haxachtorobutadiene
Pentachtoroethane
1.1.1-Trichtoroethane
Haxachtoroelhane
Chtoroberoene
p-Dichlorobenzene
1 ,2-Dichtoroetharte
Hexachtofoethane
Naphthalene
Phenanthrene ,
1.2.4.5-
Tetrachkxobercene.
Tetrachtoroemene
1 Z4-Trichlorobenzene
1,1.1-Trichtoroethane._
1.1.2.2-Tetrachtoroemane ...
Tetrachtofoethene
ured as Ptithalic acid).
ured as Phmafic adtf).
268.41. . 1.2-.
DtcNoroethane
Hexachtorobutadiene
Hexachloroethane
Pentachloroethane
1,1.1.2-Tetrachtoroethane ...
1 .1 .2.2-Tetrechtoroethane ....
1 .1 .1 ,-Trichtoroethane
1.1.2-Trichloroethane
Tetrachtoroethylene
Cadmium
Chromium (Total)
Nickel
* • • • .
p-Dichtorobenzene
Hexachtorobutadiene
Hexachtoroethane
Hexachloropropene
Pemachlorobenzene
Pentachloroethane
1A4.5-
Tetrachlorobenzene.
Tetrachtoroethene :
1 ,2.4-Trichtorobenzene
— NA. ._ ... _ 2 4-Dichlorbphenol
2.6-Oichtoropheno
2.4,5-Trichtorophenol
2,4.6-Trichlorophenol
CAS number
tor regulated
hazardous
constituent
207-08-9
85-01-8
108-88-3
7440-47-32
7440-02-0
118-74-1
87-68-3
77-47-4
67-72-1
127-18-4
76-00-3
74-87-3
75-34-3
107-06-2
118-74-1
87-68-3
76-01-7
71-55-8
67-72-1
111-44-4
108-80-7
67-66-3
106-46-7
107-06-2
86-73-7
67-72-1
91-20-3
85-01-8
95-64-3
127-18-4
120-82-1
71-55-6
106-93-4
73-34-6
127-18-4
85-44-9
85-44-9
75-34-3
87-66-3
87-72-1
76-01-7
630-20-*
78-34-6
71-55-6
79-00-5
127-18-4
7440-43-9
7440-47-32
7439-92-1
7440-02-0
85-50-1
106-46-7
87-68-3
67-72-1
1888-71-7
608-93-5
76-01-7
95-84-3
127-18-4
120-82-1
120-83-2
167-65-0
85-95-4
88-06-2
Wastewaters
Concentrat)On m^m*
(mg/0 ™°I)
14 (')
6.0 (')
19 (')
0.38 (')
0.34 (')
8.2 (')
7.8 (')
-------
37276 Federal Register / Vol. 57. No. 160 / Tuesday.-August 18, 1992 / Rules and Regulations
268.43.— TABLE CCW.— CONSTITUENT CONCENTRATIONS IN WASTES— Continued
Waste coca Commercial c^ ^ Regulated hazardous
3518 "**" chemical name aee "*° constituent
Tetrachlorophenols (Total)
PentacNorophenol
Tetracnioroerhene
HetacNorodiberoo-p-
donns.
Hexachtorodibenzohirans
Pentachlorodibenzo-p-
dionns.
PentacMorodibenzo furans—
TetracWcrodibenzo-p-
dionns.
TatracfiJorodibenzoruraro
• • • t .
KO-J8 NA Table CCWE in Benzene
268.41.
Benzcjajpyrene
Bs<2-etnytneiyf) phtnalata _
Di-n-butyl phmalaa
Ethylbercene
Fluo(8O6 ..j- ..T-.L-L-.TL.^
Phenantivene
Pyrn'M*
Cyanides (Totan
Chromium (Total)
Lead
K049 NA .. Table CCWE in Anthracene
. 268.41.
Bertzo(a)pyrene _ _ .
Bis(2-ethymar/r) phthalata_
Carbon disulfide
Chrysene :
2.4-Oimetftyl phenol
Ettiylbenzene
Naphthalene
Phenarrthrene '..... _..
Pnenol •.
Pyrene .
Totuono ___.....„.»....„.
Xytene(s) - _
Cyanides (Total) '....
Chromium (Total)
K050.._ _ NA _ Table CCWE. in Lead
268.41.
Benzo(a)pyren«
Pnenol
Cyanides (Total)
Chromium (Total)
Lead
K051 NA Table CCWE «i Acenaphthene .
268.41.
Benzo(a)pyreoe
Dwvbuiyl phthalale
Fluocene
Pyflp*
TQlv^nf)
XyfcyyW])
Cyandides (Totai)
Ovomium (Totaf)
Und
CAS number
for regulated
hazardous
constituent
87-86-5
79-01-6
71-S3-2
50-32-8
117-81-7
218-01-9
84-74-2
100-41-4
86-73-7
91-20-3
85-01-8
108-95-2
129-00-0
108-8&-3
57-12-5
7440-47-32
7439-92-1
120-12-7
71-43-2
117-61-7
75-150-0
75-15-0
2218-01-9
105-67-9
100-41-4
91-20-3
85-01-8
1O8-95-2
129-00-0
106-&8-3
56-12-5
7440-47-32
7439-92-1
50-32-8
108-95-2
57-12-5
7440-47-32
7439-29-1
83-32-9
120-12-7
71-43-2
50-32-8
117-81-7
75-15-0
2218-01-9
105-67-9
100-41-4
86-73-7
91-20-3
85-01-8
108-95-2
129-00-0
108-88-3
57-12-5
7440-47-32
7439-92-1
71-43-3
50-32-8
Wastewaiers Noowastewaters
Concentration •.!_,_« Concerrtra-
(mg/l) ™°*BS tion (mg/l)
NA
0.089
-0.056
0.000063
0.000063
0.000063
0.000063
0.000063
0.000063
0.14
0.061
0.28
0.059
0.057
0.057
0.059
0.059
0.059
0.039
0.067
0.080
032
0.028
02
0.037
0.059
0.14
0.061
0.28 •
0.014
0.059
0.036
0.057
0.059
0.059
0.039
0.067
0.08
0.32
0.028
0.2
0.037
0.061
0.039
0.028
0.2
0.037
0.059
0.059
0.14
0.059
0.061
0.26
0.059
0.057
0.057
0.059
0.059
0.059
0.039
0.067 .
0.08
0.32
0.028
0.2
0.037
0.14
0.081
0.68
1.9
1.7
0.001
0.001
0.001
0.001
0.001
0.001
') 14
') 12
!) 7.3
') 15
') . 3.6
3) 14
') NA
') «
') 34
•) 3.6
') 36
') 14
') 22
') 1.8
NA
NA
') 28
') n
=) 12
') 7.3
') NA
') 15
') NA
') ' 14
') 42
') 34
') "3.6
') 36
') 14
C) 22
i) 1.8
NA
NA
(') 12
3) 3.6
') 1-8
NA
NA
C) NA
(') 28
») 14
>) 20
') 12
') 7.3
n is
') 3.6
C) 1<
t3) NA
(>) 42
(') 34
(•) 3.6
») 36
«) 14
;>) 22
(') 1.8
NA
NA
(') 14
IJ) 12
Notes
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
C)
CI
CI
CI
• C)
C)
C)
C)
C)
n
"ci
CI
C)
C)
C)
C)
C)
C)
-------
Federal Register / Vol. 57. No. 160 / Tuesday. August 18. 1992 / Rules and Regulations 37277
268.43.—TABLE CCW.—CONSTITUENT CONCENTRATIONS IN WASTES—Continued
Waste code
Commercial
chemical name
See also
Regulated hazardous
constituent
CAS number
•lor regulated
hazardous
constituent
Waslewaters
Nonwaslewaters
Concentration
(mg/l)
Notes
Concentra-
tion (
Notes
K052..
NA ; TaWe CCWE in
- . 268.41.
o-Creso...
K067..
NA Table CCWE in
268.41.
K093.—
K094..._
NA..
NA.
K111 NA..
NA..
. K119...
K131..
K136..
NA..
NA.
NA...
NA_
L'028..,
U069...
U088...
U102...
U107_
U190._
Bis(2-e3>yirie)ryl)
phtM'ate.
Di-n-butyt
phtraiate.
• •
Diethyl pnthalate
• •
Dimethyl phtnalate..
» •
Di-n-ccr/1
phthalate.
• •
. Phtrialk: anhydride
(measu'ed as
Phtnalic acxf).
p-Cfesol...- - -
2.4-Dimemytpoenol._.-....
Ethylbenzene
Naphthalene
Phenanthrene—,_ .._.
Phenol
Toluene _.—
Xytenes
Cyanides (Tola/)
Chromium (Total)
|_ead_ _ _
• Acenaphtnatene.-..
95-48-7
106-«4-5
105-67-9
100-41-4
91-20-3
85-01-8
. 108-95-2
108-68-3
56-12-5
7440-47-32
7439-92-1
•
208-96-8
Benzene... .~ —
Fluor arrthene
Indeno (1,2,3-cd) pyrene.....
Naphtnatene.-
Phenanthrene
Xylenes
Lead
Phthalic anhydride (meas- •
wed as Phmabc acid).
PMnalic anhydride (meas-
ured as Prrmalic acid).
71-43-2
218-01-9
206-44-0
193-39-5
91-20-3
85-01-8
108-88-3
7439-92-1
85-44-9
85-44-9
2.4-Dinrtrotoluene
2,6-Onitrotoluene
Ethytene dibromide—
Methyl bromide
CWorolorm
Ethytene dibromide....
Methyl bromide
Chloroform
Methyl bromide....
Methyl bromide
Ethylene dioromide.._
Methyl bromide
Chloroform
Bi6(2-ethyfhexyl) pfnfialate...
Di-n-butyt phthalate
Diethyl phthalata ...._
Dimethyf phthalate
•
Di-n-octyl phthalaie....:..._
PhthaHc anhydride (meas-
ured as PnthaJic acid).
.121-14-2
606-20-2
106-93-4
74-83-9
67-66-3
106-93-4
74-83-9
67-66-3
74-83-9
74-83-9
106-93-4
74-83-9
67-66-3
117-81-7
84-74-2
84-66-2
131-11-3
117-84-0
85-44-9
0.11
0.77
0.036
0.057
0.059
0.059
0.039
0.08
0.32
0.028
0.2
0.037
0.059
0.14
0.059
0.068
0.0055
0.059
0.059
0.08
0.32
0.037
0.069
0.069 .
0.32
0.55
0.028
0.11
0.046
0.028
0.11
O.M6
0.11
0.11
0.028
0.11
0.046
0.28
0.057
•
0.2
0.047
0.017
•
0.069
C)
6.2
6.2
NA
14
42
34
3.6
14
22
1.8 '
NA
NA
.3.4
0.071
3.4
3.4
3.4
3.4
3.4
0.65
0.07
NA
28
28
140
28 '•
15
.15
5.6
15
15
5.6
15
15
15
15
5.6
28
28
28
28
28
28
I1)
1 Treatment standards for this organic constituent were established based upon incineration in units operated 'm accordance with the technical requirements of
*0 CFR 264 Subpart O or Part 265 Subpafl 0. or based upon combustion in fuel substitution units operating in accordance with applicable technical requirements. A
facility may certify compliance with mese treatment standards according to provisions in 40 CFR Serfon 268.7. . .
| Based on analysts of composite samples. ' :•
NOTE: NA means Not Applicable.
38. In subpart D. J 26445 with Table 1
is added to read as follows:
§268.45 Treatment standards for
hazardous debris. :
•(a) Treatment standards. Hazardous
debris must be treated prior to land
disposal as follows unless EPA ,
determines under 5 261.3(e)(2) of this
chapter that the debris is no longer
contaminated with hazardous waste or
-------
37278 Federal Register / Vol. 57. No. 160 / Tuesday. August 18, 1992 / Rules and Regulations
the debris is treated to the waste-
specific treatment standard provided in
this subpart for the waste contaminating
the debris:
(1) General. Hazardous debris must be
treated for each "contaminant subject to
treatment" defined by paragraph (b) of
this section using the technology or
technologies identified in Table 1 of this
section.
(2) Characteristic debris. Hazardous
debris that exhibits the characteristic of
ignitability, corrosivity. or reactivity
identified under §§ 261.21. 261.22. and
261.23 of this chapter, respectively, must
be deactivated by treatment using one
of the technologies identified in Table 1
of this section.
(3) Mixtures of debris types. The
treatment standards of Table 1 in this
section must be achieved for each type
of debris contained in a mixture of
debris types. If an immobilization
technology is used in a treatment train,
it must be the last treatment technology-
used.
(4) Mixtures of contaminant types.
Debris that is contaminated with two or
more contaminants subject to treatment
identified under paragraph [b) of this
section must be treated for each
contaminant using one or more
treatment technologies identified in
Table 1 of this section. If an
immobilization technology is used in a
.treatment train, it must be the last
treatment technology used.
(5) Waste PCBs. Hazardous debris
that is also a waste PCB under 40 CFR
part 761 is subject to the requirements of
either 40 CFR part 761 or the
requirements of this section, whichever
are more stringent.
{b) Contaminants subject to
treatment. Hazardous debris must be
treated for each "contaminant subject to
treatment." The contaminants subject to
treatment must be determined as
follows:
(1) Toxicity characteristic debris. The
contaminants subject to treatment for
debris that exhibits the Toxicity
Characteristic (TC) by § 261.24 of this
chapter are those EP constituents for
which the debris exhibits the TC toxicity
characteristic.
(2) Debris contaminated with listed
waste. The contaminants subject to
treatment for debris that is
contaminated with a prohibited listed
hazardous waste are those constituents
for which BOAT standards are
established for the waste under
§§268.41 and 268.43.
(3) Cyanide reactive debris.
Hazardous debris that is reactive
because of cyanide must be treated for
cyanide.
(c) Conditioned exclusion of treated
debris. Hazardous debris that has been
treated using one of the specified
extraction or destruction technologies in
Table 1 of this section and that does not
exhibit a characteristic of hazardous
waste identified under subpart C. part
261. of this chapter after treatment is not
a hazardous waste and need not be
managed in a subtitle C facility.
Hazardous debris contaminated with a
listed waste that is treated by an
immobilization technology, specified in
Table 1 is a hazardous waste and must
be managed in a subtitle C facility.
(d) Treatment residuals—(1) General
. requirements. Except as provided by
.paragraphs (d)(2) and (d)(4) of this
section:
(i) Residue from the treatment of
hazardous debris must be separated
from the treated debris using simple
physical or mechanical means: and
(ii) Residue from the treatment of
hazardous debris is subject to the
waste-specific treatment standards
provided by subpart D of this part for
the waste contaminating the debris.
(2) Nontoxic debris. Residue from the
deactivation of ignitable. corrosive, or
reactive characteristic hazardous debris
(other than cyanide-reactive) that is not
contaminated with a cor.t.aminar.t
subject to treatment defined by
paragraph (b) of this section, must be
deactivated prior to land disposal and is
not subject to the waste-specific
treatment standards of subpart D of this
part.
(3) Cyanide-reactive debris. Residue
from the treatment of debris that is
reactive because of cyanide must meet
the standards for D003 under § 258.43.
(4) Ignitable nonwastewater residue.
Igr.itable nonwastewater residue
containing equal to or greater than IDS
total organic carbon is subject to the
technology-based standards for D001:
"Ignitable Liquids based on
§ 261.21(a)(l)" under § 268.42.
(5) Residue from spoiling. Layers of
debris removed by spelling are
hazardous debris that remain subject to
the treatment standards of this section.
TABLE 1.—ALTERNATIVE TREATMENT STANDARDS FOR HAZARDOUS DEBRIS
Technology description
Performance and/of design and operating standard
Contaminant restrictions :
A. Extraction Technologies:
1. Physical Extraction
a Abrasive Biasing: Removal o( contaminated
debris surface layers using water and,'of air
pressure to propel a solid media (e.g.. steel
shot, aluminum oxide grit plastic beads).
0 Scarifcaicn, Grinding, and Planing: Process
utilizing st/iking pifon heads, saws, or relating
grinding wheels such mat contaminated debris
surface layers are removed.
c. Spa/ling: Drilling or chipping holes at appropriate
locations and depD in tfie contaminated debris
surface and applying a tool which exerts a (ores
on me sides of those hole* such that me sur-
face layer is removed. The surface layer re-
moved remains hazardous debris subject to the
debris treatment standards.
d. Vibratory Finishing: Process utilizing scrubbing
media, flushing fluid, and oscillating energy such
that hazardous contaminants or contaminated
debris surraca layer* ire removed.*
Glass. Metal, Plastic. Rubber Treatment to a dean
debris surface.1
Brick, doth. Concrete. Paper, Pavement. Rock,
Wood: Removal o< at least 0.6 cm of the surface
layer treatment to a clean debris surface.3
Same as above _ „ _
Same as above
Same es above
All Oeons: None.
Same as above.
Same as above.
Same *s above.
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Federal Register / Vol. 57, No. 160 / Tuesday, August -18, 1992 / Rules and Regulations . 37279
TABLE 1.—ALTERNATIVE TREATMENT .STANDARDS FOR HAZARDOUS DEBRIS '—Continued
TechnoiOQy
Perfcrmanoe (nd/or design «nd operating standard
Contaminant restrictions '
e. High Pressure Slaam and Water Spray*: Appf-
cation erf water or steam sprays ol sufficient
.temperature, pressure, residence time, agitation.
surfactants, and detergents to remove hazard-
ous contaminants from debris surfaces or to
remove contaminated debris surface layers.
2. Chemical Extraction
a. Water Washing and Spraying: Application ol
water sprays or water baths of sufficient temper-
ature, pressure. resOencu time, agnation, surfac-
tants, acids, beses, «nd detergents to remove
hazardous contaminants from debris surfaces
and surface pores or to remove contaminated
debris surface layers.
b. Liquid Prjsa Sofrent Emction: fiemoval of
hazardous contaminants from debris surfaces
and surface pores by applying, a nonaoueous
liquid or liquid solution wrich causes the hazard-
ous contaminants to enter me liquid phase and
be flushed away from the debris along with the
Squid or liquid solution while using appropriate
agitation, temperature, and residence time.4
c. Vapor Prase Sotront Extinction: Application ol
an organic vapor using sufficient agitation, resi-
dence time, and temperature to cause hazard-
ous contaminants on contaminated debris sur-
faces and surface pores "to enter the vapor
phase and be flushed sway with the organic
vapor.*
3. Thenral Extrac-ion
a. High Temperature Ue'Als Recovery Appiicason
of sufficient heat, residence one. mixing, fluxing
agents, and/or carbon in a smelting, melting, or
refining furnace to separate metals from debris.
b. Thermal Descrption: Heaing in an enclosed
chamber undo.- either oxidizing or nonoxidizing
atmospheres at suffoent temperature and resi-
dence time to vaporize hazardous contaminants
from contaminated surfaces and surface pores
and to remove the contaminants from the heat-
ing chamber in a gaseous exnausi gas.'
E. Destruction Technologies:
1. Bofacjca/ Destruction (Bodegraoaoon): Remov-
al ol hazardous contaminan'.s from debris sur-
faces and surface pores in an aqueous solution
and biodegration c4 orjarw: or ncomelallic tnor-
ganic compounds fi.e.. rorga.iics trial contain
phosphonjs. nitrogen, or suHuO In units operated
under either serotx or anaerobic conditions.
2. Chemical Destruction
a. Chemical Oxidation: Chemical or electolylJc oxi-
dation utilizing the tcflowing oxidation reagents
(or waste reagents) or comtjination ol rea-
gents—(1) hypochlorite (e.g, bleach); (2) chtc-
rine; (3) chlorine dioxide. (4) ozone or UV (uttra-
vctel light) assisted ozone; (5) peroxide's: (6)
persjilates; (7) perehkxaies; (8) permangan-
ates: and/or (9) ether oxidizing reagents of
equivalent destruction efficiency.4 Chemical oxi-
dation specifically includes what is referred to as
alkaline chlorination.
Same as above
All Debris: Treatment to a dean debris surface;'
S/TC*. Qotfi. Concrete. Paper. Pavement. Roc*.
Wood: Debris must be no more than 1.2 cm (Vi
inch) in one dimension (i.e., thick/ess Imrt,1
except that this thickness Imrt may be waived
under an "Equivalent Technology" approval under
1268.42(6):' debris surfaces must be in contact
with water solution for at leas; 15 mmutes
Same as aDove _ _
Same as above, except that bricX, doth, concrete,
paper, pavement, reck and wood surfaces must be
in contact with the organic vapor tor at least 60
minutes.
For refining furnaces, trea'.ed defcns must be sepa-
ra:ed from treatment residuals usMg simple physi-
cal or mechanical means,1 and, prior to further
feavnent such residuals must meet the waste-
specific treatment sta/xJarcs for organic com-
pounds in the waste comarrmating the debris.
A3 Debris: Obtain an "Eguivalerrt Technology" ap-
proval under j 268.420));' treated flefirts must be
separated from treatment residuals using simple
physical or mechanical means," and, prior to fur-
met treatment, such residue must meet the waste-
specfx: treatment standards tor organic com-
pounds in the waste coniamina'Jng the debris.
fine*. Clotr:, Concrete, Paper. PavemenL Rock.
Wooct Debris must be no more Than 10 cm (4
inches) in one dimension (le.. thickness limit).'
except that this thickness limit may be waived
unoer the "Equivalent Technology approval
At! Debris: Obtain an "Equivalent Technology" ap-
proval under } 268.42(b):' treated debris must be
separated from treatment residuals using simple
physical or mechanical means." and, pnor to fur-
ther treatment, such residue must meet the waste-
specrSc treatment standards tor organic com-
pounds 'n the waste contaminating the debris.
E-ist, CtorA Concrete. Paper. Pavement Roc*.
Wood: Debris must be no mote than \2 cm \Vi
inch) in one dimension fie., thickness kmrt).'
except that this thickness vrii may be waived
under the "Equivalent Technology" approval
All Debris: Obtain an "Equivalent Technology" ap-
proval under $ 268.42(1:):" treated Cetoris must be
separated from treatment residuals using simple
physical or mechanical means," «nd, prior to fur-
ther treatment, joch residue must meet the waste-
specific treatment standards for organic com-
pounds in the waste contaminating the debris.
Bride. Ctotn. Concrete. Paper, Pavement, Rock.
Wood: Debris must be no more than 1.2 cm (Vi
inch) In one dimension (le., thickness limit).'
except that this thickness tnrt may be waived
under the "Equivalent Technology" approval
Same as above.
Brick. Ctotti. Concrete. Psper. Pavement Pock.
Wood: Contaminant musi be soluble to at least
5% by weight in water solution or 5% by weight in
emuisJon; if debris is comaminsied wrth a rJoxin-
bted waste." an "Equrratent Technology" approv-
al under J 268.42
-------
37280 Federal Register / Vol. 57. No. 160 / Tuesday, August 18. 1992 / Rules and Regulations
TABLH 1 .—ALTERNATIVE TREATMENT STANDARDS FOR HAZARDOUS DEBRIS '—Continued
Technology description
Performance and/or design and operating standard
Contaminant restrictions '
b. &&T.IC3I Reduction: Chemical reacion utilizing
the fcllcrg reducing reagents (or waste rea-
gents) or combination ol reagents: (1) su.tur
dioxide: (2) sodium, potassium, or aToii sa!3 ol
sulfites. tasulfiies. and melabisuifites, and pety-
etnyiene gr/tols (e.g.. NaPEG and KrEG): (3)
sodium hydrosulfide; (4) ferrous salts: and/or (5)
otner reding reagents o( equivalent erfeerv
cy.'
3. Thermal Destrjcaon: Treatment in an incinerator
operairjg in accordance with Subpart 0 of Parts
264 or 2i5 ol this chapter a boiler or industrial
furnace ote^ting in accordance with Subpart H
o< Part 256 of mis chapter, or other thermal
treawrrer.t unit operated in accordance with Sub-
pad X, Pn 264 ol this chapter, or S*A?a.l P.
Part 2££ c' rts chapter, but excluding lor pur-
pcsea ol T.ese debris treatment star-cards Ther-
mal Desertion units.
C. im.Tio&'iaron Technologies;
1. MacrxncaffSjladon: Application of surface
coar.ig materials such as polymeric organics
(e.g.. resirs and plastics) or use of a jacket ol
inert inc'c.ar.ic materials to substantially redu»
surface exposure to potential leaching media.
2. kiicf^e^cassu/aoO-f StabiSzation of B"* debris
win tho ,'oilowing reagents (or waste reagents)
such that the teachability ol the hazardous corv
larrenar.a 'a reduced: (1) Portland cement or (21
iime/pccolans (e.g., fly ash and earner! tin
dust). P.eagonis (e.g., iron salts. silicates, and
clays) may be added to enhanca the set/cure
time ar-d/or compressive strengA or to reduce
trie leacr.as«irry of trie hazardous consStue.-ts.*
3. Sealing: Application of an appropriate material
which adheres tightly to the debris surface to
avoent of the
debris su^aca to remove foreign matter and to
clean and roughen the surface. Sealrvg materi-
als induce epoxy. silicooe. and ureihane com-
pounds, cut paint may not be used as a sealant.
Same as above _ _ Same as above.
Treated debris must be separated from treatment
residuals using smple physical or mechanical
means.* and. prior to runner treatment, such resi-
- due must meet the waste-specific treatment stand-
ards for organic compounds in the waste contami-
nating the deor*.
Encapsulai.-ig material must completely encapsulate
debris and be resistant to degradation by the
. debris and its contaminants and materals in;o
which it may come ir.:o contacl after placement
(leacrate. offier waste, microoes).
Leac?iabir,ty of the hazardous contaminants must be
reduced.
Sealing must avoid exposure of the debris surface to
-potential leaching media and sealant must be
resistent to degradation by the debris and its
contaminants and materials into which it may
come into contact after p^rement (leachate. other
waste, microbes).
Brick. Concrete. Gtess. Uatal. Pavement. Roc*.
Metal: Metals other Dan mercury, eicept that
tnere are no metal restrictions for vitrification.
Debris contaminated with a diorin-Ksiad waste.'
Obtain an "Ec'jivalent Technology" approval under
5 268.42(b).§ except that this requirement does net
appry to vitrificaioa
None.
Nor.e.
None.
1 Hazardous debris must be treated by either these standards or the waste-specific t/eatment standards for tt>e waste centaminaUng the debris. The treatment
star^ards must be met for each type of dears contained in a mixture of debrs types, unless the debris is converted into treatment residue as a resu!t ol the
treatment process. [Jeoris treatment resides are subject to the waste-specific t-eatment standards for the waste contaminating the debris.
* Contaminant restriction means that the technology is not BOAT for that contaminant if debris containing a restricted contaminant is treated by the technology.
tne contaminant must be subsecfuenBy treated by a technology lor which it is not restricted in order to be land disposed (and exduded from Subote C regvdation).
3 "Clean debris surface" means the surface, when viewed without magnification, shall be free of all visible contaminated soil and hazardous waste except trial
residual stin^g from sofl and waste consisting of fight shadows, slight streaks, or minor discotorations, and soil and waste in cracks, crevices, and pits may be
present provided that such staining and waste and soil in cracks, crevices, and pits shall be limited to no more than 5% of each souare ir.cn of surface area.
4 Acids, solvents, and chemical reagents may react with some debris and contaminants to form hazardous compounds. For example, acid washing o< cyanide-
contaninatee debris could result in the formation of hydrogen cyanide. Some acids may also react violent!y with some debris and contaminants, deoencrig on the
concentration of the acid and the type ot debris and contaminants. Debris treaters should refer 19 eve safety precautions specrfied in Material Salary Data Sheets for
various acics to avoid applying an incomoastHe acid to a particular decris/contaminant combination. For example, concentrated sutfuric acid may react violency wrai
certain organic compounds, such as acrylonrsiie.
1 If reducing the particle size ol debris to meet the treatment standards results in material that no longer meets the 60 mm minimum particle size limit tor debris.
Such matenal is subject to the waste-specific treatment standards for the waste contaminating the material, unless the debris has been cleaned and separated from
contaminated sort and waste prior to size reduction. At a minimum, simple pnysical or mechanical means must be used to provide such c'eaning and separation ol
roodeoris materials to ensure that the debra surface is free of caked soil, waste, or other nondetoris material.
• OioiirWisted wastes are EPA Hazardous Waste numbers FO20. FO21. FO22. FO23. FD28. and F027.
1 Thermal cesorption is distinguished from Thermal Destruction in that the primary purpose of Thermal Desorpton is to volatilize contaminants arxj to remove
them from tr>o treatment chamber lor subsequent destruction or other treatment.
• The demonstration "Equivalent Technology" under J 263.42(6) must documenl that the technology treats contaminants subject to trsatment to a leva
equivalent to that required by the performance and design and operating standards tor other technologies in this tabia such that residual levels of hazardous
contaminants will not pose a hazard to human hearth and the environment absent management controls.
' Any soil, waste, and other nondebris material that remains on the debris surface (or remains mixed whn the debris) after treatment 'n considered a treatment
residual that must be separated from the debris using, at a minimum, simple physical or mechanical means. Examples of simple physical or mechanical means are
vibratory or trommel screening or water washing. The debris surface need not be cleaned to a "clean, debris surface" as defined in rote 3 when separating treated
debris from residue: rather, the surface must be tree of caked soil, waste, or other nondebris material. Treatment residua's are subject to the waste-specific
treatment standards tor the waste contanv\ating the debris. ,
39. In subpart D, § 268.46 is added to
read as follows:
§ 266.46 Alternative treatment standards
based on KTMR.
Table 1 identifies alternative
treatment standards for F006 and K062 .
nonwaste waters.
-------
Federal Register / Vol. 57, No. 160 / Tuesday, August 18, 1992 / Rnles and Regulations 37281
TABUE 1 .—ALTERNATIVE TREATMENT STANDARDS
Waste
code
F006 -
K062 _
•See also
TsWe CCWE« 268 41 and TatfeCCW »> 26843
Table CCV/E in 268.41 and Table CCW in 268.43
- •
Regulated hazardous constaenl
Artomony
Befyfhrm , , ., _ _., ,, ._.....
Oremknn potai)
Cyanide (mQ/kg) (lotaJ)
Lead
Niriftl
Setenuw .._ .
*>r . .
Zinc _
Antimony «..__„._.„.„ .. ....
A.'!W*T>iC ._ ..
Barium ,. _._
CaoVrwuni .... ..
Loan __...
KJt-knT
Selenium ... .«.........__„. „....„_
Sitvw „ .. .. .......
Ttvdbrt^
frf
CAS No. tor
regutesed
hazardous
constituent .
7440-36-0
7440-38-2
7440-39-3
7440-41-7
7440-43-9
7440-47-32
S7-12-5
7439-92-1
7439-97-6
7440-02-0
7782-49-2
7440-22-4
7440-66-6
7440-36-0
7440-38-2
7440-39-3
7440-41-7
7440-13-g
7440-47-32
7439-92-1
7439-97-6
7440-02-0
7782-49-2
7440-22-1
7440-66-6
rtorv
wasiewaters
ooocc^if a hoft
(mgM)TClP
2.1
0.055
76
0.014
0.19
0.33
1.8
0.37
0.009
5.0
0.16
0.30
0.078
5.3
2.1
0.055
7.6
0014
0.19
0.33
0.37
0009
5.0
0.16
0.30
DOTS
5.3
40. In § 268.50, paragraph (a)(l) and
the introductory text of paragraph (a)(2)
are revised to read as follows:
§ 268.50 Prohibitions on storage of
restricted wastes.
(a) ' ' •
(1) A generator stores such wastes in
tanks, containers, or containment
buildings on-site solely for the purpose
of the accumulation of such quantities of
hazardous waste as necessary to
facilitate proper recovery, treatment, or
disposal and the generator complies
with the requirements in | 262.34 and
parts 264 and 265 of this chapter.
(2) An owner/operator of a hazardous
waste treatment, storage, or disposal
facility stores such wastes in tanks,
containers, or containment buildings
soiely for the purpose of the
accumulation of such quantities of
hazardous waste as necessary to
facilitate proper recovery, treatment, or
disposal and:
• • • • .
-------
TJ
TJ
m
z
o
X
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Appendix III
Associated Design and
Larry Jackson's
TCLP Bench Sheets
and Calculations
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Associated Design and Manufacturing Co.
TCLP Guidelines
Page 1 of 15
Guidelines for the Conduct of the
Toxicity Characteristic Leaching Procedure
These guidelines have been prepared by Associated Design and Manufacturing Company for
the informational use of environmetal professionals engaged in the conduct of the Toxicity
Characteristic Leaching Procedure (TCLP). They are intended to focus attention on important
data collection activities associated with the TCLP. They are for guidance only and are not
intended to replace sound professional judgment or regulatory requirements.
The guidelines are presented in the form of laboratory worksheets that can be used to
document some of the most important points of the procedure. Each worksheet is supported
by a discussion and recommendations of the data that should be recorded to document of the
TCLP. The discussion is keyed to the worksheet for easy reference.
The paragraph references (f x.x.x.x) given in this document refer to the version of the TCLP
which appeared in the July 29, 1990, Federal Register, p. 26986.
MayS, 1993
Revision: 1
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Associated Design and Manufacturing Co.
TCLP Guidelines
Page 2 of 15
TCLP Worksheet No. 1
Sample Description
laboratory Sample No.
Field Sample No.
-*. /ta|& 9*ml|rfiMe -" " " ~ - , - ;v
Number of phases
1. solid
2. liquid
a. lighter than water
b. water
e. heavier than water
8, >«ttfrtSi}!dMu«
1. weight of filter
2. weight of subsample
3. weight of filtrate
4. weight percent solids (wet)'
S. weight percent solids (dry)1
6 volume of initial aqueous filtrate
7. volume of initial organic filtrate
%
* -
••
•• "• ^ x
1. The weight percent wet solids is given by the equation:
weight of subsample - weight of filtrate x^
weight of subsample
2. The weight percent dry solids is given by the equation:
(weight of dry waste + fitter) - weight of filter ^1Q
weight of subsample
May 8, 1993
Revision: 1
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Associated Design and Manufacturing Co.
TCLP Guidelines
Page 3 of 15
Discussion and Recommendations
TCLP Worksheet No. 1
Sample Description
This worksheet documents important information regarding the general description of the
sample and the number of phases observed in the sample as received from the field. This
information is used to determine the amount of leaching fluid used to leach solid materials and
the weighting factors used when calculating final analyte concentrations from multi-phasic
samples.
A. Sample Description
Number of phases -- The number of phases present in the sample determine how the
TCLP is conducted. Solid materials having no visible liquid phase are extracted as
received from the field and the analyte concentration found in the leachate is the reported
value. Liquid materials having no measurable solids content ( < 0.5 wt. % dry solids) are
defined as the TCLP extract (fl 2.1) and are filtered and analyzed directly.
Multi-phase samples must be separated ( f 7.1.1.2) and each phase treated individually.
Aqueous phases may be combined with the leachate from solid phase materials before
analysis if the two aqueous materials are compatible ( H 7.2.13.2). If the two aqueous
materials are not compatible, than each liquid must be analyzed by the appropriate
methods and the results combined numerically to determine the final reported value (
117.2.14).
A.1. Solid - record the visible presence of a solid material heavier than water. If the sample
contains more than one solid phase ( example, wood chips and sediment mixed with
water) record the information in the laboratory notebook.
A.2. Liquid -- record the number of liquid phases observed in the sample according to their
apparent density. It may be impossible to distinguish apparent density if only one liquid
phase is observed and there is no indication on the accompanying chain-of-custody
form (COC). If this is the case, record it as aqueous material and let the subsequent
analytical record show if the liquid is organic after the container is opened at the
appropriate time.
B. Percent of Solid / Liquid Phase(s) -- paragraphs 7.1.1 through 7.1.2.3 of the method
describe the procedure to follow for the determination of the percent solids of the samples.
It is also convenient to measure the percent of any non-miscible liquid phases at this point
because the information is required in
H 7.2.14.
Laboratory subsampling of the material delivered to the laboratory must be thoroughly
documented. The total contents of the sample container should be considered as "the
sample" and care must be taken to ensure the representativeness of any subsample.
May 8, 1993
Revision: 1
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Associated Design and Manufacturing Co.
TCLP Guidelines
Page 4 of 15
Heterogeneous and multi-phasic materials can be difficult to subsample properly and
frequently require significant judgment on the part of the analyst.
Discussion -- At this point, it is important to review the COC and confirm the number of
containers of each sample provided to the laboratory and the types of analyses requested.
If the analysis of volatile components is requested, the determination of percent solids in
multi-phasic samples must be completed before proceeding to the leaching of the solid
material in the zero headspace extractor (ZHE) to prevent overfilling the ZHE. It is best if
a separate sample has been provided for this purpose (] 6.2). The laboratory should
establish an SOP to address how to proceed if only one container is available.
It is common that when more than one container of multi-phasic materials is received from
the field, each container will show different amounts of each phase. This provides a
challenge to the laboratory which must report the data based on percent phase
composition of the sample. A practical solution is to record the depth (measured from
outside the container) of the layers in the each container after the contents have been
allowed to settle and determine the combined volume of each phase in all the containers.
Then measure the phase composition on a single container (after thorough mixing to
obtain a representative subsample). Combine these two sets of values to determine the
correct volume/mass adjustments on the TCLP results.
The laboratory should also establish an SOP on how to proceed when only a limited
amount of sample is available and the analyses requested exceed the amount of sample
provided.
B.1. Weight of filter -- This value must be measured before loading the filter into the filter
holder because the mass of the filter is used in performing the calculation for percent
dry solids.
B.2 Weight of sample aliquote -- a representative 100 gram sample (fl 7.1.1.5) is withdrawn
from the sample container for filtration. If liquid material is decanted from the sample
before subsampling, its volume/weight must be recorded and factored into the
calculations of percent solids.
Discussion - Many multi-phasic samples are difficult to filter. This is especially true of
oily wastes and sludges. The method directs that any material retained by the filter
after following the instructions is defined as solid waste (117,1.18). Experience has
shown that the reproducibility of the percent solids determination with these types of
samples is highly variable. Subsequent steps in the extraction procedure flf 7.2.5 and
7.3.4.2) use the % solids value to estimate the mass of the original waste used to
obtain an appropriate sized subsample of the solid for extraction.
The method directs that the material retained by the filter be dried at 100 ± 20 °C (H
7.1.2.2) to determine the percent dry solids. This may not be achievable for organic
multi-phasic materials because of safety considerations and the fact that many organic
liquids boil considerably higher than water and it may be impossible to achieve a
constant weight for successive weighings (± 1%).
May8, 1993
Revision: 1
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Associated Design and Manufacturing Co.
TCLP Guidelines
Page 5 of 15
The laboratory should establish a standard operating procedure (SOP) addressing
these types of samples. Basically, the laboratory has three choices of how to proceed.
It may
• attempt to dry all samples as directed by the method;
• dry samples containing only water as the liquid phase; and/or
• define the retained material as a dry solid for the purpose of further testing.
This decision may have significant impact on the amount of material selected for leach
testing and on the reported analyte values. The laboratory should consider discussing
this issue with their clients and any regulatory groups to whom the data will be
submitted.
B. 4 Weight percent solids(wet) equals:
weight of subsample - weight of filtrate x "\QO
weight of subsample
The procedure defines the material retained by the filter as the solid phase of the
waste (f 7.1.1.8). This value is used to calculate the volume of the original multi-phasic
material which must be filtered to yield the proper amount of solid waste for the
extraction procedure.
B.5 Weight percent solids (dry) -- the total mass of the filtered solids and the filter are
removed from the filtration apparatus and dried at 100 ± 20 °C until a constant weight
is achieved (If 7.1.2.2). This value is used to calculate the dry solids content of the
waste. Use caution when drying samples that may contain flammable material. It is
important to factor in the tare weight of the filter for samples that have low solids
values.
The weight percent solids (dry) is calculated by the equation:
(weight of dry waste + filter) - weight of filter
weight of subsample
If the weight percent dry solids is > 0.5%, the total waste is defined as a solid waste
and steps must be taken to collect the appropriate weight of solid material for
extraction (1f 7.1.2.4).
B.6 Volume of initial aqueous filtrate -- this value is used in f 7.2.14 and 7.3.14 in the final
calculation of analyte concentration.
B.7 Volume of initial organic filtrate -- this value is used in f 7.2.14 and 7.3.14 in the final
calculation of analyte concentration.
MayS, 1993
Revision: 1
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Associated Design and Manufacturing Co.
TCLP Guidelines
Page 6 of 15
TCLP Worksheet No. 2
Selection of Extraction Fluid
laboratory Sample No.
Fiold Sample No.
''&ti*iM& fe&Mit»M« - ftttttttift3*
1. particle size reduction? yes/no
2. sample weight, / if S.O ± 0.1 grams
3. volume of water, / if 96.5 ± 1.0 ml added
4. initial pH (after S min. mixing time)
5. if pH > 5.0, /if 3.5 ml IN HCI added
6. / if heated and held at 50 "C for ten minutes
7. secondary pH (at room temp.)
'&:$^^tsti^ta: "-" *-: '''''„'-$'.;,
1. /if pH from C.4 or C.7 is < S.O, use
extraction fluid No. 1.
2. / if pH from C.7 is > S.O, use extraction
fluid No. 2
4tt«*>*S>tf$t
' ''
, -. „ "
' /•• ',
titit WW»«^
- ;
t " '"•• "'
'-, ™,
May8. 1993
Revision: 1
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Associated Design and Manufacturing Co.
TCLP Guidelines
Page 7 of 15
Discussion and Recommendations
TCLP Worksheet No. 2
Selection of Extraction Fluid
for
Metals, Semi-volatile Organic Components, and Pesticides/Herbicides
This worksheet documents the important steps which should be followed to correctly
determine the appropriate extraction fluid for leaching solid wastes for the analysis of metals,
semi-volatile organic components, and pesticides/herbicides. This procedure does not apply to
the determination of volatiles using the zero headspace extractor (ZHE).
Discussion -- the Environmental Protection Agency's "worst case" waste disposal model
assumes mismanaged wastes will be co-disposed with municipal solid waste in a 5:95 ratio.
These wastes will be exposed to leaching by the acidic fluids formed in municipal landfills.
The EPA's model further assumes the acid/base characteristics of the waste will be dominated
by the landfill fluids. The TCLP laboratory procedure directs that alkaline wastes be extracted
with a stronger acidic leach fluid than acid or neutral wastes so that the alkaline nature of the
waste will not control the leaching chemistry of the TCLP test. This is in keeping with the
waste disposal model's assumption that the acid fluids in the landfill will dominate leaching
chemistry over time.
The procedure described in U 7.1.4 of the method addresses the determination of the
appropriate extraction fluid. It is a short term test whose results can have a significant impact
of the final analytical results if the wrong extraction fluid is selected. This is especially true for
metals determinations because of their sensitivity to the pH of the leach medium. The
following discussion examines each step of the procedure and points out some sensitive
technical points and how they can affect the results.
H 7.1.4.1 Particle size of test material - The requirement to use 1mm particle size material in
the test recognizes the fact that in a short term reaction between a liquid and a solid, high
surface area is the most important characteristic of the solid. The rate of the reaction is
controlled by the rate of diffusion of the liquid into the pores of the solid so a high surface
area is necessary if the results of a short term test are to be reliable. Therefore, failure to take
a representative subsample of the solid material and perform the necessary particle size
reduction can result in significant bias. This is especially true if the waste contains a wide
range of particle sizes and only the fines are selected for testing.
y 7.1.4.3 Heating of the reaction mixture - The method specifies that the waste/acid slurry is
to be held at 50 °C for ten (10) minutes. Care should be taken to heat the sample to 50 °C as
rapidly as possible without overheating. When the sample has completed the ten minute
period at temperature, it should be allowed to cool and the pH determined as soon as
possible. The longer the reaction between the acid solution and the solid waste is allowed to
continue, the more likely that a falsely high pH reading will result. This will result in improper
selection of the more acidic extraction fluid. Failure to reach and hold the required
temperature can result in an artificially low pH reading for the test solution, leading the
incorrect selection of the less acidic extraction fluid.
May8, 1993
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Associated Design and Manufacturing Co.
TCLP Guidelines
Page8 of 15
C. Extraction Fluid Determination (f 7.1.4)
C.1. Indicate if particle size reduction is required for the sample.
Discussion - the laboratory should consider establishing an SOP to address the
particle size reduction requirements for the TCLP procedure. Most solid samples will
not be received from the field with a particle size of 1mm as required for this step of
the procedure (j 7.1.4.1). Many multi-phasic samples will not be amenable to size
reduction because of the nature of the sample. Samples containing pebbles, rocks, or
debris may be difficult to size reduce if the larger particles are hard. Proper
subsampling of the waste may be difficult if the waste is heterogeneous.
C.2. Sample weight -- check the box if 5.0g of sample is used in the test. Record the
actual weight if a different sized sample is used.
C.3. Volume of water -- the volume of water used in the test is dependant on the weight of
sample being tested. If the sample weight (above) is 5g and 96.5 ml_ of water is
added, check the box. If the weight is not 5g, record the volume of water added.
(# of grams X 19.3mL).
C.4. Initial pH -- record the pH of the slurry after a five minute mixing period. Use narrow
range pH indicator paper if organic material is observed floating on the top of the slurry
to avoid damage to pH electrodes.
C.5. Procedure for alkaline wastes -- if the initial pH of the slurry is > 5.0, add 3.5 ml of 1N
HCI to determine if the alkalinity of the waste is sufficient to require the use of the
stronger acid extraction fluid.
C.6. Neutralization reaction conditions -- the slurry should be heated to 50 °C and held for
ten minutes.The laboratory should consider validating their procedure to confirm these
conditions are met. A bench procedure specifying the hot plate setting (or other source
of heat), the time required to reach the desired temperature, the ten minute time at
temperature, and the time required to return to room temperature should be
established. This will assure the maximum degree of reproducibility in the
determination of the alkaline potential of the wastes tested.
C.7. Secondary pH -- record the pH of the slurry after it has completed the cooling cycle.
D. Selection of Extraction Fluid
D.1. If either the initial pH or the secondary pH is < 5.0, select Extraction Fluid #1 as the
leaching medium.
D.2. If the secondary pH is >5.0, select Extraction Fluid #2 as the leaching medium.
May8, 1993
Revision: 1
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Associated Design and Manufacturing Co.
TCLP Guidelines
Page 9 of 15
TCLP Worksheet No. 3
Determination of Extraction Fluid Volume
for
Metals, Semi-Volatile Organic Components and Pesticides/Herbicides
Laboratory Sample No.
Field Sample No.
L E. Determination of Sample Size lor Leach Testing ~. the melhod requires a minimum 100 ., .
^ ;graro sample,size for extraction (%7J2,5), , x * ; XvX;\
1 . particle size reduction? yes/no
2. amount of dry solids (100g min.)
3. amount of multi-phasic sample1
a. weight of material
b. weight of filtrate
c. weight of solid material
•.-,•.-. v. ..v.-, •.•,•,-.•.;.•. -.^^^s s % •.-.•.'•'I;. -. -, %«, -. •,"•"•-.•,% s ^ -.
F;;-" Determination of Amount of Sxtractfon Fliffcl -» the selection d tie correct extradferi ftjld is
/-found! to SedioaO* WorKsbeel NbA ; '- ;; ^ ;x ,,*_"> -: ^; ^- 5; , —,- , '
1 . for dry solids (20X sample wt.)
2. for multi-phasic samples2
L<ecOHf «l Extraction Test - tte extfaction period is specified as 1^± 2 hours, : 7 ^ s ;v >
1 . extraction start time
2. extraction stop time
3. filtration complete time
4. pH of filtrate
5. volume of filtrate
1. The theoretical amount of multi-phasic waste necessary to yield a 100g sample is given
by:
Amount of multi-phasic material = C\tf)l(wt percent wet solids)
2. The amount of extraction fluid needed to extract the solid material from a filtered multi-
phasic waste is given by:
Amount of extraction fluid - 20 (weight of material filtered - weight of filtra
May 8, 1993
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TCLP Guidelines
Page 10 of 15
Discussion and Recommendations
TCLP Worksheet No. 3
TCLP Extraction Procedure
for
Metals, Semi-volatile Organic Components, and Pesticides/Herbicides
This worksheet documents the performance of the TCLP extraction procedure for metals,
semi-volatile organic compounds and pesticides/herbicides.
E. Determination of Sample Size for Leaching -- the specified size of sample for the leaching
test is a minimum of 100g (U 7.2.5). The regulatory control limit for defining if the waste is
hazardous is based on the levels of analytes reported in the leachate based on this size
sample and a twenty to one (20:1) liquid to solid ratio. If the amount of waste subjected to
extraction is not 100g, than the volume of extraction fluid must be adjusted to preserve the
liquid to solid ratio.
E.1. Amount of dry solids -- record the weight of dry solids.
E.2. Amount of multi-phasic sample ~ the amount of multi-phasic waste material necessary
to produce a 100g sample after filtration can be estimated by the equation:
Amount of multi-phasic material = (]Q*)l(wt percent wet solids)
F. Determination of the Amount of Leaching Fluid
F.1. Dry solids -- for dry solids containing no filtrable fluids, the calculation of the correct
volume of leaching fluid is straightforward. The amount is equal to twenty (20) times
the mass of solid being leached. Note that the method specifies a 20:1 ratio based on
the weight of extraction fluid required (K 7.2.1.1). If the laboratory elects to use
extraction fluid volume, rigorous adherence to the method requires a one time specific
gravity correction to convert the required weight into the appropriate volume.
F.2. Multi-phasic samples -- the method says (U 7.2.11) the percent wet solids can be used
to calculate the weight of extraction fluid used to extract the solid waste resulting from
the filtration of a known weight of multi-phasic waste. The equation for this calculation
is:
Amount of extraction fluid = 0.2 (percent wet solids) (weight of waste filtered)
This assumes there is no subsampling error between the original determination of the
weight percent solid phase (wet) and the subsequent selection of a weight of the multi-
phasic waste for filtration and extraction. This is frequently not so. The nature of many
multi-phasic wastes and/or the necessity to use more than one sample container for
the two determinations means that subsamplng error can be significant. This error can
be eliminated if the actual weight of filtered solids is determined at the time the
material is separated for extraction. The equation for this calculation is:
MayS, 1993
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TCLP Guidelines
Page 11 of 15
Amount of extraction fluid - 20 (weight of material filtered - weight of filtrate)
The actual filtration procedure is detailed in K's 7.2.2 though 7.2.8. Requirements for
sample particle size reduction are given in fl 7.1.3 and 7.2.10. These should be
followed as closely as the nature of the samples will allow and all departures from the
instructions should be described in the laboratory notebook.
G. Record of the TCLP Extraction Test -- the period of the extraction test is given as
18 ± 2 hours (f 7.2.12). Extraction should be started so the resulting slurry can be filtered
as soon as possible after the 18 hours has past. The filtration effectively stops the
extraction process. If the extraction fluid is left in contact with the waste for longer than the
specified period (overnight or over the weekend), the extraction process continues and
may lead to elevated levels of contaminants.
G.1. Extraction start time -- record the time and date the extraction begins.
G.2. Extraction stop time -- record the time and date the extraction is completed.
G.3. Filtration completion time -- record the time and date the filtration is complete.
G.4. pH of filtrate -- while not required by the method, this is a good indicator of test
performance when performing duplicate laboratory analysis or analyzing field
replicates. It can be a reliable measure of sample heterogeneity.
G.5. Volume of filtrate -- record the total volume of filtrate collected from the sample. This
value is required to make the appropriate volume corrections when reporting the
results from multi-phasic wastes.
May8, 1993
Revision: 1
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Associated Design and Manufacturing Co.
TCLP Guidelines
Page 12 of 15
TCLP Worksheet No. 4
Zero Headspace Extraction (ZHE)
Laboratory Sample No.
Field Sample No.
ti •• Detenntoation of Sample Slz« ttwr teach Testing « hjaxirnyin 25 grams
1 . amount of dry solids
2. amount of multi-phasic sample1
; t .O^ie^iR^oiiofAinotjmot^rae^on^lu^No.,15 , \ '
1 . for dry solids (20X sample wt.)
2. for multi-phasic samples2
a. weight of material
b. weight of filtrate
c. weight of solid material
£ Record of SHE Exfcactio** fesl - ths $*fractfcr» perk** is as 18 i 2 houis (f 7&1&3I* ; " ";
1 . extraction start time
2. starting pressure
3. extraction stop time
4. S if positive pressure
5. filtration completion time
6. pH of filtrate
7. volume of filtrate
1 . Determination of amount of multi-phasic sample for extraction:
a. if weight percent dry solids is < 5% (from Worksheet No. 1 , B. 5), the waste is filtered
and the filtrate is defined as the TCLP leachate (\ 7.3.4).
b. if weight percent dry solids is > 5% (from Worksheet No. 1 , B. 5), the amount of multi-
phasic material which should be filtered to yield a 25 gram sample is given by:
Amount of multi-phasic material = (2.5 x
percent dry solids)
2. The amount of extraction fluid #1 needed to extract the solid material from the filtered
multi-phasic waste (H.2) is given by:
Amount of extraction fluid = 20 (weight of material filtered - weight of filtrate)
May 8, 1993
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TCLP Guidelines
Page 13 of 15
Discussion and Recommendations
TCLP Worksheet No. 4
Zero Headspace Extraction
for
Determination of Volatile Organic Compounds
This worksheet describes the important information regarding the conduct of the zero
headspace extraction (ZHE) of solid waste materials for volatile organic compounds.
Samples containing < 5.0 % dry solids are NOT subjected to ZHE leaching procedure. They
are filtered in the ZHE device and the resulting filtrate is defined as the TCLP leachate and
analyzed directly (f 7.3.4).
H. Determination of Sample Size for Leach Testing -- the maximum sample size for this test
is limited by the volume of the ZHE to approximately 25g (f 7.3).
H.1. Amount of dry solids - record the weight of dry solids charged to the ZHE but do not
exceed 25g.
H.2. Amount of multi-phasic sample -- the amount of multi-phasic waste material necessary
to produce a 25g sample after filtration can be estimated by the equation:
Amount of multi-phasic material = (2.5 x l&)l(wt. percent wet solids)
I. Determination of the Amount of Leaching Fluid #1
1.1. Dry solids -- for dry solids containing no filterable fluids, the calculation of the correct
volume of leaching fluid is straightforward. The amount is equal to twenty (20) times
the mass of solid being leached. Note that the method specifies a 20:1 ratio based on
the weight of extraction fluid required (H 7.3.11). If the laboratory elects to use
extraction fluid volume, rigorous adherence to the method requires a one time specific
gravity correction to convert the required weight into the appropriate volume.
I.2. Multi-phasic samples -- the method indicates (f 7.3.11) that the percent wet solids can
be used to calculate the weight of extraction fluid used to extract the solid waste
resulting from the filtration of a known weight of multi-phasic waste. The equation for
this calculation is:
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Associated Design and Manufacturing Co.
TCLP Guidelines
Page 14 of 15
Amount of exaction fluid = * ^°w/7f ** «** ("*** of "***
100
This assumes there is no subsampling error between the original determination of the
weight percent solid phase (wet) and the subsequent selection of a weight of the multi-
phasic waste for filtration and extraction. This is frequently not the case. The nature of
many multi-phasic wastes and/or the necessity to use more than one sample container
for the two determinations means that subsamplng error can be significant. This error
can be eliminated if the actual weight of filtered solids is determined at the time the
material is separated for extraction. The equation for this calculation is:
Amount of extraction fluid = 20 (weight of material filtered - weight of filtrate)
The actual filtration procedure is detailed in fl's 7.3.7 though 7.3.9. Requirements for
sample particle size reduction are given in f 7.3.5 and 7.3.6. These should be followed
as closely as the nature of the samples will allow and all departures from the
instructions should be described in the laboratory notebook.
The addition of extraction fluid #1 to the ZHE is described in detail in fl 7.3.12.
J. Record of the ZHE Extraction Test -- the period of the extraction test is given as
18 ± 2 hours (If 7.3.12.3). Extraction should be started so the resulting slurry can be
filtered as soon as possible after the 18 hours has past. The filtration effectively stops the
extraction process. If the extraction fluid is left in contact with the waste for longer than the
specified extraction period (overnight or over the weekend), the extraction process
continues and may lead to elevated levels of contaminants.
J.1. Extraction start time ~ record the time and date the extraction begins.
J.2. Starting pressure -- the method requires the ZHE be pressurized to approximately 10
psi at the beginning of the test.
J.3. Extraction stop time - record the time and date the extraction is completed.
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Associated Design and Manufacturing Co.
TCLP Guidelines
Page 15 of 15
J.4. Positive final pressure -- the method requires that the ZHE retain positive pressure at
the conclusion of the extraction period or the test must be reported (f 7.3.13). Loss of
pressure is an indication the ZHE leaked during the test resulting in a loss of volatile
components.
J.5. Filtration completion time -- record the time and date the filtration is complete.
J.6. pH of filtrate -- while not required by the method, this is a good indicator of test
performance when performing duplicate laboratory analysis or analyzing field
replicates. It can be a reliable measure of sample heterogeneity.
J.7. Volume of filtrate -- record the total volume of filtrate collected from the sample. This
value is required to make the appropriate volume corrections when reporting the
results from multi-phasic wastes. The filtration of oily wastes may be especially difficult.
May8, 1993
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TJ
•o
m
z
o
X
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Appendix IV
USEPA Region II
Organic, Inorganic and TCLP Data Validation
Methods
-------
SOP NO. H»-7
Revision # 3
TCLP DATA VALIDATION
— M I n lf)?\
Date: / ifo/^ /«* / ' ' /
Toxic and Hazardous Waste Section
BY:
Toxic and Tiazardous Waste Section
CONCURRED BY:
APHROVED BY;
n/ £ihief
Monitoring Management Branch
-------
ALL LAND BAN TCLP ANALYSIS MUST USE SW-846 METHODS.
THIS SOP ONLY APPRAISES THE TCLP EXTRACTION PROCEDURE. TO COMPLETELY VALIDATE A
TCLP ANALYSIS, YOU MUST ALSO USE THE REGION II SOPS FOR ORGANIC AND INORGANIC DATA
VALIDATION.
BEFORE VALIDATING TCLP DATA, THE DATA VALIDATOR MUST DETERMINE IF ANY TOXICTTY
CHAI^CTERISTIC OR IAND BAN REGULATORY ACTION LEVELS ARE APPLICABLE.
YES NO N/A
Was a ZHE vessel used for VOAs? [ ]
Was there any evidence of leakage? [ ]
Action: If a ZHE vessel leaked, or was not used,
reject (R) all VOA data, except data which
exceeds the regulatory level for any analyte.
See attached list for TC regulatory levels.
If other analytes are being validated, the validator
must determine which, if any, Land Ban regulatory
levels are applicable. The Land Ban TCLP
regulatory levels are listed in 40CFR268.
Did the lab use proper bottles? [ ]
Action:" If a plastic bottle was used, except for PTFE,
reject (R) all non detect organic data. All positive
organic values should be flagged as presumptively present
at an estimated quantity (JN).
Did the lab correctly compute % solids? [ ]
Action: If the lab made an error, request revised data.
If appropriate, did the lab reduce particle size? [ ]
Action: If the lab did not perform a required
particle size reduction, reject (R) all non detects.
All positive values should be flagged as
presumptively present at an estimated quantity (JN).
Was the correct extraction fluid used? [ ]
Was the pH of the extraction fluid correct? . [ ]
(4.88-4.98 for fluid #1) (2.83 - 2.93 for
extraction fluid #2)
Action: If the extraction fluid pH was wrong, or the
wrong fluid was used, reject (R) all non detects.
All positive values 'should be flagged as presumptively
present at an estimated quantity (JN).
-1-
-------
YES NO N/A
Was the correct weight of extraction fluid used? [_ ]
Action: If the extraction fluid weight is not +15%
of the correct value, flag all results as estimated (J).
If the extraction fluid weight is more than 30% above
the correct value, reject (R) all non detects, and
flag all positive values as presumptively present at
an estimated quantity (JN).
For volatile analytes, was the sample weight 25
grams or less? [ ]
Action: If the sample weight is more than
25 grains, flag all data as estimated (J).
Were the TCLP extracts properly preserved? [ ]
(Metals must be preserved to a pH <2 with HNOj) .
Action: If the preservative causes precipitation,
the sample should not be preserved, but the sample
should be analyzed as soon as possible after
extraction." The use of organic preservatives is optional.
If proper inorganic preservation .procedures were not
followed, reject (R) all non detects, and flag all
positive values below regulatory action levels as
presumptively present at an estimated quantity (JN).
Positive data at concentrations above regulatory
action levels should not be qualified.
Is there a TCLP blank with the appropriate TCLP [ ]
fluid for every 20 samples? (This is in
addition to the method blanks, which are required
for each analytical method).
Action: If there is no TCLP blank, call laboratory
for explanation/resubmittal. If not available,
reject (R) all associated positive data.
Contaminants in TCLP blanks should be
treated as method blank contaminants when validating
data.
Have samples been analyzed within TCLP holding
times from date of collection ? [ ]
t
NOTE: CLP holding times do not apply to TCLP analysis.
The following table lists TCLP holding times:
-2-
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TCLP Holding Times
TCLP HOLDING
TIMES (DAYS)
VQA
ORGANIC
EXTRACTABLES
MERCURY
OTHER METALS
FROM COLLECTION
TO TCLP EXTRACTION
14
14
28
180
FROM TCLP EXTRACTION
TO PREPARATIVE
EXTRACTION
N/A
7
N/A
N/A
FROM PREPARATIVE
EXTRACTION TO
ANALYSIS
14
40
28
180
HOLDING TIME DECISION TABLE
Have samples been analyzed within TCLP holding time?
If Yes.
Action: Do not qualify data because of holding time.
If- No. " .....
Action: In the sample, does any analyte exceed the regulatory level?
Toxicity Characteristic regulatory action levels are listed on page 5 of this SOP.
The Land Ban regulatory action levels are listed in 40CFR268.
If No.
Action: Reject (R) all
analytes.
If Yes.
Action: Do not qualify
analytes which exceed
regulatory levels.
Mention in data
assessment that
reported value
represents the
minimum concentration
present.
Assume that TCLP analysis of TC analytes is for the purpose of determining
compliance with the TC regulatory levels (attached). If other analytes are being
validated, the validator must determine which, if any, Land Ban regulatory levels
are applicable. ThQ Land Ban TCLP regulatory levels are listed in 40CFR268.
-3-
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ANALYTICAL DATA MUST BE VALIDATED ACCORDING TO THE REGIONAL ORGANIC AND INORGANIC
DATA VALIDATION SOPS BEFORE THE FOLLOWING QUESTIONS MAY BE ADDRESSED.
YES NO N/A
Have any acetates, acetic acid, or acetic anhydride
been reported as TICs? [ ]
Action : If yes, reject (R) TICs.
Are all organic compounds analyzed by the TCLP method
properly calibrated? [ ]
Analytes on Form I that have not been calibrated should
be qualified as follows: non-detects should be
rejected (R); positive values should be reported as
TICs, and flagged "JN".
Have multi-phasic samples been properly analyzed? [ ]
(Check to see if aqueous samples have > .5% solids.)
If not, reject (R) all data below regulatory action
levels.
Have adequate raw data deliverables been submitted? [ ]
Action: If not, contact the laboratory.
If the raw data is not available,
use professional judgement to qualify analytical
data, and mention in data assessment.
Was the method of standard additions properly [ ]
utilized for analysis of metals?
Action: If not, all metals data should be
qualified as estimated "J".
THE FOLLOWING STATEMENT MUST BE ADDED TO ALL TCLP DATA VALIDATION REPORTS:
*
9
Analytical data qualified as "JN" or "R" may not be used to demonstrate compliance
with Toxicity Characteristic or Land Ban Regulations.
-4-
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TC ANALYTES AND THEIR REGULATORY LEVELS
Regulatory
Constituent Level (mcr/1)
benzene
carbon tetrachloride
chlordane
chlorobenzene
chloroform
o-cresol
m-cresol
p-cresol
1 , 4-dichlorobenzene
1 , 2-dichloroethane
1 , 1-dichloroethylene
2 , 4-dinitrotoluene
heptachlor
arsenic
barium
cadmium
chromium
lead
mercury
selenium
0.5
0.5
0.03
100.0
6.0
200.0
200.0
200.0
7.5
0.5
0.7
0.13
0.008
5.0
100.0
1.0
5.0
5.0
0.2
1.0
Constituent
Regulatory
Level (ncr/1)
hexachlorobenzene 0.13
hexachloro-l,3-butadiene 0.5
hexachloroethane 3.0
methyl ethyl ketone 200.0
nitrobenzene 2.0
pentachlorophenol 100.0
pyridine 5.0
tetrachloroethylene 0.7
trichloroethylene 0.5
2,4,5-trichlorophenol 400.0
2,4,6-trichlorophenol 2.0
vinyl chloride 0.2
silver 5.0
endrin " 0.02
lindane 0.4
methoxychlor 10.0
toxaphene 0.5
2,4-D 10.0
2,4,5^TP (silvex) 1.0
-5-
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SOP NO. HW-6
Revision £8
CLP ORGANICS DATA REVIEW
AND PRELIMINARY REVIEW
BY:
Leon Lazarui, Environmental Scientist
Toxi3 and Hazardous Waste Section
BY:
George K^rras, Chemist
Toxic and" Hazardous Waste Section
BY:
Stelios Gerazounfs/' Chemist
Toxic and Hazardotis Waste Section
CONCURRED BY
: KL,:» UjYAD
Date
Date:
Date: I
APPROVED BY:
s Waste Section
Robert RunyonY Ch/ef
Monitoring Management Branch
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
~YESNON/A
PACKAGE COMPLETENESS AND DELIVERABLES
CASE NUMBER: LAB:.
SITE:
1.0 Data Completeness and Deliverables
1.1 Have any missing deliverables been received
and added to the data package? I ]_
ACTION: Call lab for explanation/resubmittal of any
missing deliverables. If lab cannot provide
them, note the effect on review of the
package under the "Contract
Problems/Non-Compliance" section of reviewer
narrative.
1.2 Was SMO CCS checklist included with package? _[ ]_
2.0 Cover Letter SPG Narrative
2.1 Is the Narrative or Cover Letter Present? j; 1
2.2 Are Case Number and/or SAS number contained
in the Narrative or Cover letter? _[ 1
3.0 Data Validation Checklist
The following checklist is divided into three parts.
Part A is filled out if the data package contains any
VGA analyses, Part B for any BNA analyses and Part C
for Pesticide/PCBs.
Does this package contain:
VOA Data?
BNA Data?
Pesticide/PGB data?
Action: Complete corresponding parts of checklist.
- 1 -
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STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
PART A: VOA ANALYSES
1.0 Traffic Reports and Laboratory Narrative
1.1 Are the Traffic Report Forms present for
all samples?
ACTION: If no, contact lab for replacement
of missing or illegible copies.
1.2 Do the Traffic Reports or Lab Narrative
indicate any problems with sample receipt,
condition of samples, analytical problems
or special circumstances affecting the
quality of the data?
ACTION: If any sample analyzed as a soil,
"other than TCLP, contains 50%-90%
water, all data should be flagged as
estimated (J). If a soil sample
other than TCLP contains more than
90% water, all data should be
qualified as unusable (R).
ACTION: If samples were not iced upon
receipt at the laboratory, flaq all
positive results "J" and all Non-
Detects "UJ".
ACTION: If both VOA vials for a .sample have
air bubbles or the VOA vial analyzed
had air bubbles, flag all positive
results "J" and all non-detects "R".
- 2 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YES NO N/A
2.0 Holding Times
2.1 Have any VOA technical holding times,
determined from date of collection to date of
analysis, been exceeded? J 1
If unpreserved, aqueous samples maintained at 4°C which are to
be analyzed for aromatic hydrocarbons must be analyzed within
7 days of collection. If preserved with HCl (pH<2) and stored
at 4°C, then aqueous samples must be analyzed within 14
days of collection. If uncertain about preservation, contact
sampler to determine whether or not samples were preserved.
The holding time for soils is 10 days.
Table of Holding Time Violations
(See Traffic Report)
Sample Sample Date Date Lab Date
ID Matrix Preserved? Sampled Received Analyzed
ACTION: If technical holding times are exceeded, flag all
positive results as estimated ("J") and sample
quantitation limits as estimated ("UJ"), and document in
the narrative that holding times were exceeded. If
analyses were done more than 14 days beyond holding
time, either on the first analysis or upon re-analysis,
the reviewer must use professional judgement to
determine the reliability of the data and the effects of
additional storage on the sample results. At a minimum,
all results must be qualified "J", but the reviewer may
determine that non-detect data are unusable (R). If
holding times are exceeded by more than 28 days, all non
detect data are unusable (R).
- 3 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
3.0 System Monitoring Compound (SMC) Recovery (Form II)
3.1 Are the VOA SMC Recovery Summaries (Form II) present
for each of the following matrices:
a. Low Water J ]_
b. Low Soil _[ 1
c. Med Soil r 1 _
3.2 Are all the VOA samples listed on the appropriate
System Monitoring Compound Recovery Summary for each
of the following matrices:
a. Low Water _[ 1
b. Low Soil _[ 1
c. Med Soil r 1 _
ACTION: Call lab for explanation/
resubmittals. If missing
deliverables are unavailable,
document effect in data assessments.
3.3 Were outliers marked correctly with an
asterisk? _[ 1
ACTION: Circle all outliers in red.
3.4 Was one or more VOA system monitoring
compound recovery outside of contract
specifications for any sample or method
blank? _LJ_
If yes, were samples re-analyzed? _[ 1
Were method blanks re-analyzed?
- 4 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YES ' NON/A
ACTION: If recoveries are > 10% but 1 or
more compounds fail to meet SOW
specifications:
1. All positive results are qualified
as estimated (J).
2. Flag all non-detects as estimated
detection limits ("UJ") where
recovery is less than the lower
acceptance limit.
3. If SMC recoveries are above allowable
levels, do not qualify non-detects.
If any system monitoring compound
recovery is <10% :
1. Flag all positive results as
estimated ("J").
2. Flag all non-detects as unusable"
("R").
Professional judgement should be used to qualify
data that only have method blank SMC recoveries out
of specification in both original and re-analyses.
Check the internal standard areas.
3.5 Are there any transcription/calculation
errors between raw data and Form II? _[ 1
ACTION: If large errors exist, call lab for
explanation/resubmittal, make any
necessary corrections and note
errors in the data assessment.
4.0 Matrix Spikes (Form III)
4.1 Is the Matrix Spike/Matrix Spike Duplicate
Recovery Form (Form III) present? I 1
- 5 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
. YES NO ' N/A
4.2 Were matrix spikes analyzed at the required
frequency for each of the following matrices:
a. Low Water j; 1
b. Low Soil [ ]
c. Med Soil r 1
ACTION: If any matrix spike data are missing, take
the action specified in 3.2 above.
4.3 How many VOA spike recoveries are outside QC
limits?
Water Soils
out of 10 out of 10
4.4 How many RPD's for matrix spike and matrix spike
duplicate recoveries are outside QC limits?
Water Soils
out of 5 out of 5
ACTION: No action is taken based on MS/MSD
data alone. However, using informed
professional judgement, the MS/MSD
results may be used in conjunction
with other QC criteria to determine
the need for qualification of the
data.
5.0 Blanks (Form IV)
5.1 Is the Method Blank Summary (Form IV)
present? I 1
5.2 Frequency of Analysis: for the analysis
of VOA TCL compounds, has a reagent/method
blank been analyzed for each SDG or every
20 samples of similar matrix (low water,
low soil, medium soil), whichever is more
frequent? I ]_
- 6 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
5.3 Has a VOA method/instrument blank been
analyzed at least once every twelve hours for
each concentration level and GC/MS system
used?
ACTION: If any method blank data are missing, call
lab for explanation/ resubmittal. If
method blank data are not available,
reject (R) all associated positive data.
However, using professional judgement, the
data reviewer may substitute field blank
or trip blank data for missing method
blank data.
5.4 Chromatography: review the blank raw data -
chromatograms (RICs), quant reports or data system
printouts and spectra.
Is the chromatographic performance (baseline
stability) for each instrument acceptable
for VOAs? r 1
ACTION: Use professional judgement to
determine the effect on the data.
6.0
NOTE:
6.1
Contamination
"Water blanks", "drill blanks", and distilled water
blanks" are validated like any other sample, and are
not used to qualify data. Do not confuse them with
the other QC blanks discussed below.
Do any method/instrument/reagent blanks have
positive results (TCL and/or TIC) for VOAs?
When applied as described below, the
contaminant concentration in these blanks are
multiplied by the sample dilution factor and
corrected for % moisture when necessary.
6.2
ACTION:
Do any field/trip/rinse blanks have positive
VOA results (TCL and/or TIC)?
*
Prepare a list of the samples associated with
each of the contaminated blanks. (Attach a
separate sheet.)
- 7 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
NOTE: All field blank results associated to a particular
group of samples (may 'exceed one per case) must be
used to qualify data. Trip blanks are used to
qualify only those samples with which they were
shipped and are not required for non-aqueous
matrices. Blanks may not be qualified because of
contamination in another blank. Field Blanks & Trip
Blanks must be qualified for system monitoring
compound, instrument performance criteria, spectral
or calibration QC problems.
ACTION: Follow the directions in the table below to qualify
TCL results due to contamination. Use the largest
value from all the associated blanks. If any blanks
are grossly contaminated, all associated data should
be qualified as unusable (R).
Sample cone > CRQL
but < lOx blank
value
Sample cone < CRQL'
& <10x blank value
Sample cone > CRQL
& >10x blank value
Methylene
Chloride Flag sample result
Acetone with a "U;
Toluene
2-Butanone
Report CRQL &
qualify "U"
No qualification
is needed
Sample cone > CRQL Sample cone < CRQL & Sample cone > CRQL
but < 5x blank is < 5x blank value value & > 5x blank
value
Other
Contam-
inants
Flag sample result Report CRQL &
with a "U" qualify »U"
No qualification
is needed
NOTE: Analytes qualified "U" for blank contamination are
still considered as "hits" when qualifying for
calibration criteria.
- 8 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
~. YESNON/A
ACTION:
6.3
ACTION:
7.0
7.1
7.2
7.3
For TIC compounds, if the concentration in the
sample is less than five times the concentration in
the most contaminated associated blank, flag the
sample data "R" (unusable).
Are there field/rinse/equipment blanks
associated with every sample?
.L_L
For low level samples, note in data assessment that
there is no associated field/rinse/equipment blank.
Exception: samples taken from a drinking water tap
do not have associated field blanks.
GC/MS Instrument Performance Check (Form V)
Are the GC/MS Instrument Performance Check
Forms (Form V) present for Bromofluorobenzene
-(BFB)? . . L_L .
Are the enhanced bar graph spectrum and
mass/charge (m/z) listing for the BFB
provided for each twelve hour shift?
L_L
Has an instrument performance compound been
analyzed for every twelve hours of sample
analysis per instrument? I ]_
- 9 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
ACTION: List date, time, instrument ID, and
sample analysis for which no
associated GC/MS tuning data are
available.
DATE TIME INSTRUMENT SAMPLE NUMBERS
ACTION: If lab cannot provide missing data, reject ("R") all
data generated outside an acceptable twelve hour
calibration interval.
7.4 Have the ion abundances been normalized to
m/z 95? r 1 _
ACTION: If mass assignment is in error,
qualify all associated data as
unusable (R).
7.5 Have the ion abundance criteria been met for
each instrument used? J 1 _
ACTION: List all data which do not meet ion
abundance criteria (attach a
separate sheet).
ACTION: If ion abundance criteria are not
met, the Region II TPO must
be notified.
7.6 Are there any transcription/calculation errors
between mass lists and Form Vs? (Check at least
two values but if errors are found, check
more.) I 1
- 10 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
7.7 Have the appropriate number of significant
figures (two) been reported?
ACTION: If large errors exist, call lab for
explanation/resubmittal, make
necessary corrections and document
effect in data assessments.
7.8 Are the spectra of the mass calibration
compound acceptable?
ACTION: Use professional judgement to
determine whether associated data
should be accepted, qualified, or
rejected.
8.0 Target Compound List (TCP Analytes
8.1 Are the Organic Analysis Data Sheets (Form I VOA)
present with required header information on each
page, for each of the following:
a. Samples and/or fractions as appropriate _[ ]_
b. Matrix spikes and matrix spike
duplicates _[ 1
c. Blanks _[ 1
8.2 Are the VOA Reconstructed Ion Chromatograms, the
mass spectra for the identified compounds, and the
data system printouts (Quant Reports) included in
the sample package for each of the following?
a. Samples and/or fractions as appropriate I 1
b. Matrix spikes and matrix spike
duplicates (Mass spectra not required) _[ 1
c. Blanks _[ 1
f
ACTION: If any data are missing, take action
specified in 3.2 above.
- 11 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
. YESNON/A
8.3 Are the response factors shown in the Quant
Report?
8.4 Is chromatographic performance acceptable with
respect to:
Baseline stability? _[ 1
Resolution? I ]_
Peak shape? r 1
Full-scale graph (attenuation)? j; ]_
Other: f 1
ACTION: Use professional judgement to
determine the acceptability of the
data.
8.5 Are the lab-generated standard mass spectra
of the identified VOA compounds present for
each sample? I 1
ACTION: If any mass spectra are missing,
take action specified in 3.2 above.
If lab does not generate their own
standard spectra, make note in
"Contract Problems/Non-compliance".
8.6 Is the RRT of each reported compound within
0.06 RRT units of the standard RRT in the
continuing calibration? S. 1
8.7 Are all ions present in the standard mass
spectrum at a relative intensity greater
than 10% also present in the sample mass
spectrum? S. 1
- 12 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
. YESNON/A
8.8 Do sample and standard relative ion
intensities agree within 20%? _[ 1
ACTION: Use professional judgement to
determine acceptability of data. If
it is determined that incorrect
identifications were made, all such
data should be rejected (R), flagged
"N" (presumptive evidence of the
presence of the compound) or changed
to not detected (U) at the
calculated detection limit. In
order to be positively identified,
the data must comply with the
criteria listed in 8.6, 8.7, and 8.8.
ACTION: When sample carry-over is a
possibility, professional judgement
should be used to determine if
instrument cross-contamination has
affected any positive compound
identification.
9.0 Tentatively Identified Compounds (TIC)
9.1 Are all Tentatively Identified Compound Forms
(Form I Part B) present; and do listed TICs
include scan number or retention time,
estimated concentration and "JN" qualifier? _[ 1
9.2 Are the mass spectra for the tentatively identified
compounds and associated "best match" spectra
included in the sample package for each of the
following:
a. Samples and/or fractions as appropriate J 1
b. Blanks f 1
ACTION: ,If any TIC data are missing, take
•action specified in 3.2 above.
ACTION: Add "JN" qualifier if missing.
- 13 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
9.3 Are any TCL compounds (from any fraction)
listed as TIC compounds (example: 1,2-
dimethylbenzene is xylene- a VOA TCL
analyte - and should not be reported as a TIC)? _[ 1
ACTION: Flag with "R" any TCL compound
listed as a TIC.
9.4 Are all ions present in the reference mass
spectrum with a relative intensity greater
than 10% also present in the sample mass
spectrum? J[ ]_
9.5 Do TIC and "best match" standard relative
ion intensities agree within 20%? j; ]_
ACTION: Use professional judgement to
determine acceptability of TIC
identifications. If it is
determined that an incorrect
identification was made, change
identification to "unknown" or to
some less specific identification
(example: "C3 substituted benzene")
as appropriate.
Also, when a compound is not found
in any blank, .but is detected in a
sample and is a suspected artifact
of a common laboratory contaminant,
the result should be qualified as
unusable (R)'. (i.e. Common Lab
Contaminants: C02 (M/E 44),
Siloxanes (M/E 73) Hexane, Aldol
Condensation Products, Solvent
Preservatives, and related by
products - see Functional Guidelines
for more guidance).
- 14 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
10.0 Compound Quantitation and Reported Detection
Limits
10.1 Are there any transcription/calculation
errors in Form I results? Check at least two
positive values. Verify that the correct
internal standard, quantitation ion, and RRF
were used to calculate Form I result. Were
any errors found?
10.2 Are the CRQLs adjusted to reflect sample
dilutions and, for soils, sample moisture?
ACTION: If errors are large, call lab for
explanation/resubmittal, make any
necessary corrections and note errors
under "Conclusions".
ACTION: When a sample is analyzed at more than one
dilution, the lowest CRQLs are used
(unless a QC exceedance dictates the use
of the higher CRQL data from the diluted
sample analysis). Replace concentrations
that exceed the calibration range in the
original analysis by crossing out the "E"
and its associated value on the original
Form I and substituting the data from the
analysis of the diluted sample. Specify
which Form I is to be used, then draw a
red "X" across the entire page of all Form
I's that should not be used, including any
in the summary package.
11.0 Standards Data (GC/MS)
11.1 Are the Reconstructed Ion Chromatograras,
and data system printouts (Quant. Reports)
present for initial and continuing
calibration?
ACTION: .If any calibration standard data are
'missing, take action specified in
3.2 above.
.L-l
- 15 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
12.0 GC/MS Initial Calibration (Form VI)
12.1 Are the Initial Calibration Forms (Form VI)
present and complete for the volatile
fraction at concentrations of 10, 20,
50, 100, 200 ug/1? Are there separate
calibrations for low water/med soils
and low soil samples?
ACTION: If any calibration standard forms are missing, take
action specified in 3.2 above.
12.2 Were all low level soil standards, blanks
and samples analyzed by heated purge? J 1 _
ACTION: If low level soil samples were not heated during
purge, qualify positive hits "J" and non-detects "R"
12.3 Are response factors stable for VGA's
over the concentration range of the
calibration (%Relative Standard Deviation
(%RSD) <30.0% )? f 1 _
ACTION: Circle all outliers in red.
NOTE: Although 11 VOA compounds have a minimum
RRF and no maximum %RSD, the technical
criteria are the same for all analytes.
ACTION: If %RSD > 30.0%, qualify-associated positive
results for that analyte "J" and non-detects
using professional judgement.. When RSD > 90%,
flag all non-detects for that analyte R (unusable)
NOTE: Analytes previously qualified "U" for blank
contamination are still considered as "hits"
when qualifying for initial calibration
criteria.
12.4 Are the RRFs above 0.05?
Action: Circle all outliers in red.
Action: If any RRF are < 0.05, qualify associated
non-detects (R) and flag associated positive
data as estimated (J).
- 16 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
12.5 Are there any transcription/calculation errors
in the reporting of average response factors
(RRF) or %RSD? (Check at least 2 values, but
if errors are found, check more.) _[ 1
13.0 GC/MS Continuing Calibration (Form VII)
13.1 Are the Continuing Calibration Forms
(Form VII) present and complete for the
volatile fraction?
13.2 Has a continuing calibration standard
been analyzed for every twelve hours of
sample analysis per instrument? _[ 1
ACTION: List below all sample analyses that
were not within twelve hours of the
previous continui-ng calibration
analysis.
ACTION: If any forms are missing or no continuing
calibration standard has been analyzed within twelve
hours of every sample analysis, call lab for
explanation/resubmittal. If continuing calibration
data are not available, flag all associated sample
data as unusable ("R").
13.3 Do any volatile compounds have a % Difference
(% D) between the initial and continuing
RRF which exceeds the + 25% criteria? _[ 1
ACTION: Circle all outliers in red.
ACTION: ,Qualify both positive results and
'non-detects for the outlier compound(s)
as estimated. When % D is above 90%, reject
all non-detects for that analyte (R) unusable.
- 17 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
13.4 Do any volatile compounds have a RRF <0.05? I 1
ACTION: Circle all outliers in red.
ACTION: If the RRF <0.05, qualify associated
non-detects as unusable (R) and "J"
associated positive values.
13.5 Are there any transcription/calculation
errors in the reporting of average response
factors (RRF) or %difference (%D) between
initial and continuing RRFs? (Check at least
two values but if errors are found,
check more.) I 1
ACTION: Circle errors in red.
ACTION: If errors are large, call lab for
explanation/resubmittal, make any
necessary corrections and note
errors under "Conclusions".
14.0 Internal Standard (Form VIII)
14.1 Are the internal standard areas (Form VIII)
of every sample and blank within the upper
and lower limits (-50% to + 100%) for each
continuing calibration? _[ 1
ACTION: List all the outliers below.
Sample % Internal Std Area Lower Limit Upper Limit
(Attach additional sheets if necessary.)
- 18 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
. YESNON/A
ACTION: 1. If the internal standard area count
is outside the upper or lower limit,
flag with "J" all positive results
quantitated with this internal standard.
2. Non-detects associated with IS area counts
> 100% should not be qualified.
3. If IS area is below the lower limit
(< 50%), qualify all associated non-
detects (U values) "J". If extremely
low area counts are reported, (< 25%)
or if performance exhibits a major
abrupt drop off, flag all associated
non-detects as unusable ("R").
14.2 Are the retention times of the internal
standards within 30 seconds of the
associated calibration standard? j; ]_
ACTION: Professional judgement should be
used to qualify data if the
retention times differ by more than
30 seconds.
15.0 Field Duplicates
15.1 Were any field duplicates submitted for
VGA analysis? r 1
ACTION: Compare the reported results for
field duplicates and calculate
the relative percent difference.
ACTION: Any gross variation between
duplicate results must be addressed
in the reviewer narrative. However,
if large differences exist,
,identification of field duplicates
'should be confirmed by contacting
the sampler.
- 19 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
PART B: BNA ANALYSES
1.0 Traffic Reports and Laboratory Narrative
1.1 Are the Traffic Report Forms present for all
samples? _[ ]_
ACTION: If no, contact lab for replacement of
missing or illegible copies.
1.2 Do the Traffic Reports or Lab Narrative
indicate any problems with sample receipt,
condition of samples, analytical problems or
special notations affecting the quality of
the data? f 1
ACTION: If any sample analyzed as a soil, other
than TCLP, contains 50%-90% water,
all data should be flagged as estimated
("J"). If a soil sample, other than TCLP,
contains more than 90% water, all data
should be qualified as unusable (R) .
\
ACTION: If samples were not iced upon receipt at
the laboratory, flag all positive results
"J" and all non-detects "UJ".
2.0 Holding Times
2.1 Have any BNA technical holding times,
determined from date of collection to date of
extraction, been exceeded? _[ ]_
Continuous extraction of water samples for
BNA analysis must be started within seven
days of the date of collection. Soil/
sediment samples must be extracted within
7 days of collection. Extracts must be
analyzed within 40 days of the date of
extraction.
- 20 -
-------
Date: January 1992
Revision: 8
YES NO N/A
Table of Holding Time Violations
(See Traffic Report)
Sample Date Date Lab Date Date
Sample Matrix Sampled Received Extracted Analyzed
ACTION: If technical holding times are exceeded,
flag all positive results as estimated
("J") and sample quantitation limits
as estimated ("UJ"), and document in
the narrative that holding times were
exceeded.
If analyses were done more than 14 days beyond
holding time, either on the first analysis or
upon reanalysis, the reviewer must use
professional judgement to determine the
reliability of the data and the effects of
additional storage on the sample results.
At a minimum, all results should be qualified
"J", but the reviewer may determine that non-detect
data are unusable ("R"). If holding times are exceeded by
more than 28 days, all non detect data are unusable (R).
3.0 Surrogate Recovery (Form II)
3.1 Are the BNA Surrogate Recovery Summaries
(Form II) present for each of the following
matrices:
a. Low Water I 1
b. Low Soil _[ 1
0
c. Med Soil r 1
- 21 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
3.2 Are all the BNA samples listed on the
appropriate Surrogate Recovery Summaries
for each of the following matrices:
a. Low Water _[ ]_
b. Low Soil _[ 1
c. Low Soil _[ 1
ACTION: Call lab for explanation/resubmittals.
If missing deliverables are unavailable,
document effect in data assessments.
3.3 Were outliers marked correctly with an
asterisk? r 1
ACTION: Circle all outliers in red.
3.4 Were two or more base-neutral OR acid surrogate
recoveries out of specification for any sample
or method blank? " ' ~ j; 1
If yes, were samples reanalyzed? _[ ]_
Were method blanks reanalyzed?
ACTION: If all BNA surrogate recoveries are
> 10% but two within the base-neutral
or acid fraction do not meet SOW
specifications, for the affected
fraction only (i.e. base-neutral or
acid compounds):
1. Flag all positive results as estimated
("J").
2. Flag all non-detects as estimated
detection limits ("UJ") when recoveries
are less than the lower acceptance limit.
3. If recoveries are greater than the upper
acceptance limit, do not qualify non-detects.
- 22 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
If any base-neutral or acid surrogate has a
recovery of <10%:
1. Positive results for the fraction with
<10% surrogate recovery are qualified
with "J".
2. Non-detects for that fraction should be
qualified as unusable (R) .
Professional judgement should be used to qualify
data that have method blank surrogate recoveries
out of specification in both original and
reanalyses. Check the internal standard areas.
3.5 Are there any transcription/calculation errors
between raw data and Form II? [ 1
ACTION: If large errors exist, call lab for
explanation/resubmittal, make any
necessary corrections and document effect
in data assessments.
4.0 Matrix Spikes (Form III)
4.1 Is the Matrix Spike/Matrix Spike Duplicate
Recovery Form (Form III) present? _[ 1_
4.2 Were matrix spikes analyzed at the required
frequency for each of the following matrices:
a. Low Water I ]_
b. Low Soil I 1
c. Med Soil r 1
ACTION: If any matrix spike data are missing,
take the action specified in 3.2 above,
- 23 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YES NO N/A
4.3 How many BNA spike recoveries are outside
QC limits?
Water „ Soils
out of 22 out of 22
4.4 How many RPD's for matrix spike and matrix
spike duplicate recoveries are outside QC
limits?
Water Soils
out of 11 out of 11
ACTION: No action is taken on MS/MSD data
alone. However, using informed
professional judgement, the data
reviewer may use the matrix spike and
matrix spike duplicate results in
conjunction with other QC criteria and
determine the need for some
qualification of the data.
5.0 Blanks (Form IV)
5.1 Is the Method Blank Summary (Form IV) present? J 1
5.2 Frequency of Analysis:
Has a reagent/method blank analysis been
reported per 20 samples of similar matrix,
or concentration level, and for each extraction
batch? r 1
5.3 Has a BNA method blank been analyzed for
each GC/MS system used? I 1
(See SOW p. D - 59/SV, Section 8.7)
ACTION: If any method blank data are missing,
call lab for explanation/resubmittal.
If not available, use professional
judgement to determine if the associated
sample data should be qualified.
- 24 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
5.4 Chromatography: review the blank raw data -
chromatograms (RICs), quant reports or data
system printouts and spectra."
Is the chromatographic performance•(baseline
stability) for each instrument acceptable for
BNAs? r 1
ACTION: Use professional judgement to determine
the effect on the data.
6.0 Contamination
Note: "Water blanks", "drill blanks" and
"distilled water blanks" are validated
like any other sample and are not used
to qualify the data. Do not confuse them
with the other QC blanks discussed below.
6.1 Do any method/instrument/reagent blanks have
positive results (TCL and/or TIC) for BNAs?
When applied as described below, the
contaminant concentration in these blanks -are
multiplied by the sample dilution factor and
corrected for % moisture where necessary. .T l_
6.2 Do any field/rinse/ blanks have positive
BNA results (TCL and/or TIC)? r 1
ACTION: Prepare a list of the samples associated
with each of the contaminated blanks.
(Attach a separate sheet.)
Note: All field blank results associated to
a particular group of samples (may
exceed one per case) must be used to
qualify data. Blanks may not
be qualified because of contamination
in another blank . Field Blanks must be
qualified for surrogate, spectral, instrument
performance or calibration QC problems.
- 25 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
ACTION: Follow the directions in the table
below to qualify TCL "results due to
contamination. Use the largest value
from all the associated blanks. If
gross contamination exists, all data .
in the associated samples should be qualified
as unusable (R).
Sample cone > CRQL Sample cone CRQL
but < lOx blank is< lOx blank value value & >10x blank
Common Phthalate Esters
Flag sample result Report CRQL & No qualification
with a "U"; qualify "U" is needed
Sample cone > CRQL Sample cone < CRQL & Sample cone > CRQL
but < 5x blank is < 5x blank value value & >5 blank value
Other Co'ntaminants " ." "
Flag sample result Report CRQL & No qualification
with a "U"; qualify "U" is needed
NOTE: Analytes qualified "U" for blank contamination
are still considered as "hits" when qualifying
for calibration criteria.
ACTION: For TIC compounds, if the
concentration in the sample is less
than five times the concentration in
the most contaminated associated blank,
flag the sample data "R" (unusable).
6.3 Are there field/rinse/equipment blanks
associated with every sample?
ACTION: For low level samples, note in data
assessment that there is no associated
field/rinse/equipment blank. Exception:
samples taken from a drinking water tap
.'do not have associated field blanks.
- 26 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNO N/A
7.0 GC/MS Instrument Performance Check
7.1 Are the GC/MS Instrument Performance Check Forms
(Form V) present for Decafluorotriphenylphosphine
(DFTPP)? f 1
7.2 Are the enhanced bar graph spectrum and mass/
charge (m/z) listing for the DFTPP provided for
each twelve hour shift? j; 1
7.3 Has an instrument performance check solution
been analyzed for every twelve hours of sample
analysis per instrument? _[ 1
ACTION: List date, time, instrument ID, and
sample analyses for which no
associated GC/MS tuning data are
available.
DATE TIME INSTRUMENT SAMPLE NUMBERS
ACTION: If lab cannot provide missing data,
reject ("R") all data generated outside
an acceptable twelve hour calibration
interval.
ACTION: If mass assignment is in error, flag all
associated sample data as unusable (R).
7.4 Have the ion abundances been normalized to m/z
198? r 1
- 27 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
7.5 Have the ion abundance criteria been met .for
each instrument used? , " _[ ]_
ACTION: List all data which do not meet ion
abundance criteria (attach a separate
sheet).
ACTION: If ion abundance criteria are not
met, the Region II TPO must
be notified.
7.6 Are there any transcription/calculation errors
between mass lists and Form Vs? (Check at least
two values but if errors are found, check more.) j; 1
7.7 Have the appropriate number of significant
figures (two) been reported? _[ ]_
ACTION: If large errors exist, call lab for
explanation/resubmittal, make
necessary corrections and document effect
in data assessments.
7.8 Are the spectra of the mass calibration compound
acceptable? J ]_
ACTION: Use professional judgement to determine
whether associated data should be
accepted, qualified, or rejected.
8.0 Target Compound List (TCP Analytes
8.1 Are the Organic Analysis Data Sheets (Form I BNA)
present with required header information on each
page, for each of the following:
a. Samples and/or fractions as appropriate _[ ]_
b. Matrix spikes and matrix spike duplicates _[ 1
c. Blanks j; 1
- 28 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNO N/A
8.2 Has GPC cleanup been performed on all soil/
sediment sample extracts? _[ 1
ACTION: If data suggests that GPC was not
performed, use professional judgement.
Make note in "Contract
Problems/Non-Compliance".
8.3 Are the BNA Reconstructed Ion Chromatograms,
the mass spectra for the identified compounds,
and the data system printouts (Quant Reports)
included in the sample package for each of the
following?
a. Samples and/or fractions as appropriate I ]_
b. Matrix spikes and matrix spike duplicates
(Mass spectra not required) I ]_
c. Blanks j; ]_
ACTION: If any data are missing, take action
specified in 3.2 above.
8.4 Are the response factors shown in the Quant
Report? r 1
8.5 Is chromatographic performance acceptable with
respect to:
Baseline stability? _[ ]_
Resolution?
Peak shape?
Full-scale graph (attenuation)? j; 1
Other: r 1
ACTION: Use professional judgement to determine
the acceptability of the data.
- 29 -
-------
Date: January 1992
Revision: 8
YES NO N/A
8.6 Are the lab-generated standard mass spectra of
identified BNA-compounds present for each
sample?
ACTION: If any mass spectra are missing, take
action specified in 3.2 above. If lab
does not generate their own standard
spectra, make note in "Contract Problems/
Non-compliance". If spectra are missing,
reject all positive data.
8.7 Is the RRT of each reported compound within 0.06
RRT units of the standard RRT in the continuing
calibration? . _[ 1
8.8 Are all ions present in the standard mass
spectrum at a relative intensity greater than
10% also present in the sample mass spectrum?
8.9 Do sample and standard relative ion intensities
agree within 20%?
9.0
ACTION: Use professional judgement to determine
acceptability of data. If it is
determined that incorrect identifications
were made, all such data should be
rejected (R), flagged "N" (Presumptive
evidence of the presence of the compound)
or changed to not detected (U) at
the calculated detection limit. In order
to be positively identified, the data
must comply with the criteria listed in
8.7, 8.8, and 8.9.
ACTION: When sample carry-over is a possibility,
professional judgement should be used to
determine if instrument cross-contamination
has affected any positive compound
identification.
Tentatively Identified Compounds (TIC)
9.1 Are all Tentatively Identified Compound Forms
(Form I, Part B) present; and do listed TICs
include scan number or retention time, estimated
concentration and "JN" qualifier?
- 30 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
9.2 Are the mass spectra for the tentatively
identified compounds and associated "best match"
spectra included in the sample package for each
of the following:
a. Samples and/or fractions as appropriate _[ ]_
b. Blanks . _[ 1
ACTION: If any TIC data are missing, take
action specified in 3.2 above.
ACTION: Add "JN" qualifier if missing.
9.3 Are any TCL compounds (from any fraction) listed
as TIC compounds (example: 1,2-dimethylbenzene is
xylene a VOA TCL - and should not be reported as
a TIC)? r 1
ACTION: Flag with "R" any TCL compound
listed as a TIC.
9.4" Are all ions present in the reference mass
spectrum with a relative intensity greater than
10% also present in the sample mass spectrum? _[ ]_
9.5 Do TIC and "best match" standard relative ion
intensities agree within 20%? _[ ]_
ACTION: Use professional judgement to
determine acceptability of TIC
identifications. If it is determined
that an incorrect identification
was made, change identification to
"unknown" or to some less specific
identification (example: "C3
substituted benzene") as appropriate.
Also, when a compound is not found in
any blank, but is a suspected artifact
of a common laboratory contaminant, the
result should be qualified as unusable
(R).
- 31 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
10.0 Compound Ouantitation•and Reported Detection Limits
10.1 Are there any transcription/calculation errors in
Form I results? Check at least two positive values.
Verify that the correct internal standard,
quantitation ion, and RRF were used to calculate
Form I result. Were any errors found?
10.2 Are the CRQLs adjusted to reflect sample
dilutions and, for soils, sample moisture? j; ]_
ACTION: If errors are large, call lab for
explanation/resubmittal, -make any
necessary corrections and document
effect in data assessments.
ACTION: When a sample is analyzed at more
than one dilution, the lowest CRQLs
are used (unless a QC exceedance
dictates the use of the higher CRQL
data from the diluted sample analysis).
Replace concentrations that exceed the
calibration range in "the original
analysis by crossing out the "E" and it's
associated value on the original Form I
and substituting the data from the analysis
of the diluted sample. Specify which Form I
is to be used, then draw a red " X" across
the entire page of all Form I's that should
not be used, including any in the summary
package.
11.0 Standards Data (GC/MS^
11.1 Are the Reconstructed Ion Chromatograms, and
data system printouts (Quant, Reports) present
for initial and continuing calibration? J 1
ACTION: If any calibration standard data
are missing, take action specified
in 3.2 above.
- 32 -
-------
STANDARD OPERATING
Date: January 1992
Revision: 8
YESNON/A
12.0 GC/MS Initial Calibration (Form VI)
12.1 Are the Initial Calibration Forms (Form VI)
present and complete for the -BNA fraction? j; 1
ACTION: If any calibration standard forms
are missing, take action specified
in 3.2 above.
12.2 Are response factors stable for BNAs over
the concentration range of the calibration?
(% Relative standard deviation (%RSD) < 30.0%) r 1
ACTION: Circle all outliers in red.
NOTE: Although 20 BNA compounds have a minimum
RRF and no maximum %RSD, the technical
criteria are the same for all analytes.
ACTION: If the % RSD is > 30.0%, qualify
positive results for that analyte "J"
and non-detects using professional
judgement. When RSD >'90%, flag all non-
detect results for that analyte R (unusable)
NOTE: Analytes previously qualified "U" due to
blank contamination are still considered
as "hits" when qualifying for calibration
criteria.
12.3 Are all BNA compound RRFs > 0.05? f 1
ACTION: Circle all outliers in red.
ACTION: If any RRF < 0.05
1. "R" all non-detects.
2. "J" all positive results.
12.4 Are there any transcription/calculation errors in
the reporting of average response factors (RRF)
or % RSD? (Check at least two values but if errors
are found, check more.) I 1
ACTION: Circle Errors in red.
- 33 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
ACTION: If errors are large, call lab for
explanation/resubmittal, make any
necessary .corrections and note
errors in ..data assessments.
13.0 GC/MS Continuing Calibration (Form VII)
13.1 Are the Continuing Calibration Forms (Form VII)
present and complete for the BNA fraction? I ]_
13.2 Has a continuing calibration standard been
analyzed for every twelve hours of sample
analysis per instrument?
J_L
ACTION: List below all sample analyses
that were not within twelve hours
of a continuing calibration analysis
for each instrument used.
ACTION: If any forms are missing or no
continuing calibration standard
has been analyzed within twelve
hours of every sample analysis,
call lab for explanation/
resubmittal. If continuing
calibration data are not available,
flag all associated sample data as
unusable ("R").
3.3 Do any semivolatile compounds have a % Difference
(% D) between the initial and continuing RRF
which exceeds the + 25.0% criteria?
ACTION: Circle all outliers in red.
ACTION: Qualify both positive results and
non-detects for the outlier
compound(s) as estimated (J). When %D is
above 90%, reject all non-detects for that
analyte (R) unusable.
- 34 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
13.4 Do any semivolatile compounds have a RRF <0.05? _[ 1
ACTION: Circle all outliers in red.
ACTION: If RRF <0.'o5, qualify as unusable (R)
associated non-detects and "J" associated
positive values.
13.5 Are there any transcription/calculation errors
in the reporting of average response factors
(RRF) or % difference (%D) between initial and
continuing RRFs? (Check at least two values
but if errors are found, check more). I 1
ACTION: Circle errors in red.
ACTION: If errors are large, call lab for
explanation/resubmittal, make any
necessary corrections and document
effect in data assessments.
14.0 Internal Standards (Form VIII)
14.1 Are the internal standard areas (Form VIII) of
every sample and blank within the upper and
lower limits (-50% to + 100%) for each continuing
calibration? I 1
ACTION: List all the outliers below.
Sample = Internal Std Area Lower Limit Upper Limit
(Attach additional sheets if necessary.)
ACTION: 1. If the internal standard area count
is outside the upper or lower limit,
flag with "J" all positive results
and non-detects (U values) quantitated
with this internal standard.
- 35 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
~~ ' YES NO N/A
2. Non-detects associated with IS areas
> 100% should not be qualified.
3. If the IS area is below the lower limit
(<50%), qualify all associated non-detects
(U-values) "J". If extremely low area counts
are reported (<25%) or if performance
exhibits a major abrupt drop off, flag all
associated non-detects as unusable (R).
14.2 Are the retention times of the internal standards
within 30 seconds of the associated calibration
standard? _[ 1
ACTION: Professional judgement should be
used to qualify data if the
retention times differ by more than
30 seconds.
15.0 Field Duplicates
15". 1 Were any field duplicates submitted for BNA"
analysis? J 1
ACTION: Compare the reported results for
field duplicates and calculate
the relative percent difference.
ACTION: Any gross variation between field
duplicate results must be addressed
in the reviewer narrative. However,
if large differences exist,
identification of field duplicates
should be confirmed by contacting the
sampler.
- 36 -
-------
Date: January 1992
Revision: 8
YES NO N/A
PART C; PESTICIDE/PCB ANALYSIS
1.0 Traffic Reports and Laboratory Narrative
1.1 Are Traffic Report Forms present for all _[ 1
samples?
ACTION: If no, contact lab for replacement of
missing or illegible copies.
1.2 Do the Traffic Reports or SDG Narrative indicate
any problems with sample receipt, condition of
the samples, analytical problems or special
circumstances affecting the quality of the data? _[ 1
ACTION: If any sample analyzed as a soil, other
than TCLP, contains 50%-90% water,
all data should be qualified as estimated
(J). If a soil sample, other than TCLP,
contains -more than 90% water, all data
should be qualified as unusable (R) ..
ACTION: If samples were not iced upon receipt at
the laboratory, flag all positive results
"J" and all non-detects "UJ".
2 .0 Holding Times
2.1 Have any PEST/PCB technical holding times,
determined from date of collection to date of
extraction, been exceeded? _[ 1
Water and soil samples for PEST/PCB analysis
must be extracted within 7 days of the date of
collection. Extracts must be analyzed within 40
days of the date extraction.
- 37 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
.YESNON/A
ACTION: if technical holding times are exceeded,
flag all positive results as estimated .
(J) and sample quantisation limits (UJ)
and document in the narrative that holding
times were exceeded. If analyses were done
more than 14 days beyond holding time,
either on the first analysis or upon
re-analysis, the reviewer must use
professional judgement to determine the
reliability of the data and the effects
of additional storage on the sample results.
At a minimum, all the data should at least be
qualified "J", but the reviewer may determine
that non-detects are unusable (R).
3.0 Surrogate Recovery (Form II)
3.1 Are the PEST/PCB Surrogate Recovery Summaries
(Form II) present for each of the following
matrices?
a. Low Water I 1
b. Soil r 1 :
3.2 Are all the PEST/PCB samples listed on the
appropriate Surrogate Recovery Summary for
each of the following matrices?
a. Low Water I 1
b. Soil r 1
ACTION: Call lab for explanation/resubmittals.
If missing deliverables are unavailable,
document effect in data assessments.
3.3 Were outliers marked correctly with an
asterisk? I 1
ACTION: Circle all outliers in red.
3.4 Were surrogate recoveries of TCX or DCB
outside of the contract specification for
any sample or blank? (60-150%) I 1
- 38 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
ACTION: No qualification is done if surrogates
are diluted out. If recovery for both
surrogates is below the contract limit,
but above 10%, flag all results for that
sample 'J". If recovery is < 10% for
either surrogate, qualify positive
results "J" and flag non-detects "R".
If recovery is above the contract advisory
limits for both surrogates qualify positive
values "J".
3.5 Were surrogate retention times (RT) within the
windows established during the initial 3-point
analysis of Individual Standard Mixture A? I 1
ACTION: If the RT limits are not met, the
analysis may be qualified unusable (R)
for that sample on the basis of
professional judgement.
3.6 Are there any transcription/calculation errors
between raw data-and Form II? - ••-- [ • 1
ACTION: If large errors exist, call lab for
explanation/resubmittal. Make any
necessary corrections and document
effect in data assessments.
4.0 Matrix Spikes (Form III)
4.1 Is the Matrix Spike/Matrix Spike Duplicate
Recovery Form (Form III) present? S. 1
4.2 Were matrix spikes analyzed at the required
frequency for each of the following matrices?
(1 MS/MSD must be performed for every 20 samples
of similar matrix or concentration level)
a. Low Water j; 1
b. Soil r 1
ACTION: If any matrix spike data are missing,
/take the action specified in 3.2 above.
- 39 -
-------
Date: January 1992
Revision: 8
YES NO N/A
4.3 How many PEST/PCB spike recoveries are outside
QC limits?
Water Soil
out of 12 out of 12
4.4 How many RPD's for matrix spike and matrix spike
duplicate recoveries are outside QC limits?
Water Soil
out of 6 out of 6
ACTION: No action is taken on MS/MSD data alone.
However, using informed professional
judgement, the data reviewer may use the
matrix spike and matrix spike duplicate
results in conjunction with other QC
criteria and-determine the need for some
qualification of .the data.
5.0 Blanks rForm IV)
5.1 Is the Method Blank Summary (Form IV) present?^ 1
5.2 Frequency of Analysis: For the analysis of
Pesticide/PCB TCL compounds, has a reagent/
method blank been analyzed for each SDG or
every 20 samples of similar matrix
or concentration or each extraction batch,
whichever is more frequent? .[ 1
ACTION: If any blank data are missing, take
the action specified above in 3.2. If
blank data is not available, reject
(R) all associated positive data.
However, using professional judgement,
the data reviewer may substitute field
blank data for missing method blank data.
5.3 Has a PEST/PCB instrument blank been analyzed
at the beginning of every 12 hr. period following
the initial calibration sequence? (minimum
contract requirement)
- 40 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
~~~~ YES NO N/A
ACTION: If any blank data are missing, call lab for
explanation/resubmittals. If missing
deliverables are unavailable, document the
effect in data assessments.
5.4 Chromatography: review the blank raw data -
chromatograms, quant reports or data system
printouts.
Is the chromatographic performance (baseline
stability) for each instrument acceptable.for
PEST/PCBs? f 1
ACTION: Use professional judgement to determine
the effect on the data.
6.0 Contamination
NOTE: "Water blanks", "distilled water blanks" and
"drilling water blanks" are validated like any
other sample and are not used to qualify the
data. Do not confuse them with the other QC
blanks discussed-below.
6.1 Do any method/instrument/reagent/cleanup blanks
have positive results for PEST/PCBs? When applied
as described below, the contaminant concentration
in these blanks are multiplied by the sample
Dilution Factor and corrected for % moisture when
necessary. I 1
6.2 Do any field/rinse blanks have positive
PEST/PCB results? r 1
ACTION: Prepare a list of the samples associated
with each of the contaminated blanks.
(Attach a separate sheet)
NOTE: All field blank results associated to a particular
group of samples (may exceed one per case or one per
day) may be used to qualify data. Blanks may not be
qualified because of contamination in another blank.
Field blanks must be qualified for
surrogate, or calibration QC problems.
- 41 -
-------
.STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
ACTION: Follow the directions in the table below
to qualify TCL results due to contamination.
Use the largest value from all the associated blanks.
Sample cone > CRQL Sample cone < CRQL & Sample cone > CRQL
but < 5x blank is < 5x blank value & > 5x blank value
Flag sample result Report CRQL & No qualification
with a "U"; qualify "U" is needed
NOTE: If gross blank contamination exists, all data
in the associated samples should be
qualified as unusable (R).
6.3 Are there field/rinse/equipment blanks associated
with every sample? _[ 1
ACTION: For low level samples, note in data assessment
that there is no associated field/rinse/equipment blank.
Exception: samples taken from a drinking water tap
do not have associated field blanks.
7.0 Calibration and GC Performance
7.1 Are the following Gas Chromatograms and Data
Systems Printouts for both columns present
for all samples, blanks, MS/MSD?
a. peak resolution check _[ 1
b. performance evaluation mixtures _[ ]_
c. aroclor 1016/1260 r 1
d. aroclors 1221, 1232, 1242, 1248, 1254 \ 1
e. toxaphene I 1
f. low points individual mixtures A & B _[ ]_
g. med points individual mixtures A & B _[ ]_
h. high points individual mixtures A & B _[ }.
- 42 -
-------
O -L 41 IN U/\J\U
Date: January 1992
Revision: 8
YES NO N/A
i. instrument blanks _[ 1
ACTION: If no, take action specified in 3.2 above.
7.2 Are Forms VI - PEST 1-4 present and complete
for each column and each analytical sequence? j; ]_
ACTION: If no, take action specified in 3.2
above.
7.3 Are there any transcription/calculation errors
between raw data and Forms VI?
ACTION: If large errors exist, call lab for
explanation/resubmittal, make
necessary corrections and
document effect in data assessments.
7.4 Do all standard retention times, including each
pesticide in each level of Individual Mixtures
A & B, fall within the windows established
during the initial calibration analytical
sequence? (For Initial Calibration Standards,
Form VI - .PEST - 1)-. r 1
ACTION: If no, all samples in the entire
analytical sequence are potentially
affected. Check to see if the
chromatograms contain peaks within an
expanded window surrounding the expected
retention times. If no peaks are found
and the surrogates are visible, non-
detects are valid. If peaks are present
and cannot be identified through pattern
recognition or using a revised RT window,
qualify all positive results and non-detects
as unusable (R).
For aroclors, RT may be outside the RT window,
but the aroclor may still be identified from the
individual pattern.
7.5 Are the linearity criteria for the initial
analyses of Individual Standards A & B within
limits for both columns? (% RSD must be < 20.0%
for all analytes except for the 2 surrogates,
which must not exceed 30.0 % RSD). See Form VI
PEST - 2. r 1
- 43 -
-------
STANDARD OPERATING PKOCtUUKh
Date: January 1992
Revision: 8
"YESNON/A
ACTION: If no, qualify all associated positive
results generated during the entire
analytical sequence "J" and all non-
detects "UJ". When RSD >90%, flag all
non-detect results for that analyte R
(unusable).
7.6 Is the resolution between any two adjacent
peaks in the Resolution Check Mixture > 60.0%
for both columns? (Form VI-PEST - 4) r 1
ACTION: If no, positive results for compounds
that were not adequately resolved should
be qualified "J". Use professional
judgement to determine if non-detects
which elute in areas affected by co-eluting
peaks should be qualified "N" as presumptive
evidence of presence or unusable (R).
7.7 Is Form VII - Pest-1 present and complete for
each Performance Evaluation Mixture analyzed -
during the "analytical sequence for both
columns? _[ 1
ACTION: If no, take action as specified in
3.2 above.
7.8 Has the individual % breakdown exceeded 20.0%
on either column.
- for 4,4' - DDT?
- for endrin? I ]_
Has the combined % breakdown for 4,4'- DDT/
Endrin exceeded 30.0% on either column?
(required in all instances) _[ 1
ACTION: 1. If any % breakdown has failed the
QC criteria in either PEM in steps
2 and 17 in the initial calibration
sequence (p. D-38/Pest SOW 3/90),
qualify all sample analyses in the
entire analytical sequence as described
below.
- 44 -
-------
STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
'YESNON/A
2. If any % breakdown has failed the QC
criteria in a PEM "Verification
calibration, review data beginning
with the samples which followed the
last in-control standard until the
next acceptable PEM & qualify the
data as described below.
a. 4,4'-DDT Breakdown: If 4,4'-DDT breakdown
is greater than 20.%:
i. Qualify all positive results for DDT
with 'J". If DDT was not detected, but
DDD and DDE are positive, then qualify
the quantitation limit for DDT as
unusable (R).
ii. Qualify positive results for DDD and/or
DDE as presumptively present at an
approximated quantity (NJ) .
b. Endrin Breakdown: If endrin breakdown is greater
'" ' than 20.0%:
i. Qualify all positive results for endrin
with "J". If endrin was not detected, but
endrin aldehyde and endrin ketone are
positive, then qualify the quantitation
limit for endrin as unusable (R).
ii. Qualify positive results for endrin ketone and
endrin aldehyde as presumptively present at an
approximated quantity (NJ).
c. Combined Breakdown: If the combined 4,4'-DDT and
endrin breakdown is greater than 30.0%:
i. Qualify all positive results for DDT and
endrin with "J". If endrin was not
detected, but endrin aldehyde and endrin
ketone are positive, then qualify the
quantitation limit for endrin as unusable
(R). If DDT was not detected, but DDD and
DDE are positive, then qualify the
quantitation limit for DDT as unusable (R) .
- 45 -
-------
Date: January 1992
Revision: 8
YES NO N/A
7.9
ii. Qualify positive results for endrin ketone
and endrin aldehyde as presumptively present
at an approximated "quantity (NJ). Qualify positive
results for DDD and/or DDE as presumptively present
at an approximated quantity (NJ).
Are the relative percent difference (RPD) values
for all PEM analytes <25.0%? (Form VII-PEST-1) r 1
ACTION: If no, qualify all associated positive
results generated during the analytical
sequence "J" and sample quantitation
limits "UJ".
NOTE: If the failing PEM is part of the
initial calibration, all samples are
potentially affected. If the offending
standard is a verification calibration,
the associated samples are those which
followed the last in-control standard
until the next passing standard.
7.10 Have all samples been injected within a 12 hr.
period beginning with the injection of an
Instrument Blank? j; 1
ACTION: If no, use professional judgement to
determine the severity of the effect
on the data and qualify accordingly.
7.11 Is Form VII - Pest-2 present and complete for
each INDA and INDB Verification Calibration
analyzed? _[ 1
ACTION: If no, take action specified in 3.2 above.
7.12 Are there any transcription/calculation errors
between raw data and Form VII - Pest-2?
ACTION: If large errors exists, call lab for
explanation/resubmittal, make any
necessary corrections and document
effect in data assessments.
under "Conclusions".
- 46 -
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STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YES. NON/A
7.13 Do all standard retention times for each INDA
and INDB Verification Calibration fall within
the windows established by the initial
calibration sequence? ' _[ 1
ACTION: If no, beginning with the samples which
followed the last in-control standard,
check to see if the chromatograms contain
peaks within an expanded window surrounding
the expected retention times. If no peaks
are found and the surrogates are visible,
non-detects are valid. If peaks are present
and cannot be identified through pattern
recognition or using a revised RT window,
qualify all positive results and non-detects
as unusable (R).
7.14 Are RPD values for all verification calibration
standard compounds < 25.0%? _[ ]_
ACTION: If the RPD is >25.0% for the compound
being quantitated, qualify all associated
positive results "J" and non-detects "UJ"
The "associated samples" are those which
followed the last in-control standard up
to the next passing standard containing
the analyte which failed the criteria.
If the RPD is >90%, flag all non-detects
for that analyte R (unusable).
8.0 Analytical Sequence Check (Form VIII-PEST)
8.1 Is Form VIII present and complete for each column
and each period of analyses? j; ]_
ACTION: If no, take action specified in 3.2 above.
8.2 Was the proper analytical sequence followed for
each initial calibration and subsequent analyses?
(see CLP SOW p. D-39 & D-41/PEST) \ ^
ACTION: If no, use professional judgement to
determine the severity of the effect
on the data and qualify it accordingly.
Generally, the effect is negligible
/unless the sequence was grossly altered
or the calibration was also out of limits.
- 47 -
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STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YES NO N/A
9.0 Cleanup Efficiency Verification (Form IX)
9.1 Is Form IX - Pest-1 present and complete for each
lot of Florisil Cartridges used? (Florisil Cleanup
is required for all Pest/PCB extracts.) j; 1
ACTION: If no, take action specified in 3.2 above.
If data suggests that florisil cleanup
was not performed, make note in "Contract
Problems/Non-Compliance".
9.2 Are all samples listed on the Pesticide Florisil
Cartridge Check Form? _[ ]_
ACTION: If no, take action specified in 3.2 above.
9.3 If GPC Cleanup was performed, (mandatory for all
soil sample extracts) is Form IX - Pest-2
present? I 1
ACTION: If no, take action specified in 3.2 above.
ACTION: If GPC was not performed when required,
make note in" Contract "Problems/Non-
Compliance" section of data assessment.
9.4 Are percent recoveries (% R) of the pesticide and
surrogate compounds used to check the efficiency
of the cleanup procedures within QC limits:
80-120% for florisil cartridge check?
80-110% for GPC calibration?
Qualify only the analyte(s) which fail the recovery
criteria as follows:
ACTION: If % R are < 80%, qualify positive
results "J" and quantitation limits
"UJ". Non-detects should be qualified
"R" if zero %R was obtained for
pesticide compounds. Use professional
judgement to qualify positive results
if recoveries are greater than the upper
limit.
- 48 -
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STANDARD OPERATING PROCEDURE
Date: January 1992
Revision: 8
YESNON/A
NOTE: Sample data should be evaluated for
potential interferences if recovery
of 2,4,5-trichlorophenol was > 5% in the
Florisil Cartridge Performance Check
analysis. Make note in Contract Problems/
Non-Compliance section of reviewer narrative.
NOTE: The raw data of the GPC Calibration
Check analysis is evaluated for pattern
similarity with previously run Aroclor
standards.
10.0 Pesticide/PCB Identification
10.1 Is Form X complete for every sample in which a
pesticide or PCB was detected? j; ]_
ACTION: If no, take action specified in 3.2 above.
10.2 Are there any transcription/calculation errors
between raw data and Forms 6E, 6G, 7E, 7D, 8D, _[ 1
9A, B, 10A.
ACTION: If large errors" exist, call lab for
explanation/resubmittal, make necessary
corrections and note error under
"Conclusions".
10.3 Are retention times (RT) of sample compounds
within the established RT windows for both
analyses? j; 1
Was GC/MS confirmation provided when required
(when compound concentration is > 10 ug/ml in
final extract)? _[ ]_
Action: Use professional judgement to qualify
positive results which were not confirmed
by GC/MS. Qualify as unusable (R) all
positive results which were not confirmed
by second GC column analysis. Also qualify
as unusable (R) all positive results not
meeting RT window unless associated standard
compounds are similarly biased, (see
Functional Guidelines) The reviewer should
;use professional judgement to assign an
appropriate quantitation limit.
- 49 -
-------
STANDARD OPERATING
Date: January 1992
Revision: 8
YESNON/A
10.4 Is the percent difference (% D) calculated for the
positive sample results on the two GC columns
< 25.0%? • r 1
ACTION: If the reviewer finds neither column
shows interference for the positive
hits, the data should be flagged
as follows:
% Difference Qualifier
25-50 % J
50-90 % JN
> 90 % R
NOTE: The lower of the two values is reported
on Form I. If using professional judgement,
the reviewer determines that the higher
result was more acceptable, the reviewer
should replace the value and indicate the
reason for the change in the data assessment.
10.5 Check chromatograms for false negatives, especially
the multiple peak compounds toxaphene and PCBs.
Were there any false negatives? j; 1
ACTION: Use professional judgement to decide
if the compound should be reported. If
the appropriate PCB standards were not
analyzed, qualify the data unusable (R) .
11.0 Compound Quantitation and Reported Detection Limits
11.1 Are there any transcription/calculation errors in
Form I results? Check at least two positive values.
Were.any errors found? _[ 1
NOTE: Single-peak pesticide results can be checked for rough
agreement between quantitative results obtained on the two GC
columns. The reviewer should use professional judgement to
decide whethera much larger concentration obtained on one
column versus the other indicates the presence of an
interfering compound. If an interfering compound is
indicated, the lower of the two values should be reported and
qualified as presumptively present at an approximated
quantity (NJ). This necessitates a determination of an
estimated concentration on the confirmation column. The
narratiye should indicate that the presence of interferences
has interfered with the evaluation of the second column
confirmation.
- 50 -
-------
STANDARD
Date: January 1992
Revision: 8
YES NO N/A
11.2 Are the CRQLs adjusted to reflect sample dilutions
and, for soils, % moisture? ' _[ 1 _
ACTION: If errors are large, call lab for
explanation/resubmittal, make any
necessary corrections and document
effect in data assessments.
ACTION: When a sample is analyzed at more than
one dilution, the lowest CRQLs are used
(unless a QC exceedance dictates the use
of the higher CRQL data from the diluted
sample analysis). Replace concentrations
that exceed the calibration range in the
original analysis by crossing out the "E"
value on the original Form I and substituting
it with data from the analysis of diluted
sample. Specify which Form I is to be used,
then draw a red "X" across the entire page
of all Form I's that should not be used,
including any in the summary package.
ACTION: Quantitation limits affected by large,
off-scale peaks should be qualified as
unusable (R). If the interference is
on-scale, the reviewer can provide an
approximated quantitation limit (UJ) for
each affected compound.
12.0 Chromatogram Quality
12.1 Were baselines stable?
12.2 Were any electropositive displacement
(negative peaks) or unusual peaks seen?
ACTION: Address comments under System
Performance of data assessment.
- 51 -
-------
STANDARD
Date: January 1992
Revision: 8
YESNON/A
13.0 Field Duplicates
13.1 Were any field duplicates submitted for
PEST/PCB analysis? ^ • r 1
ACTION: Compare the reported results for
field duplicates and calculate the
relative percent difference.
ACTION: Any gross variation between field
duplicate results must be addressed
in the reviewer narrative. However, if
large differences exist, identification
of field duplicates should be confirmed
by contacting the sampler.
- 52 -
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ATTACHMENT 1
SOP NO. HW-6 Page of
CLP DATA ASSESSMENT
Functional Guidelines for Evaluating Organic Analysis
Case No. SDG No. LABORATORY SITE
DATA ASSESSMENT:
The current Functional Guidelines for evaluating organic data have
been applied.
All data are valid and acceptable except those analytes which have
been qualified with a "J" (estimated) , "N" (presumptive evidence
for the presence of the material) , "U" (non-detects) , "R"
(unusable),or "JN" (presumptive evidence for the presence of the
material at an estimated value). All action is detailed on the
attached sheets.
Two facts should be noted by all data users. First, the "R" flag
means that the associated value is unusable. In other words, due
to significant QC problems, the analysis is invalid and provides no
information as to whether the compound is present or not. "R"
values should not appear on data tables .because they cannot be
relied upon, even as a last resort. The second fact to keep in
mind is that no compound concentration, even if it has passed all
QC tests, is guaranteed to be accurate. Strict QC serves to
increase confidence in data but any value potentially contains
error.
Reviewer's
S ignature: Date: / /19 9
Verified By: Date: / /199
-------
ATTACHMENT 1
SOP NO. HW-6 Page of
DATA ASSESSMENT
1. HOLDING TIME:
The amount of an analyte in a sample can change with time due to
chemical instability, degradation, volatilization, etc. If the
specified holding time is exceeded, the data may not be valid.
Those analytes detected in the samples whose holding time has been
exceeded will be qualified as estimated, "J". The non-detects
(sample quantitation limits) will be flagged as estimated, "J", or
unusable, "R", if the holding times are grossly exceeded.
The following analytes in the samples shown were qualified because
of holding time:
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ATTACHMENT 1
SOP NO. HW-6 Page of
DATA ASSESSMENT
2. BLANK CONTAMINATION:
Quality assurance (QA) blanks, i.e., method, trip, field, or rinse
blanks are prepared to identify any contamination which may have
been introduced into the samples during sample preparation or field
activity. Method blanks measure laboratory contamination. Trip
blanks measure cross-contamination of samples during shipment.
Field and rinse blanks measure cross- contamination of samples
during field operations. If the concentration of the analyte is
less than 5 times the blank contaminant level (10 times for the
common contaminants), the analytes are qualified as non- detects,
"U". The following analytes in the samples shown were qualified
with "U" for these reasons:
A) Method blank contamination
B) Field or rinse blank contamination ("water blanks" or
"distilled water blanks" are validated like any other sample)
C) Trip blank contamination
-------
ATTACHMENT 1
SOP NO. HW-6 Page of
DATA ASSESSMENT
3. MASS SPECTROMETER TUNING:
Tuning and performance criteria are established to ensure adequate
mass resolution, proper identification of compounds, and to some
degree, sufficient instrument sensitivity. These criteria are not
sample specific. Instrument performance is determined using
standard materials. Therefore, these criteria should be met in all
circumstances. The tuning standard for volatile organics is
bromofluorobenzene (BFB) and for semi-volatiles is
decafluorotriphenyl- phosphine (DFTPP).
If the mass calibration is in error, or missing, all associated
data will be classified as unusable, "R". The following samples
shown were qualified with "R" because of tuning:
-------
ATTACHMENT 1
SOP NO. HW-6 Page of
DATA ASSESSMENT
4. CALIBRATION:
Satisfactory instrument calibration is established to ensure that
the instrument is capable of producing acceptable quantitative
data. An initial calibration demonstrates that the instrument is
capable of giving acceptable performance at the beginning of an
experimental sequence. The continuing calibration verifies that
the instrument is giving satisfactory daily performance.
A) RESPONSE FACTOR
The response factor measures the instrument's response to specific
chemical compounds. The response factor for the VOA/BNA Target
Compound List (TCL) must be > 0.05 in both the initial and
continuing calibrations. A value < 0.05 indicates a serious
detection and quantitation problem (poor sensitivity). If the mean
RRF of the initial calibration or the continuing calibration has a
response factor <0.05 for any analyte, those analytes detected in
environmental samples will be qualified as estimated, "J". All
non-detects for those compounds will be rejected ("R"). The
following analytes in the samples shown were qualified because of
response factor:
-------
ATTACHMENT 1
SOP NO. HW-6 Page of
DATA ASSESSMENT
5. CALIBRATION:
A) PERCENT RELATIVE STANDARD DEVIATION (%RSD) AND PERCENT
DIFFERENCE (%D):
Percent RSD is calculated from the initial calibration and is used
to indicate the stability of the specific compound response factor
over increasing concentration. Percent D compares the response
factor of the continuing calibration check to the mean response
factor (RRF) from the initial calibration. Percent D is a measure
of the instrument's daily performance. Percent RSD must be <30%
and %D must be <25%. A value outside of these limits indicates
potential detection and quantitation errors. For these reasons,
all positive results are flagged as estimated, "J"; and
non-detects are flagged "UJ". If %RSD and %D grossly exceed QC
criteria, non-detect data may be qualified "R".
For the PCB/PESTICIDE fraction, if %RSD exceeds 20% for all
analytes except for the 2 surrogates (which must not exceed 30%
RSD), qualify all associated positive results "J" and non-detects
"UJ".
The following analytes in the samples shown were qualified for %RSD
and %D:
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ATTACHMENT 1
SOP NO. HW-6 Page of
DATA ASSESSMENT
6. SURROGATES/ SYSTEM MONITORING COMPOUNDS (SMC):
All samples are spiked with surrogate/ SMC compounds prior to
sample preparation to evaluate overall laboratory performance and
efficiency of the analytical technique. If the measured surrogate/
SMC concentrations were outside contract specifications,
qualifications were applied to the samples and analytes as shown
below. The following analytes for the samples shown were qualified
because of surrogate/ SMC recovery:
-------
ATTACHMENT 1
SOP NO. HW-6 Page of
DATA ASSESSMENT
7. INTERNAL STANDARDS PERFORMANCE:
Internal Standard (IS) performance criteria ensure that the GC/MS
sensitivity and response are stable during every experimental run.
The internal standard area count must not vary by more than a
factor of 2 (-50% to +100%) from the associated continuing
calibration standard. The retention time of the internal standard
must not vary more than +30 seconds from the associated continuing
calibration standard. If the area count is outside the (-50% to
+100%) range of the associated standard, all of the positive
results for compounds quantitated using that IS are qualified as
estimated, "J", and all non-detects as "UJ" only if IS area is
< 50%. Non detects are qualified as "R" if there is a severe loss
of sensitivity ( < 25% of associated IS area counts).
If an internal standard retention time varies by more than 30
seconds, the reviewer will use professional judgment to determine
either partial or total rejection of the data for that sample
fraction. The following analytes in the samples shown were
qualified because of internal standards performance:
-------
ATTACHMENT 1
SOP NO. HW-6 Page of
DATA ASSESSMENT
8. COMPOUND IDENTIFICATION:
A) VOLATILE AND SEMI-VOLATILE FRACTIONS
TCL compounds are identified on the GC/MS by using the analyte's
relative retention time (RRT) and ion spectra. For the results to
be a positive hit, the sample peak must be within +0.06 RRT units
of the standard compound, and have an ion spectra which has a ratio
of the primary and secondary m/e intensities within 20% of that in
the standard compound. For tentatively identified compounds (TIC),
the ion spectra must match accurately. In the cases where there is
not an adequate ion spectrum match, the laboratory may have
provided false positive identifications. The following analytes in
the samples shown were qualified for compound identification:
B) PESTICIDE FRACTION:
The retention times of reported compounds must fall within the
calculated retention time windows for the two chromatographic
columns. The percent difference (%D) of the positive results
obtained on the two GC columns should be <25% The following
analytes in the samples shown were qualified because of compound
identification:
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ATTACHMENT 1
SOP NO. HW-6 Page of
DATA ASSESSMENT
9. MATRIX SPIKE/SPIKE DUPLICATE, MS/MSD:
The MS/MSD data are generated to determine the long-term precision
and accuracy of the analytical method in various matrices. The
MS/MSD may be used in conjunction with other QC criteria for some
additional qualification of data. The following analytes, for the
samples shown, were qualified because of MS/MSD:
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ATTACHMENT 1
SOP NO. HW-6 Page of
DATA ASSESSMENT
10. OTHER QC DATA OUT OF SPECIFICATION:
11. SYSTEM PERFORMANCE AND OVERALL ASSESSMENT (continued on next
page if necessary):
12. CONTRACTUAL NON-COMPLIANCE:
13. This package contains re-extraction, re-analysis or
dilution. Upon reviewing the QA results, the following form
I(s) are identified to be used:
-------
ATTACHMENT 1
SOP NO. HW-6 . Pa<3e of
DATA ASSESSMENT
11. SYSTEM PERFORMANCE AND OVERALL ASSESSMENT (continued):
-------
Evaluation of Metals Data far tbe Contract Laboratory Program (CLP)
based on
SOW. 3/90
(SOP Revision XIj
PREPARED BY:
DATE:
Hanir Sheifch, Quality Assurance Chemist
Toxic and Hazardous Waste Section
APPROVED BY
V • 'o •-' I -l\
: TV .-.«-..'>\ VX^ • \ .v-i \,-V.
APP/^OVED BY:
Robert Runyon, Chi^f
Monitoring Management Branch
DATE:
Kevin Kubik, Chief
Toxic and Hazardous Waste Section
DATE: L
-------
STANDARD OPERATING PROCEDURE Page 1- of 35
Title: Evaluation of Metals Data for the Date: Sept. 1991
Contract Laboratory Program Number: HW-2
Revision: 11
1.0 Scope
1.1 This procedure is applicable to inorganic data obtained from contractor
laboratories working for Hazardous Waste Site Contract Laboratory
Program (CLP).
1.2 The data validation is based upon analytical and quality assurance
requirements specified in Statement of Work (SOW) 3/90.
2.0 Responsibilities - Data reviewers will complete the following tasks as assigned by the Data
Review Coordinator:
2.1. For a total review;
.2.1.1 Data Assessment - "Total Review-Inorganics" Checklist Appendix (A.I).
The reviewer must answer every question on the checklist.
2.1.2 Data Assessment - Data Assessment Karrative (Appendix A.2)
The answer on the checklist must match the action in the narrative
(appendix A.2) and on Form I's. Do not use pencil to write the narrative.
2.1.3 Contract Non-Ccroplianee - SMD Report (Appendix A.3)
This report is to be completed only when a serious contract violation is
encountered, or upon the request of the Data Review Manager or Deputy Project
Officer (DPO). Forward 5 copies: one each for internal files, appropriate
Regional DPO, Sample Management Office (SMO) and last two addresses of
Mailing List for Data Reviewers (Appendix A.4). In other cases, all contract
violations should be appended to end of Data Assessment Narrative (Sec. A.2.2).
2.1.4 Data Sunnp.ry Sheet - Sumnary of Inorganic Quality Control Data (Appendix A.5).
Enter in ink on Data Summary Sheet required QC values from Forms I through IX. Circle
all values that require data qualification "Action".
2.1.5 CLP Data Assessment Stannary Fonns
2.1.5.1 Appendix A.6
Fill in the total number of analytes analyzed by different analyses and
the number of analytes rejected or flagged as estimated due to corresponding
quality control criteria. Place an "X" in boxes where analyses were not
performed, or criteria do not apply.
2.1.5.2 Appendix A.7
Data reviewer is also required to fill out Inorganic Regional Data Assessment
-------
form (Appendix A.7) provided by EPA Headquarters. Codes listed on the form
will be used to describe the Data Assessment Summary.
STANDARD OPERATING PROCEDURE Page 2 of 35
Title: Evaluation of Metals Data for the Date: Sept. 1991
Contract Laboratory Program Number: HW-2
Revision: 11
2.1.6 Data Review Log; It is recommended that each data reviewer should maintain a log of the
reviews completed to include: a. date of start of case review
b. date of completion of case review
c. site
d. case number
e. contract laboratory
f. number of samples
g. matrix
h. hours worked
i. reviewer's initials
2.1.7. Telephone Record Log - the data reviewer should enter the bare facts of
inquiry, before initiating any phone conversation with CLP laboratory.
After the case review has been completed, mail white copy of Telephone
Record log to the laboratory and pink copy to SMO. File yellow copy in
the Telephone Record Log folder, and attach a xerox copy of the Telephone
Record Log to the completed Data Assessment Narrative (Appendix A. 2).
2.1.8 Forwarded Paperwork
2.1.8.1 Upon completion of review, the following are to be forwarded to the Regional
Sample Control Center (RSCC) located in the Surveillance and Monitoring Branch:
a. data package
b. completed data assessment checklist (Appendix A.I,original) .
c. SMO Contract Compliance Screening (CCS)
d. Data Summary Sheet (Appendix A. 5) along with completed Data Assessment
Narrative (Appendix A.2)
e. Record of Conrounication (copy)
f. CLP Preanalysis Request/Approval Record (original + 3 copies)
g. Appendix A.7 (original).
2.1.8.2 Forward 2 copies of completed Data Assessment Narrative (Appendix A.2)
along with 2. copies of the Inorganic Data Assessment Form (Appendix A. 7) and
Telephone Record Log „ if any,: one each for appropriate Regional TPO,
and the other one to EPA EMSL office in Las Vegas. The addresses of TPOs and EPA office
in Las Vegas are given in Appendix A-4.
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STANDARD OPERATING PROCEDURE Page 3 of 35
Title: Evaluation of Metals Data for the Date: Sept. 1991
Contract laboratory Program Number: HW-2
Revision: 11
2.1.9 Filed Paperwork - Upon completion of review, the following are to be filed
within MMB files:
a. Two copies of completed Data Assessment Narrative (Appendix A.2) each carrying
Appendix A.7.
b. Telephone Record Log (copy)
c. SMO Report (copy Appendix A-3)
d. CLP Reanalysis Request/Approval Record (copy)
3.0 Data Completeness
Each data package is checked by a Regional Sample Control Coordinator (RSSC) for
completeness. A data package is assumed to be complete when all the deliverables
required under the contract are present. If a data package is incomplete,the RSSC
would call the laboratory for missing document (s). If the laboratory does not respond
within, a week, .SMO and MMB coordinator of Region II will be notified.
.0 Rejection of Data - All values determined to be unacceptable on the Inorganic Analysis Data
Sheet (Form I) must be lined over with a red pencil. As soon as any review criteria causes
data to be rejected, that data can be eliminated from any further review or consideration.
5.0 Acceptance Criteria - In order that reviews be consistent among reviewers, acceptance
criteria as stated in Appendix A.I (pages 4-25) should be used. Additional guidance can
be found in the National Inorganic Functional Guidelines of October 1, 1989.
6.0 SMO Contract Ccmpliance Screening (CCS) - This is intended to aid reviewer in locating any
problems, both corrected and uncorrected. However, the validation should be carried out
even if CCS is not present. Resubmittals received from laboratory in response to CCS must
be used by the reviewer.
7.0 Request for Brana lysis - Data reviewers must note all items of contract non-compliance
within Data Assessment Narrative.If holding times and sample storage times have not been
exceeded, TPO may request reanalysis if items of non-compliance are critical to data
assessment. Requests are to be made on "CLP Re-Analysis Request/Approval Record".
/
8.0 Record of Cctnmunication - Provided by the Regional Sample Control Center (RSCC) to
indicate which data packages have been received and are ready to be reviewed.
9.0 Roundiixj off numbers - The data reviewer will follow the standard practice.
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STANDARD OPERATING PROCEDURE Page 4 of 35
Title: Evaluation of Metals Data for the Date: Sept. 1991
Contract Laboratory Program Number: HW-2
Appendix A.I: Data Assessment - Contract Revision: 11
Compliance (Total Review)
YES NO N/A
A. 1.1 Contract Conpliance Screening Report (CCS) - Present? [ .]
ACTION: If no, contact RSCC.
A. 1.2 Record of Comn mi cation (from RSCC) - Present? [ ]
ACTION: If no, request from RSCC.
A. 1.3 Trip Report - Present and complete? [ ]
ACTION: If no, contact RSCC for trip report.
A.1-.4 Sample Traffic Report - Present? [ ] - : -' •
Legible? [ ]
ACTION: If no, request from Regional Sample Control
Center (RSCC).
A. 1.5 Cover Page - Present? [ ]
Is cover page properly filled in and signed by the lab
manager or the manager's designee? [ ]
ACTION: If no, prepare Telephone Record Log, and
contact laboratory.
Do numbers of samples correspond to numbers on Record
of Communication? [ ]
Do sample numbers on cover page agree with sample
numbers on:
(a) Traffic Report Sheet? [ ]
(b) Form I's? [ ]
ACTION: If no for any of the above, contact RSCC for
clarification.
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STANDARD OPERATING PROCEDURE Page 5 of 35
.tie: Evaluation of Metals Data for the Date: Sept. 1991
Contract Laboratory Program Number: HW-2
Appendix A.I: Data Assessment - Contract Revision: 11
Compliance (Total Review)
A.I.6 Form I to IX Yes No N/A
A.1.6.1 Are all the Form I through Form IX labeled with:
Laboratory name? [ ]
Case/SAS number? [ ]
EPA sample No.? [ ]
SDG No.? [ ]
Contract No.? [ ]
Correct units? [ ]
Matrix? [ ]
ACTION: If no for any of the above, note under
Contract Problam/Non-Compliance section
of the "Data Assessment Narrative".
A. 1.6.2 Do any computation/transcription errors exceed 10% of
reported values on Forms I-IX for:
(NOTE: Check all forms against raw data.)
(a) all analytes analyzed by ICP? [ ]
(b) all analytes analyzed by GFAA? [ ]
(c) all analytes analyzed by AA Flame? [ ]
(d) Mercury? [ ]
(e) Cyanide? [ ]
ACTION: If yes, prepare Telephone Log, contact
laboratory for corrected data and
correct errors with red pencil and initial.
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STANDARD OPERATING: PROCEDURE
Page 6 of 35
Title: Evaluation of Metals Data for the
Contract laboratory Program
Appendix A.I: Data Assessment - Contract
Compliance (Total Review)
Date: Sept. 1991
Number: HW-2
Revision: 11
[ _ ]
[ _ ]
A.I.7 Raw Data
A. 1.7.1 Digestion Log* for flame AA/ICP (Form XIII) present?
Digestion Log for furnace AA Form XIII present?
Distillation Log for mercury Form XIII present?
Distillation Log for cyanides Form XIII present?
Are pH values (pH<2 for all metals, pH>12 for cyanide)
present?
*Weights, dilutions and volumes used to obtain values.
Percent solids calculation present for soils/sediments?
Are preparation dates present on sample preparation
logs/bench sheets?
A. 1.7.2 Measurement read out record present? ICP
Flame AA
Furnace AA
Mercury
Cyanides
A. 1.7.3 Are all raw data to support all sample analyses and
QC operations present?
Legible?
Properly labeled?
ACTION: If no for any of the above questions
in sections A.1.7.1 through A.1.7.3,
write Telephone Record Log and contact
laboratory for resubmittals.
[ _ ]
[ _ ]
[ _ ]
[ _ ]
[ _ ]
[ -1
[ _ ]
[ _ ]
[ _ ]
[ ]
[ ]
data as estimated if pH
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STANDARD OPERATING PROCEDURE Page 7 of 35
.title: Evaluation of Metals for the Contract Date: Sept. 1991
Laboratory Program ' Number: HW-2
Appendix A.I: Data Assessment - Contract Revision: 11
Compliance (Total Review)
A. 1.8 Holding Times - (aqueous and soil samples )
(Examine sample traffic reports and digestion/distillation logs.)
Mercury analysis (28 days) exceeded? [ ]
Cyanide distillation (14 days) exceeded? [ ]
Other Metals analysis (6 months).... exceeded? [ ]
NOTE: Prepare a list of all samples and analytes
for which holding times have been exceeded. Specify
the number of days from date of collection to the date
of preparation (from raw data). Attach to checklist.
ACTION; If yes, reject (red-line) values less than
Instrument Detection Limit (IDL) and flag
as estimated (J) the values above IDL even-
though sample(s) was preserved properly.
A. 1.8.2 Is pH of aqueous samples for:
Metals Analysis >2
Cyanides Analysis <12
Action: If yes, flag the associated metals and cyanides
as estimated.
A.1.9 Form I (Final Data)
Are all Form I's present and complete? [ ]
ACTION; If no, prepare telephone record log and contact
laboratory for submittal.
Are correct units (ug/1 for waters and mg/k<3 f°r soils)
indicated on Form I's? [ ]
Are soil sample results for each parameter corrected for
percent solids? [ ]
Are EPA sample # s and corresponding laboratory sample
ID # s the same as on the Cover Page, Form I's and
in the raw data? [ ]
Are all "less than IDL" values properly coded with "U"? [ ]
-------
Was a brief physical description of samples given on Form I's? [ ]
STANDARD OPERATING PROCEDURE Page 8 of 35
Title: Evaluation of Metals Data for the
Contract Laboratory Program
Appendix A.I: Data Assessment - Contract
Compliance (Total Review)
Date: Sept. 1991
Number: HW-2
Revision: 11
Were the correct concentration qualifiers used with
final data?
ACTION; If no for any of the above, prepare Telephone
Record Log, and contact laboratory for corrected
data.
Were any samples diluted beyond the requirements of
contract?
If yes, were dilutions noted on Form I's?
ACTION: If no, note under Contract-Problem/Non-Compliance
of the"Data Assessment Narrative".
YES
NO N/A
A.1.10 Calibration
A.1.10.1 Is record of at least 2 point calibration
present for ICP analysis? [ ]
Is record of 5 point calibration present for
Hg analysis? [ ]
ACTION; If no for any of the above, write in the
Contract Problem/Non-compliance section of
the "Data Assessment Narrative".
A.1.10.2 Is record of 4 point calibration present for:
Flame AA? [
Furnace AA? [
Cyanides? [
NOTE: 1. If less than 4 standards are measured in absorbance
mode, then the remaining standards in concentration
mode must be run immediately after calibration and
be within +10% of true value.
2. For all AA (except Hg) and Cyanide analyses, one
calibration standard is at CRDL level. If not,
write in the Contract-Problem/Non-Compliance section
-------
of the "Data Assessment Narrative".
STANDARD OPERATING PROCEDURE Page 9 of 35
Title: Evaluation of Metals Data for the . Date: Sept. 1991
Contract Laboratory Program Number: HW-2
Appendix A.I: Data Assessment - Contract Revision: 11
Compliance (Total Review)
YES NO N/A
ACTION: Flag associated data as estimated if standards
are not within +10% of true values. Do not flag
the data as estimated in linear range indicated by
good recovery of standard(s).
A. 1.10.3 Is correlation coefficient* less than 0.995 for:
Mercury Analysis? [ ]
Cyanide Analysis? [ ]
Atomic Absorption Analysis? [ ]
ACTION; If-yes, flag the associated data as estimated.. .
A.1.11 Form II A (Initial and Continuing Calibration Verification)-
A. 1.11.1 Present and complete for every metal and cyanide? [ ]
Present and complete for AA and ICP when both are
used for the same analyte? [ _ ]
ACTION: If no for any of the above, prepare Telephone
Record Log and contact laboratory.
A. 1.11. 2 Circle on each Form II A all percent recoveries that
are outside the contract windows. Are all calibration
standards (initial and continuing) within control
limits:
Metals- 90-110R%? [ _ ]
Hg - 80-120R%? [ _ ]
Cyanides- 85-115R%? [ _ ]
* The reviewer will calculate correlation coefficient.
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STANDARD OPERATING PROCEDURE Page 10 of 35
Title: Evaluation of Metals Data for the Date: Sept. 1991
Contract Laboratory Program Number: HW-2
Appendix A.I: Data Assessment - Contract Revision: 11
Compliance (Total Review)
YES NON/A
ACTION: Flag as estimated (J) all positive data (not
flagged with a "U") analyzed between a
calibration standard with %R between 75-89%
(65-79% for Hg; 70-84% for CM) or 111-125%
(121-135% for Hg; 116-130% for CN) recovery and
nearest good calibration standard. Qualify results
CRDL) analyzed (CRI)
for each ICP run? [ ]
(Note: CRI for AL,Ba,Ca,Fe,Mg,Na,or K is not required.)
ACTION: If no for any of the above, flag as estimated
all data falling within the affected ranges.
The affected ranges are:
AA Analysis - **True Value ± CRDL
ICP Analysis - **True Value + 2CRDL
CN Analysis - **True Value + 0.5 x True Value.
**True value of CRA, CRI or mid-range standard. Substitute IDL for CRDL when IDL > CRDL.
Compute the concentration of the missing mid-range standard from the calibration range.
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STANDARD OPERATING PROCEDURE Page 11 of 35
..tie: Evaluation of Metals Data for the Date: Sept. 1991
Contract Laboratory Program Number: HW-2
Appendix A.I: Data Assessment - Contract Revision: 11
Compliance (Total Review)
YES NO N/A
A. 1.12.2 Was CRI analyzed after ICV/ICB and before the final
CCV/CCB, and twice every eight hours of ICP run? [ ]
ACTION: If no, write in Contract Problem/Non-Compliance
Section of the "Data Assessment Narrative".
A. 1.12.3 Circle on each Form IIB all the percent recoveries that
are outside the acceptance windows.
Are CRA and CRI standards within control limits:
Metals 80 - 120%R? [ ]
Is mid-range standard within control limits:
Cyanide 80 - 120%R? [ ]
ACTION: Flag as estimated all sample results within
the affected ranges if the recovery of the
standard is between 50-79%; flag only positive
data if the recovery is between 121-150%; reject
(red line) all data if the recovery is less
than 50%; reject only positive data if the
recovery is greater than 150%. Qualify 50% of
the samples on either side of CRI standard outside
the control limits.
Note: Flag or reject the final results only when sample
raw data are within the affected ranges and the CRDL
standards are outside the acceptance windows.
A. 1.13 Form III (Initial and Continuiixr Calibration Blanks)
A.1.13.1 Present and complete? [ ]
For both AA and ICP when both are used for the
same analyte? [ ]
Was an initial calibration blank analyzed? [ ]
Was a continuing calibration blank analyzed after
every 10 samples o'r every 2 hours (whichever is more
frequent)? [ ]
ACTION; If no, prepare Telephone Record Log, contact
laboratory and write in the Contract-Problems/
Non-Compliance section of the "Data Assessment Narrative".
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STANDARD OPERATING PROCEDURE Page 12 of 35
Title: Evaluation of Metals Data for the Date: Sept. 1991
Contract Laboratory Program . Number: HW-2
Appendix A.I: Data Assessment - Contract Revision: 11
Compliance (Total Review)
YES NO N/A
A. 1.13.2 Circle on each Form III all calibration blank values
that are above CRDL (or 2 x IDL when IDL > CRDL).
Are all calibration blanks (when IDL
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STANDARD OPERATING PROCEDURE Page 13 of 35
.tie: Evaluation of Metals Data for the Date: Sept. 1991
Contract laboratory Program Number: HW-2
Appendix A.I: Data Assessment - Contract Revision: 11
Compliance (Total Review)
YES NO N/A
ACTION: If yes, reject (red-line) all associated
data greater than CRDL concentration but
less than ten times the prep, blank value.
A. 1.14.3 Is concentration of prep, blank value (Form III) less
than two times IDL, when IDL is greater than CRDL? [ ]
ACTION: If no, reject (red-line) all positive sample
results when sample raw data are less than 10
times the prep, blank value.
A. 1.14.4 Is concentration of prep, blank below the negative CRDL?
ACTION: If yes, reject (red-line) all associated sample
results less than lOxCRDL.
A. 1.15 Form IV (1CP Interference Check Sample)
VI. 15.1 Present and complete? [ ]
(NOTE: Not required for furnace AA, flame AA, mercury,
cyanide and Ca, Mg, K and Na.)
Was ICS analyzed at beginning and end of run
(or at least twice every 8 hours)? [ ]
ACTION: If no, flag as estimated (J) all the samples for
which AL, Ca, Fe, or Mg is higher than in ICS.
A. 1.15.2 Circle all values on each Form IV that are more
than + 20% of true or established mean value. Are all
Interference Check Sample results inside the control
limits (+ 20%)? [ ]
If no, is concentration of Al, Ca, Fe, or Mg lower
than the respective concentration in ICS? [ ]
ACTION: If no, flag as estimated (J) those positive
results for which ICS recovery is between 121-150%;
flag all sample results as estimated if ICS
recovery falls within 50-79%; reject (red-line)
those sample results for which ICS recovery is less
than 50%; if ICS recovery is above 150%, reject
positive results only (not flagged with a "U").
-------
STANDARD OPERATING PROCEDURE Page 14 of 35
Title: Evaluation of Metals Data for the Date: Sept. 1991
Contract laboratory Program Number: HW-2
Appendix A.I: Data Assessment - Contract 'Revision: 11
Compliance (Total Review)
YES NO N/A
A. 1.16 Form V A (Spiked Sample Recovery - Pre-Diqestion/Pre-Distillation)-
( Note: Not required for Ca, Mg, K, and Na (both matrices), Al, and Fe
(soil only.)
A. 1.16.1 Present and complete for: each 20 samples? [ ]
each matrix type? [ ]
each cone, range (i.e. low, med., high)? [ ]
If no, is sample concentration greater than or equal
to four times spike concentration? [ ]
ACTION: If yes, disregard spike recoveries for analytes
whose concentrations are greater than or equal
to four times spike added. If no, circle those
analytes on Form V for which sample concentration
is less than four times the spike concentration.
For both AA and ICP when both are used for the
same analyte? [ ]
ACTION: If no for any of the above, flag as
estimated (J) all the positive data less
than four times the spiking levels specified
in SOW for which spiked sample was not analyzed.
NOTE: If one spiked sample was analyzed for more
than 20 samples, then first 20 samples
analyzed do not have to be flagged as
estimated (J).
A. 1.16.2 Was field blank used for spiked sample? [ ]
ACTION: If yes, flag all positive data less than
4 x spike added as estimated (J) for which
field blank was used as spiked sample.
A. 1.16.3 Circle on each Form VA all spike recoveries that
are outside control limits (75% to 125%).
Are all recoveries within control limits? [ ]
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STANDARD OPERATING PROCEDURE Page 15 of 35
Title: Evaluation of Metals Data for the Date: Sept. 1991
Contract Laboratory Program Number: HW-2
Appendix A.I: Data Assessment - Contract Revision: 11
Compliance (Total Review)
Are results outside the control limits (75-125%)
flagged with "N" on Form I ' s and Form VA?
YES
[ ]
NO
N/A
ACTION: If no, write in the Contract - Problem/Non -
Compliance section of "Data Assessment Narrative".
A.1.16.4 Aqueous
Are any spike recoveries:
(a) less than 30%? [ ]
(b) between 30-74%? [ ]
(c) between 126-150%? [ ]
(d) greater than 150%? [ ]
ACTION: If less than 30%, reject all "associated aqueous
data; if between 30-74%, flag all associated
aqueous data as estimated (J); if between
126-150%, flag as estimated (J) all associated
aqueous data not flagged with a "U"; if
greater than 150%, reject (red-line) all
associated aqueous data not flagged with a "U".
A.I.16.5 Soil/Sediment
Are any spike recoveries:
(a) less than 10%? [ ]
(b) between 10-74%? [ ]
(c) between 126-200%? [ ]
(d) greater than 200%? [ ]
ACTION: If less than 10%, reject all associated data; if
between 10-74%, flag all associated data as estimated;
if between 126-200%, flag as estimated all associated
data was not flagged with a "U"; if greater than 200%,
reject all associated data not flagged with a lrU".
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STANDARD OPERATING PROCEDURE Page 16 of 35
Title: Evaluation of Metals Data for the Date: Sept. 1991
Contract Laboratory Program Number: HW-2
Appendix A.I: Data Assessment - Contract Revision: 11
Compliance (Total Review)
YES NO N/A
A. 1.17 FOPH VI (Lab Duplicates)
A. 1.17.1 Present and complete for: each 20 samples? [ ]
each matrix type? [ ]
each concentration range (i.e. low, med., high)? [ ]
both AA and ICP when both are used for the same
analyte? [ ]
If no, are all results outside the control limits
flagged with an * on Form I's and VI? [ ]
ACTION: If no, write in the Contract - Problems/Non-
Compliance section of "Data Assessment Narrative".
NOTE: 1. .RPD is not calculable for an analyte of the
sample - duplicate pair when both values are
less than IDL.
* Substitute IDL for CRDL when IDL > CRDL.
ACTION: If no for any the above, flag as estimated
(J) all the data >CRDL* for which duplicate
sample was not analyzed.
Note: 1. If one duplicate sample was analyzed for
more than 20 samples, then first 20 samples do not
have to be flagged as estimated.
2. If percent solids for soil sample and its duplicate
differ by more than 1%, prepare a Form VI for each
duplicate pair, report concentrations in ug/L
on wet weight basis and calculate RPD or Difference
for each analyte.
A. 1.17.2 Was field blank used for duplicate analysis? [ ]
ACTION: If yes, flag all data >CRDL* as estimated
(J) for which field blank was used as duplicate.
A. 1.17.3 Are all values within control limits (RPD 20% or
difference < +CRDL)? [ ]
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STANDARD OPERATING PROCEDURE Page 17 of 35
.itle: Evaluation of Metals Data for the Date: Sept. 1991
Contract laboratory Program . Number: HW-2
Appendix A.I: Data Assessment - Contract Revision: 11
Compliance (Total Review)
YES NON/A
2. If lab duplicate result is rejectable due
to coefficient of correlation of MSA,
analytical spike recovery, or duplicate
injections criteria, do not apply precision
criteria.
A. 1.17.4 Aqueous
Circle on each Form VT all values that are:
RPD > 50%, or
Difference > CRDL*
Is any RPD greater than 50% where sample and duplicate
are both greater than or equal to 5 times *CRDL? [ ]
Is any dlfference** between sample and duplicate greater
than *CRDL where sample and/or duplicate is less than
5 tiroes *CRDL? [ ]
ACTION: If yes, flag the associated data as estimated.
A. 1.17.5 Soil/Sediment
Circle on each Form VI all values that are:
RPD > 100%, or
Difference > 2 x CRDL*
Is any RPD (where sample and duplicate are both
greater than or equal to 5 times *CRDL) :
> 100%? [ ]
Is any **difference between sample and duplicate
(where sample and/or duplicate is less than 5x*CRDL) :
> 2x*CRDL? [ ]
* Substitute IDL for CRDL when IDL > CRDL.
** Use absolute values of sample and duplicate to calculate
the difference.
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STANDARD OPERATING PROCEDURE Page 18 of 35
Title: Evaluation of Metals Data for the Date: Sept. 1991
Contract Laboratory Program Number: HW-2
Appendix A.I: Data Assessment - Contract Revision: 11
Compliance (Total Review)
YES NO N/A
ACTION: If yes, flag the associated data as estimated.
A.1.18 Field Duplicates
A. 1.18.1 Were field duplicates analyzed? [ ]
ACTION: If yes, prepare a Form VI for each aqueous field
duplicate pair. Prepare a Form VI for each soil
duplicate pair, if percent solids for sample and
its duplicate differ by more than 1%; report
concentrations of soils in ug/1 on wet weight
basis and calculate RPDs or Difference for each
analyte.
NOTE: 1. Do not calculate RPD when both values are
less than-IDL.
2. Flag all associated data only for field
duplicate pair.
A. 1.18.2 Aqueous
Circle all values on self prepared Form VI for
field duplicates that are:
RPD > 50%, or
Difference > CRDL*
Is any RPD greater than 50% where sample and duplicate
are both greater than or equal to 5 times *CRDL? [ ]
Is any **difference between sample and duplicate greater
than *CRDL where sample and/or duplicate is less than
5 tiines *CRDL? [ ]
ACTION: If yes, flag the associated data as estimated.
* Substitute IDL for CRDL when IDL > CRDL.
** Use absolute values of sample and duplicate to calculate the difference.
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STANDARD OPERATING PROCEDURE Page 19 of 35
.itle: Evaluation of Metals Data for the Date: Sept. 1991
Contract Laboratory Program Number: HW-2
Appendix A.I: Data Assessment - Contract Revision: 11
Compliance (Total Review)
YES NO N/A
A. 1.18. 3 Soil/Sediment
Circle all values on self prepared Form VI for
field duplicates that are:
RPD >100%, or
Difference > 2 x CRDL*
Is any RPD (where saitple and duplicate are both
greater than 5 times *CRDL) :
Is any **difference between sample and duplicate
(where sample and/or duplicate is less than 5x *CRDL ) :
>2x *CRDL?
ACTION: If yes, flag the associated data as estimated.
A. 1.19 Form VII (Laboratory Control Sample) (Note: LCS - not
required for aqueous Hg and cyanide analyses.)
A. 1.19.1 Was one LCS prepared and analyzed for:
every 20 water samples? [ _ ]
every 20 solid samples? [ _ ]
both AA and ICP when both are used for the same
analyte? [ _ ]
ACTION: If no for any of the above, prepare Telephone
Record Log and contact laboratory for submittal
of results of LCS. Flag as estimated (J) all
the data for which LCS was not analyzed.
NOTE: If only one LCS was analyzed for more than 20
samples/ then first 20 samples close to LCS
do not have to be flagged as estimated.
* Substitute IDL for CRDL when IDL > CRDL.
-------
** Use absolute values of sample and duplicate to calculate the difference.
STANDARD OPERATING PROCEDURE Page 20 of 35
Title: Evaluation of Metals Data for the Date: Sept. 1991
Contract Laboratory Program Number: HW-2
Appendix A.I: Data Assessment - Contract Revision: 11
Compliance (Total Review)
" YES NO N/A
A.1.19.2 Aqueous LCS
Circle on each Form VII the LCS percent recoveries
outside control limits (80 - 120%) except for aqueous
Ag and Sb.
Is any LCS recovery: less than 50%? [ ]
between 50% and 79%? [ ]
between 121% and 150%? [ ]
greater than 150%? [ ]
ACTION: Less than 50%, reject (red-line) all data;
between 50% and 79%, flag all associated data
as estimated (J); between 121% and 150%, flag
all positive (not flagged with a "U") results
as estimated; greater than 150%, reject all
positive results.
A.1.19.3 Solid LCS
NOTE: 1. If "Found" value of LCS is rejectable due to duplicate
injections or analytical spike recovery criteria,
regardless of LCS recovery, flag the associated data
as estimated (J).
2. If IDL of an analyte is equal to or greater than
true value of LCS, disregard the "Action" below even
though LCS is out of control limits.
Is LCS "Found" value higher than the control
limits on Form VII? [ ]
ACTION; If yes, qualify all associated positive data
as estimated.
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STANDARD OPERATING PROCEDURE Page 21 of 35
tie: Evaluation of Metals Data for the Date: Sept. 1991
Contract laboratory Program Number: HW-2
Appendix A.I: Data Assessment - Contract Revision: 11
Compliance (Total Review)
NO N/A
Is LCS "Found" value lower than the Control
limits on Form VII? [ ]
ACTION: If yes, qualify all associated data as
estimated.
A.1.20 Form IX (TCP Serial Dilution) -
N3TE: Serial dilution analysis is required only
for initial concentrations equal to or
greater than 10 x IDL.
A. 1.20.1 Was Serial Dilution analysis performed for:
each 20 samples? [ ]
each matrix type? [ ]
each concentration range (i.e. low, med.)? [ ]
ACTION: If no for any of the above, flag as estimated
all the positive data > lOxIDLs or > CRDL when
lOxIDL £ CRDL for which Serial Dilution Analysis
was not performed.
A. 1.20.2 Was field blank(s) used for Serial Dilution Analysis? [ ]
ACTION: If yes, flag all associated data > 10 x IDL
as estimated (J). If lOxIDL < CRDL, flag all
data > CRDL.
A. 1.20.3 Are results outside control limit flagged with an "E"
on Form I's and Form IX when initial concentration on
Form IX is equal to 50 times IDL or greater. [
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STANDARD OPERATING PROCEDURE Page 22 of 35
Title: Evaluation of Metals Data for the Date: Sept. 1991
Contract laboratory Program Number: HW-2
Appendix A.I: Data Assessment - Contract Revision: 11
Compliance (Total Review)
YES NO N/A
ACTION: If no, write in the Contract-Problem/Non-
Compliance section of the "Data Assessment
Narrative".
A. 1.20.4 Circle on each Form IX all percent difference
that are outside control limits for initial
concentrations equal to or greater than 10 x IDLs only.
Are any % difference values:
> 10%? [ ]
> 100%? [ ]
ACTION: Flag as estimated (J) all the associated sample
data > lOxIDLs (or > CRDL when lOxIDL > CRDL)
for which percent difference is greater than 10%
but less than 100%. Reject (red-line) all the
associated sample results equal to or greater
than lOxIDlB (or > CRDL when lOxIDL < CRDL) for
which PD is greater than or equal to 100%.
Note; Flag or reject on Form I's only the sample results
whose associated raw data are > lOxIDL (or >. CRDL
when lOxIDIx CRDL)
A.1.21 Furnace Atonic Absorbtion (AA) PC Analysis
A. 1.21.1 Are duplicate injections present in furnace raw data
(except during full Method of Standard Addition) for
each sample analyzed by GFAA? [ ]
ACTION: If no, renect the data on Form I's for which
duplicate injections were not performed.
A. 1.21.2 Do the duplicate injection readings agree within 20%
Relative Standard Deviation (RSD) or Coefficient of
Variation (CV) for concentration greater than CRDL? [ ]
Was a dilution analyzed for sample with post digestion
spike recovery less than 40%? [ ]
ACTION: If no for any of the above, flag all the
associated data as estimated (J).
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STANDARD OPERATING PROCEDURE Page 23 of 35
tie: Evaluation of Metals Data for the Date: Sept. 1991
Contract laboratory Program Number: HW-2
Appendix A.I: Data Assessment - Contract . Revision: 11
* Compliance (Total Review)
YES NO N/A"
A. 1.21.3 Is *analytical spike recovery less than 10% or
greater than 150% for any result? [ ]
ACTION: If yes, reject (red-line) the affected data if
recovery is <10%; reject data not flagged with
"U" if spike recovery is >150%.
NOTE: Reject or flag the data only when the affected
sample (s) was not subsequently analyzed by Method
of Standard Addition.
* Post digestion spike is not required on the pre-digestion spiked sample.
A.1.22 Form VIII (Method of Standard Addition Results)
A.I.22.1 Present? [ ]
If no, is any Form I result coded with "S" or a "+"? " [___] 1_
ACTION: If yes, write request on Telephone Record Log
and contact laboratory for submittal of Form VIII.
A. 1.22.2 Is coefficient of correlation for MSA less than 0.990 for
any sample? [ ]
ACTION: If yes, reject (red-line) affected data.
A. 1.22.3 Was *MSA required for any sample but not performed? [ ]
Is coefficient of correlation for MSA less than 0.995? [ ]
Are MSA calculations outside the linear range of the
calibration curve generated at the beginning of the
analytical run? [ ]
ACTION: If yes for any of the above, flag all
the associated data as estimated (J).
A. 1.22.4 Was proper quantitation procedure followed correctly
as outlined in the' SOW on page E-23? [ ]
ACTION: If no, note exception under Contract Problem/
Non-Compliance section of the "Data Assessment
Narrative", and prepare a separate list.
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STANDARD OPERATING PROCEDURE Page 24 of 35
Title: Evaluation of Metals 'Data for the Date: Sept. 1991
Contract laboratory Program Number: HW-2
Appendix A.I: Data Assessment - Contract Revision: 11
Compliance (Total Review)
YES NO N/A
A.1.23 Dissolved/Total or Inorganic/Total Analytes -
A. 1.23.1 Were any analyses performed for dissolved as well as
total analytes on the same sample(s). • [ ]
Were any analyses performed for inorganic as well as total
(organic + inorganic) analytes on the .same sample (s)? [ ]
* MSA is not required on ICS and prep, blank.
NOTE; I. If yes, prepare a list comparing differences
between all dissolved (or inorganic) and
total analytes. Compute the differences as
a percent of the total analyte only when
dissolved concentration is greater than CRDL
as well as total concentration.
2. Apply the following questions only if in-
organic (or dissolved ) results are (i) above
CRDL, and (ii) greater than total constituents.
3. At least one preparation blank, ICS, and LCS
should be analyzed in each analytical run.
A. 1.23.2 Is the concentration of any dissolved (or inorganic)
analyte greater than its total concentration by
more than 10%? [ ]
A. 1.23.3 Is the concentration of any dissolved (or inorganic)
analyte greater than its total concentration by
more than 50%? [ ]
ACTION; If more than 10%, flag both dissolved (or
inorganic) and total values as estimated (J);
if more than 50%, reject (red-line) the data
for both values.
A.I.24 Form I (Field Blank) -
A. 1.24.1 Circle all field blank values on Data Summary Sheet
that are greater than CRDL, (or 2 x IDL when IDL > CRDL).
»
Is field blank concentration less than CRDL
(or 2 x IDL when IDL > CRDL) for all parameters
of associated aqueous and soil samples? [ ]
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STANDARD OPERATING PROCEDURE Page 25 of 35
Title: Evaluation of Metals Data for the Date: Sept. 1991
Contract Laboratory Program Number: HW-2
Appendix A.I: Data Assessment - Contract Revision: 11
Compliance (Total Review)
YES NO N/A
If no, was field blank value already rejected due to
other QC criteria? [ ]
ACTION: If no, reject (except field blank results)
all associated positive sample data less
. .than or equal to five times the field blank
value. Reject on Form I's the soil sample
results that when converted to ug/L on wet
basis are less than or equal to five times
the field blank value.
...J..25 Form X, XI, XII (Verification of Instrumental Parameters).
A.1.25.1 Is verification report present for:
Instrument Detection Limits (quarterly)? [ ]
ICP Interelement Correction Factors (annually)? [ ]
ICP Linear Ranges (quarterly)? [ ]
0
ACTION: If no, contact TPO of the lab.
A. 1.25.2 Form X (Instrument Detection Limits) - (Note: IDL is not
required for Cyanide.)
A. 1.25. 2.1 Are IDLs present for: all the analytes? [ - ]
all the instruments used? [ _ ]
For both AA and ICP when both are used for the same
analyte? *• - •*
if no for any of the above, prepare
Telephone Record Log and contact
laboratory.
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STANDARD OPERATING PROCEDURE Page 26 of 35
Title: Evaluation of Metals Data for the Date: Sept. 1991
Contract Laboratory Program Number: HW-2
Appendix A.I: Data Assessment - Contract Revision: 11
Compliance (Total Review)
" YES NO N/A
A. 1.25.2.2 Is IDL greater than CRDL for any analyte? [ ]
If yes, is the concentration on Form I of the sample
analyzes on the instrument whose IDL exceeds CRDL,
greater than 5 x CRDL. [ ]
Action : If no, flag as estimated all values less
than five times IDL of the instrument whose
IDL exceeds CRDL.
A.1.25.3 Form XI (Linear Ranges)
A. 1.25.3.1 Was any sample result higher than high linear range
of ICP. t ]
Was any sample .result higher than the highest
calibration standard for non-ICP parameters? [ ]
If yes for any of the above, was the
sample diluted to obtain the result on Form I? [ ]
ACTION: If no, flag the result reported on Form I
as estimated (J).
A.1.26 Percent Solids of Sediments
A.1.26.1 Is soil content in sediroent(s) less than 50%? [ ]
ACTION: If yes, qualify as estimated all data
not previously rejected or flagged due
to other QC criteria.
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STANDARD OPERATING PROCEDURE Page 27 of 35
,e: Evaluation of Metals Data for the Date: Sept. 1991
Contract Laboratory Program Number: HW-2
Appendix A. 2: Data Assessment Narrative Revision: 11
Case# Site Matrix: Soil
Water
Contractor Reviewer Other
A.2.1 The case description and exceptions, if any, are noted below with reason(s)
for rejection or qualification as estimated value (s) J.
-------
STANDARD OPERATING PROCEDURE Page 28 of 35
Title: Evaluation of Metals Data for the Date: Sept. 1991
Contract Laboratory Program Number: HW-2
Appendix A.2: Data Assessment Narrative Revision: 11
A. 2.1 (continuation)
-------
STANDARD OPERATING PROCEDURE Page 29 of 35
Evaluation of Metals Data for the Date: Sept. 1991
Contract Laboratory Program Number: HW-2
Appendix A.2: Data Assessment Narrative Revision: 11
A. 2.1 (continuation)
-------
STANDARD OPERATING PROCEDURE Page 30 of 35
Title: Evaluation of Metals Data for the Date: Sept. 1991
Contract laboratory Program Number: HW-2
Appendix A.2: Data Assessment Narrative Revision: 11
A.2.2 Contract-Problem/Non-Compliance
MMB Reviewer: Date:_
Signature
Contractor Reviewer: Date:
Signature
Verified by: Date:_
STANDARD OPERATING PROCEDURE Page 31 of 35
Title: Evaluation of Metals Data for the Date: Sept. 1991
-------
Contract Laboratory Program Number: HW-2
Appendix A. 3: Contract Non-Compliance Revision: 11
(SMO Report)
CONTRACT NON-ODMPLIANCE
(SMO REPORT)
Regional Review of Uncontrolled Hazardous Waste
Site Contract Laboratory Data Package
CASE NO.
The hardcopied (laboratory name)
Inorganic data package received at Region II has been reviewed and the quality assurance and
performance data summarized. The data reviewed included:
SMO Sample No.:
Cone. & Matrix:
Contract No. VJA87-K025,K026IK027(SOW787) requires that specific analytical work be done and
that associated reports be provided by the contractor to the Regions, EMSL-LV, and SMO. The
general criteria used to determine the performance were based on an examination of:
- Data Completeness - Duplicate Analysis Results
- Matrix Spike Results - Blank Analysis Results
- Calibration Standards Results - MSA Results
TJ"^nis of non-compliance with the above contract are described below.
-rents:
Reviewer's Initial Date
-------
STANDARD OPERATING PROCEDURE Page 32 of 35
Title: Evaluation of Metals Data for the Date: Sept. 1991
Contract laboratory Program Number: HW-2
Appendix A.4: Mailing List for Data Reviewers. Revision: 11
-------
STANDARD OPERATING PROCEDURE Page 33 of 35
Evaluation of Metals Data for the Date: Sept. 1991
Contract Laboratory Program Number: HW-2
Appendix A. 5: Summary of Inorganics Revision: 11
Quality Control Data
-------
STANDARD OPERATING PROCEDURE Page 34 of 35
Title: Evaluation of Metals Data for the Date: Sept. 1991
Contract Laboratory Program Number: HW-2
Appendix A. 6: CLP Data Assessment Revision: 11
Summary Form (Inorganics)
-------
STANDARD OPERATING PROCEDURE Page 35 of 35
.e: Evaluation of Metals Data for the Date: Sept. 1991
Contract Laboratory Program Number: HW-2
Appendix A.7: CLP Data Assessment Checklist Revision: 11
Inorganic Analysis
INORGANIC REGIONAL DATA ASSESSMENT Region
CASE NO. SITE
NO. OF SAMPLES/
LABORATORY MATRIX
SDC-= REVIEWER (IF NOT ESD)_
SOW= REVIEWER'S NAME
DPO: ACTION FYI COMPLETION DATE
DATA ASSESSMENT SUMMARY
ICP AA Hg CYANIDE
1. HOLDING TIMES
2. CALIBRATIONS
3. BLANKS
4. ICS
5.'. LCS •• • ____
6. • DUPLICATE ANALYSIS " • • -
MATRIX SPIKE
MSA
9. SERIAL DILUTION
.10. SAMPLE VERIFICATION
11. OTHER QC
12. OVERALL ASSESSMENT
0 = Data has no problems/or qualified due to minor problems.
M = Data qualified due to major problems.
Z = Data unacceptable.
X = Problems, but do not affect data.
ACTION ITEMS:
AREAS OF CONCERN:
NOTABLE PERFORMANCE:
-------
m
2
-------
Appendix V
References for Multi-phasic and Oily Waste
-------
v>
United States
Environmental Protection Agency
Workshop on
Predicting the Environmental
Impact of Oily Materials
July 14, 1992
Eighth Annual Waste Testing
And
Quality Assurance
Symposium
Arlington, VA
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PREDICTING THE ENVIRONMENTAL IMPACT OF OILY MATERIALS:
INTRODUCTION AND REGULATORY PERSPECTIVE
David Friedman
USEPA Office of Research and Development
401 M Street SW
Washington, DC 20460
BACKGROUND
Prevention of groundwater contamination has historically been one of the EPA's
highest priorities in implementing the RCRA program. To that end, the Agency has
developed and promulgated test methods, fate and transport models, and regulatory
standards to control the management of wastes whose properties might pose a hazard to
groundwater. Scientists are concerned with oily waste due to its volume, toxicity, and
potential for causing severe ecological damage. Such wastes take many forms including:
liquids of widely varying viscosity, contaminated soils, sludges, and tarry "plastic" masses.
Oily wastes have some unique properties. They can migrate like a liquid but appear
to be a solid. Because they result from many commercial processes and applications, they are
broadly distributed, of very large volume, and of tremendous commercial importance.
In developing the hazardous waste identification characteristics, EPA highlighted its
concerns with protecting ground water resources by developing the Extraction Procedure
Toxicity Characteristic (40 CFR 261.24). The characteristic relies on laboratory procedures to
predict toxicant mobility.
Over the years a number of laboratory extraction methods have been applied to the
problem of predicting what might migrate from oily wastes managed under landfill
conditions. Among the test methods that have been developed and employed to identify
those wastes which might pose an unacceptable hazard are: EPA methods 1310,1311 and
1330 (Extraction Procedure, Toxicity Characteristic Leaching Procedure and Oily Waste
Extraction Procedure).
The current approaches all have deficiencies with respect to predicting the mobility of
toxic chemicals from oily wastes. Methods 1310 (EP) and Method 1311 (the TCLP)
underestimate the mobility of many oily wastes due to filter clogging problems, their
precision is less than desirable, and they have certain operational problems. Conversely,
Method 1330 (OWEP) probably overestimates mobility since it emulates a worst possible case
scenario. None of the available laboratory mobility procedures is thus totally satisfactory.
Presented on July 14,1992 at EPA Workshop U Page 1
on "Predicting the Environmental Impact o/Ofly Materials"
Printed on Recycled Papt
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PROBLEM
Given the importance of this issue, it is imperative that accurate, precise, and usable
approaches to characterizing the mobility of oily materials be developed. That is what we
are here for today.
The problem of mobility estimation is too large and complicated for us to try and
solve all its aspects in a half day. Therefore, we will focus on just one aspect of the
problem - predicting the initial source term. To put it another way, we want to predict the
highest concentration of material that might be released from the waste to the soil
immediately below the point of disposal for some reasonable amount of time. This
information would then feed into the fate and transport models used to predict the final
toxicant concentration at some distance away from the disposal area.
DISPOSAL SCENARIO OF CONCERN
The priority waste management facility scenario that EPA has selected to be modeled
in this workshop is placement of the waste into or on the ground (e.g., landfill or lagoon).
Within this scenario a number of parameters need to be considered. These include:
• Temperature (assume temperate conditions),
• Rainfall regime,
• Biodegradation,
• Hydrolysis,
• Soil types (assume soil underlying the waste management unit has a
porosity similar to that of sand), and
• Amount of waste (assume amount is large enough so that it can be
considered to be infinite).
FATE AND TRANSPORT MODEL CONSIDERATIONS
To properly manage oily wastes to protect ground water sources from contamination
by waste constituents, an adequate model to predict the fate and transport in the subsurface
environment is needed. The Agency is developing a model to simulate the migration of
aqueous and nonaqueous phase liquids and the transport of individual chemical constituents
which may move by convection and dispersion in each phase.
As input parameters, the model needs information on the amount and composition of
both the aqueous and nonaqueous phase liquid portions of the waste as well as the
composition of the leachate that might be generated by action of surface waters on any
Presented an July 14.1992 at EPA Worxshop E Page 2
on "Predicting the Environmental Impact of Oily Materials"
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"solid" material that may have initially been present in the waste material. At this time, the
Agency does not have a precise way of defining either an "aqueous phase liquid" or a
"nonaqueous phase liquid". :.
REGULATORY PERSPECTIVE
In an ideal situation, an effective approach to evaluating oily wastes would:
• Be simple to use (not require sophisticated equipment, nor constant
attention by a highly trained technician),
• Be inexpensive to run,
• Take as little time as possible to perform (ideally no more than 24
hours),
• Be accurate (relative to predicting behavior of waste in the
environment),
• Be precise (i.e., be reproducible),
• Be rugged (capable of characterizing a broad range of waste types and
constituents of concern), and
• Not generate wastes (e.g., generate little if any solvent waste and waste
contaminated media).
The characteristics that the approach should have (maximum desirable values for each
parameter) are:
• A high degree of freedom from false negatives (any errors tend toward
overestimation of threat to environment),
• Precision (RSD <50%),
• Relatively low cost /
• Taking as little time as possible to perform (<24 hours), and
• Ruggedness.
Presented an July 14,1992 at EPA Workshop U Page 3
on "Predicting the Environmental Impact of Oily Materials"
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OPTIONS FOR CONSIDERATION
I. Develop a two-component mobility test that determines the fraction of the
waste which is flowable (capable of physical movement under the influence of
gravity and overburden pressure) under, the conditions of the test Suggested
conditions: room temperature and 50 psi. Define as mobile all material that is
flowable under terms of the test plus the aqueous extract of the non-flowable
fraction. Under this option, the procedures used are independent of waste
properties and disposal environment.
II. Develop a single generic laboratory procedure to estimate what disposal point
concentration would result from aqueous leaching of the hazardous
constituents from both the mobile and non-mobile fraction of the material.
Under this option, the procedures used are independent of waste properties
and disposal environment.
III. Employ a series of laboratory test procedures to evaluate the waste material.
These procedures would be keyed to the fate and transport model to be
employed to evaluate the data.. The procedure also would be independent of
the properties of the material under evaluation.
The questions we would like you to address are:
• What would be the "best" approach to use in order to predict the nature
and concentration of the components that would leach from oily wastes
if the waste were to be placed in an unlined landfill environment?
• If the necessary tools are not presently available, how should such a
test method or model be developed and evaluated?
• What form should a cooperative development program take? How
could it be organized? Who might the cooperators be? How long
would you expect it to take to develop the necessary tools?
If you think of any ideas, information, or suggestions that you feel the Agency should
consider when addressing this issue, please send them to us. Send your comments to:
David Friedman
US Environmental Protection Agency
401 M SL SW (RD-680)
Washington, DC 20460
/
We will need to receive your comments by August 21,1992 in order for them to be
incorporated into the conference final report.
Presented on July 14,1992 at EPA Workshop H Page 4
on "Predicting the Environmental Impact of Oily Materxk"
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PREDICTING THE ENVIRONMENTAL IMPACT OF OILY WASTE:
INDUSTRY PERSPECTIVE
Clifford T. Naiquis
BP Research
4440 Warrensville Center Road
Cleveland, OH 44128-2837
STATEMENT OF ISSUE
Managing solid waste in an environmentally sound manner is a subject of high
concern to industry, EPA and the public. However, we must have regulatory tools which
accurately reflect the environmental hazard, and analysis tools which accurately assess the
potential impact of various management approaches. We need to bring the best science to
bear on the evaluation of the potential environmental threat from oily waste disposal,
considering the likely management scenarios. One way EPA has decided to regulate certain
oily waste in the past is by "listing the waste as hazardous under RCRA. This approach
identifies a material as an environmental threat based on possible (but not necessarily
realistic) mismanagement scenarios. A second way to regulate the waste is to determine if it
is hazardous using the toxitity characteristic (TO and the Toxiciry Characteristics Leaching
Procedure (TCLP) test. This test is used to determine whether a waste is hazardous or not
based upon a specific leachability test and municipal landfill disposal scenario. The options
explored in this paper serve to promote thinking about new approaches for identifying the
environmental threats and thereby to better focus regulations dealing with the management
of these materials. This will be done by introducing and critiquing current most common
predictive methods and presenting potential avenues for more accurate methods.
Although it is nearly impossible to precisely define the term "oily waste", the
following analysis can provide a basis for further discussion:
a) An oil is generally an immiscible or relatively insoluble liquid, varying in
composition but consisting of organic constituents. Petroleum oils principally
consist of hydrocarbons; vegetable and animal oils are glycerides, and fatty
acids; and essential oils are terpenes, alkaloids, etc.
b) An oily waste is an industrial process waste or residual bearing oil in visual
and/or measurable proportions.
i
c) Oil in oily wastes can occur in any matrix, including: sorbed to dry solids; in
sludges or slurries; multi-phase liquids or sludges/slurries with multi-phase
Presented on ]uly 14,1992 at EPA Workshop E Page 5
on "Predicting the Environmental Impact of OHy Materials"
-------
liquids, if water is present. Proper treatment and disposal of all such matrices
is a concern of the petroleum industry.
d) Analysis of oils in oily wastes can be accomplished by techniques such as Total
Petroleum Hydrocarbons (TPH) (not constituent-specific) or TCLP (constituent-
specific). In a number of contexts, the procedures of methods such as these
serve to define what is meant by "oil" and "oily waste."
e) Oily wastes possess a wide variety of compositions and physical and
toxicological properties.
Some examples of oily waste include petroleum refinery sludges, such as oil- water
separator sludge and dissolved air floatation froth, storage tank bottom sludge, used oil and
others. Expanded beyond the petroleum community there are many types of oily wastes
(POTW sludges, polymer plants, timber processing, iron and steel, pulp and paper, meat
packing, slaughterhouse, leather tanning, coil coatingjestaurants, and miscellaneous foods
including meat, dairy and vegetable based oils and fats, etc.).
Currently there are a variety of state and local programs designed to address potential
environmental impacts of the management of various types of oily materials, such as E&P
wastes, spill residues and UST wastes. A number of RCRA listed and toxicity characteristic
wastes are also regulated under federal programs. EPA is currently evaluating the possible
listing of additional petroleum refining wastes.
Unfortunately, the current analytical methods for determination of the environmental
threat of petroleum constituents in wastes and oily materials via the TCLP test and model
and RCRA listing system remain controversial. USEPA, academia, and the regulated
community are continuing efforts to identify a sound, reproducible methodology to
accurately assess these threats. In fact, EPA has recently proposed a rule to address the over-
regulation of listed wastes created by EPA's "mixture" and "derived-from" rules. This
initiative, called the Hazardous Waste Identification Rule, could have major impacts on the
classifications and management of hazardous and nonhazardous industrial wastes, including
oily waste.
An approach that the American Petroleum Institute (APD has suggested to the
Agency is concentration-based exclusion criterion coupled with contingent management. It is
a two-tiered process for determining whether wastes captured under the RCRA listing rule
should or should not continue to be regulated as hazardous. One tier would allow wastes
with constituents below health based levels (with an appropriate multiplier to account for
dilution and attenuation) to be deemed nonhazardous provided the waste does not exhibit a
RCRA characteristic. A second tier would allow wastes that contain constituents below
somewhat higher health based levels to be deemed as nonhazardous, provided these wastes
are managed in certain environmentally protective ways. This second approach would alter
the current system by basing a waste's classification on how it is actually managed and not
how it could be hypothetically mismanaged.
Presented on July 14,1992 at EPA Workshop U Page 6
on "Predicting the Environmental Impact of Oily Materials"
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On the test method side, many, including Environment Canada, ASTM and the
USEPA, have been involved with the development of improved leachability and contaminant
fate/transport tests and models.: Despite this work, predicting the potential environmental
hazard associated with oily wastes remains problematic.
TCLF APPROACH
The toxicity characteristic leaching procedure (TCLP) was developed as a way to
evaluate the threat of solid waste disposal under "...a mismanagement scenario for toxic
wastes which constitutes a prevalent form of improper management-namely, the co-disposal
of toxic wastes in an actively decomposing municipal landfill which overlies a groundwater
aquifer..." (Fed. Reg., May 8,1990). The TCLP is a leaching and acidic aqueous extraction
test. The test was designed to model mismanagement of the disposal of process wastes. The
Toxicity Characteristic (TC) rule itself, and constituent-specific limits associated with the TC,
define wastes as hazardous on the basis of the concentrations of certain toxic constituents.
The TC and its constituent-specific limits were developed in large part to protect human
health from contamination of drinking water aquifers. The TCLP test, as currently
interpreted, is applicable to those wastes which produce a separate non-aqueous phase as
well as those which do not.
Specifically the model system that forms the basis for the regulatory limits imposed
by the current toxicity characteristic is one which assumes that the waste is disposed of in a
municipal hazardous waste landfill where it is leached by acidic landfill liquids, emerges
from the landfill bottom into underlying groundwater whereupon it migrates to -an
hydraulically down-gradient drinking water well (see Figure 1).
The current Toxicity Characteristic defined-method for determining environmental
risks uses a three-part system, consisting of a physical model (TCLP), coupled to a
mathematical model (EPACML), coupled to a toxicological model. The TCLP simulates
constituent leaching from a landfill, EPACML simulates constituent transport from a landfill
to a drinking water well, and the toxicological model relates drinking water concentration to
health-effects. The TCLP was not designed as, and fails as, a multi-phase model This is
because the oil phase is simply treated as water. Additionally any multi-phase capability
within EPACML was ignored due to the TCLP output.
Presented an July U, 1992 at EPA Workshop U Page 7
on "Predicting the Environmental Impact of Oily Materials"
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to
10
IS
K O
cr
Tozlcological
models
Groundinaler
I
to
Figure 1: Components of TC "System
-------
Significant technical aspects of the TCLP simulation can be summarized as follows
(see Figure 2).
• No vadose zone-bottom of the landfill is in direct contact with the ground
water.
• The disposal of waste liquids (oil and water) are equally mobile.
• The liquids are not leached or diluted but elute directly from the landfill into
the ground water.
• Infinite source-liquids continue to be released forever regardless of amount of
liquids in the original waste.
• The solids are leached with a 20:1 volume of acidic "landfill leachate" which
then enters the ground water.
• Infinite source - the hazardous constituent concentration in the initial 20:1
leachate volume continues to be leached from the material forever, regardless
of mass of constituents in the original waste.
• The liquids and leachate travel through the ground water to a drinking water
well Attenuation and dilution reduce concentrations by a factor of 100.
• Oil moves as water.
• Hazardous constituent concentrations achieve steady-state in the well at which
time the well-owner drinks two-liters/day for 70 years (oil and all).
VALIDITY OF THE TCLP APPROACH
Oily wastes provide a great challenge to those charged with evaluating their potential
impact on the environment. Unfortunately the design of the TCLP test in concept,
methodology and fate/transport modeling, inaccurately predicts the behavior of waste
containing separate-phase oil and organic constituents. One shortcoming is that it forces a
generic disposal scenario which may be reasonable for some cases but impossible for others.
Specific problems include operational problems with the test procedure, the assumption that
oil behaves identically to water in the environment, the validity of the disposal scenario, and
invalid contaminant fate/transport assumptions.
Presented on ]uly 14,1992 at EPA Workshop U Page 9
on "Predicting the Environmental Impact of Ofly Materials"
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•8
Landfill
1. no vadosazone
2. RquBoue and non-aqueous
liquids treated identicallu
3. Liquids not leached or diluted
prior to entering groundinalor
4. Infinite oaurco
of iDBBta liquids
5. Leachate enters
groundmatar directlg
9. Individual
drinks 2 L/dag
for 70 years
20:1
acidic
loachala
6. Infinite source
of leachata
7. Straight dilution G
attenuation b\j factor
of ion
B. Oil moves as mater
Both
liquids
and
leachale
migrate
to well
i
Figure 2: Issues inherent in TC scenario uihich ujork to
introduce inaccuracg.
-------
The test system was not designed for multi-liquid phase materials. This results in
operational problems with the TCLP methodology including non-reproducible free oil
breakthrough, filter clogging, and difficulties with volatiles equipment. The zero headspace
extractor (ZHE) test equipment is difficult to clean. Some volatile chlorinated compounds are
transformed within the TCLP extraction (Bricka, et al, 1991). EPA has, to date, not provided
approved test methods which are validated for the analysis of metals in non-aqueous liquids
(55 Fed.Reg. 4444).
One of the initial steps in the TCLP test is pressure filtration of the waste. For some
oily wastes, non-aqueous liquid may be expressed. This liquid is segregated from the
remaining solids which are then acid-leached. This acid leachate is combined with the non-
aqueous liquid to produce the 'TCLP leachate" which is compared to
hazardous/nonhazardous criteria.
Implicit in this procedure is the assumption that both aqueous and non-aqueous
liquids will behave identically, both within the landfill and upon their hypothetical release.
EPA has been able to provide little, if any, support for this critical portion of the TCLP.
"The initial liquid/solid separation problems are due to the tendency for some material,
such as certain types of oily wastes, to clog the 0.45um filter and prevent filtration This
problem is serious, since materials which do not pass the 0.45 um filter are treated as solids
even if they physically appear to be a liquid. These (liquid) wastes are then carried through
EP extraction as a solid."
"This is particularly serious -for oily wastes, since oils have been known to frequently
migrate to ground waters. It is important for the liquid (sic)/solid separation to treat, as
liquids, those materials which can behave as liquids in the environment."
"As indicated below, EPA believes that the liquid/solid separation technique....
reduces variability....and that it also provides a more adequate differentiation between those
materials that behave as liquids in the environment, and those materials which behave as
solids."(51 Fed. Reg. 21658)
As we gain experience with risk evaluations, we see that the risk posed by light, non-
aqueous phase liquids (i.e. "oil") appears to be mostly due to dissolved contaminants in
drinking water. The calculated risk due to free oil is not great due to the lack of exposure.
As it moves through the soil, oil will be immobilized in the soil and from that point may
partition into the water phase according to constituent solubilities. Any mobile oil migrating
to a water well does not represent a 2L/day, 70 year hazard since it is not realistic to project
that anyone will drink free-phase hydrocarbons daily for their entire lives. Therefore, it
makes some technical sense to leach the oil fraction with the acidic medium along with the
solids.
Presented on July 14,1992 at EPA Workshop H Page 11
on "Predicting the Environmental Impact of Oily Materials"
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The disposal scenario as depicted by EPA is not an accurate description of current
waste disposal practices. An EPA-OSW survey, several years old already, documents that
liquid-type wastes are no longer being accepted by municipal landfills (51 Fed. Reg. 21655).
New test methods based upon actual waste management situations would give more
accurate results than those based on generic hypothetical scenarios.
Industry has commented upon the shortcomings of the current TCLP/CML model.
For example, the infinite source assumptions require contaminant mass to continue to be
available for introduction into ground water until steady state is achieved. This is
unrealistic. One improvement would be to design transient, declining source terms into the
model Further, there is no consideration of a vadose zone although we know it exists and
future landfill regulations will require the presence of a vadose zone. The TCLP is not
designed to handle the separate organic phase flow. The current TCLP system does not take
into account aerobic biodegradation, volatilization, or retardation. Hydrolysis is apparently
being considered at this juncture, but is not currently part of this system.
The unilateral application of TCLP to multi-phase wastes, especially those containing
oily materials, is unsupported and inappropriate. There is no evidence that non-aqueous
liquids behave as aqueous liquids in a landfill Indeed, such liquids have an affinity for the
solid materials in the landfill which could cause contaminants to be less mobile than
predicted by the TCLP.
Until work on the behavior of non-aqueous materials and the prediction of their
movement is more mature, the non-aqueous liquids should be treated like the waste itself
and be subjected to the same extraction with acidic fluid. To the extent that hazardous
constituents are released into the extractant, they should be combined with the aqueous
extract generated from the waste solids.
THE EFFECTS OF THE CURRENT TC SCENARIO MODEL - SOME IMPACTS
A number of wastes from the petroleum industry, such as waters from tank
drawdowns, ground-water extraction, and hydrotesting, are or may be subject to the TC rule
even though there is no conceivable way that these materials would ever find their way into
a landfill.
The RCRA Corrective Action Program could potentially generate large quantities of
petroleum-contaminated soils. On-site and in-situ management techniques are not accurately
represented by the TCLP. In addition, a number of states currently have effective response
programs for clean up of spills and other releases of petroleum into the environment States
are concerned that application of the TCLP (particularly if TCLP is a poor estimator of
environmental threat) will seriously impact operation and effectiveness of these programs by
adding unnecessary and unwarranted hazardous waste handling requirements to wastes
which don't pose a threat. We can no longer afford to waste large sums of money handling
solid waste in a manner which over estimates the actual environmental threat.
Presented on July 14,1992 at EPA Workshop U page 22
on "Predicting the Environmental Impact of Oily Materials"
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A WAY FORWARD - SAB LEACHABILITY SUBCOMMITTEE
Given the problems with the applicability of the TCLP to multi-phase waste, are there
any alternatives? What are the potential ways forward?
Last year, a report was issued by the Science Advisory Board (Environmental
Engineering Committee, Leachability Subcommittee), entitled "Recommendations and
Rationale for Analysis for Contaminant Release." It contained nine recommendations:
• A variety of contaminant release tests and test conditions which in corporate
adequate understanding of the important parameters that affect leaching
should be developed and used to assess the potential lease of contaminants
from sources of concern.
• Prior to developing or applying any leaching tests or models, the controlling
mechanisms must be defined and understood.
• A consistent, repeatable and easily applied, physical, hydrologic and
geochemical representation should be developed for the waste management
scenario of concern.
• Leach tests and conditions (stresses) appropriate to the situations being
evaluated should be used for assessing long-term contaminant release
potential.
• Laboratory leach tests should be field-validated, and release test accuracy and
precision established before tests are broadly applied.
• More and improved leaching models should be developed and used to
complement laboratory tests.
• To facilitate the evaluation of risk implications of environmental releases, the
Agency should coordinate the development of leach tests and the development
of models in which release terms are used.
• The Agency should establish an inter-office, inter-disciplinary task group,
including ORD to help implement these recommendations and devise an
Agency-wide protocol for evaluating release scenarios, tests, procedures, and
their applications.
• The task group should also be charged with recommending what the
appropriate focal point(s), responsibilities, and organizational, budgetary and
communication links should be within the Agency for the most effective,
continued and ongoing support and pursuit of research, development, and
utilization of methods and procedures.
»
To fully accomplish all of the recommendations will be costly and time- consuming.
However there can be no alternate to core research on contaminant release and transport
Presented on July 14,1992 at EPA Workshop JJ Page 13
on "Predicting the Environmental Impact of Oily Materials"
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methods. SAB identified approximately 30 leach tests which are used internationally to
attempt to evaluate environmental threat of wastes. Unfortunately SAB concludes that each
method suffers from shortcomings.
APPLICATION TO OILY WASTE
If we wish to improve upon the system, there are two basic options:
1. Stick with the physical/mathematical model basis of the TCLP and improve
accuracy by modeling multi-phase transport and remove assumptions
predicated on long-term human consumption of immiscible product.
2. Replace with a single alternative model, either physical or mathematical.
We understand that EPA is exploring various enhanced modeling systems for multi-
phase disposal scenarios. These would include multi-phase flow within the unsarurated zone,
and partitioning between aqueous, oil, and air phases within the soil Also included would
be saturated zone groundwater pollutant transport models which are more accurate. Industry
favors these developments as tools to better understand oily waste disposal impact.
On the other hand, we must currently deal with an inappropriate TC rule. Currently,
industry must comply with the TC rule, which means it must run TCLP tests on oily wastes.
This has resulted in a disastrous situation. The TCLP was not designed to accurately assess
the environmental threat of oily materials, therefore it does not. However, decisions on the
"proper" management of these wastes are being made on the basis of a flawed test.
Industry has had to deal with the TC for many years. We have modified our waste
management approaches and strategies, we have complied with TC and land disposal
requirements and we are preparing to fully comply with Corrective Action. Unfortunately,
changes to the TC at this point may be just as disruptive and costly as compliance with the
TC has been to date. Modifications must be done carefully and deliberately, always using
the best possible science to ensure accuracy, not just consistency.
API supports, as mentioned in the Statement of Issue section, a concentration- based
exclusion coupled with contingent management for exempting listed hazardous waste from
subtitle C requirements. This would address the "inappropriate scenario" dilemma by
incorporating elements of actual management approaches instead of one hypothetical
approach.
The regulated community has volunteered to work with EPA both as individuals,
individual companies, and through trade organizations. We will continue to offer such
assistance. For myself, I see continued interaction between EPA- OSW and the American
Petroleum Institute. Typical industrial support to EPA includes offering technical comment,
procuring wastes, providing waste generation and characterization data, and participating in
round-robin testing of new methods.
Presented on July 14,1992 at EPA Workshop U Page 14
on "Predicting the Environmental Impact of Oily Materials"
-------
I-3
TAULF, I - EXTRACTION TESTS
I. STATIC TESTS (LEACHING FLUID NOT niDNIC
»« A. ACITATKDEXTIlACriON TESTS
TEST METHOD
LEACHING FI.UID
I.IQIIIH:SOI.in RATIO
MAXIMUM PARTICLE. SI/I:
NUM1IP.ROP
F.XTR ACTIONS T1MF. Ol: EXTRACTION
TCI.P(mi)
I
t-t
in
EPTOX(I3IO)
ASTM D3987-85
CAUPORNIA WET
LEACHATE EXTRACTION
PROCEDURE (MOH.
ONTARIO)
QUEBEC R.S.Q
(MOE.QUEDEC)
FRENCH LEACH TEST
(APMOR.PRANCP.)
EQUIUDRIUM
EXTRACTION
(ENVIRONMENT CANADA)
MULTIPLE HATCH
LEACHINO
PROCEDURE
(ENVIRONMENT CANADA)
ACUTIC ACID
O.I N ACETIC ACID
SOLUTION, pi 11.9.
POR ALKALINE WASTES
O.I M SODIUM ACP.TATP.
IIUITP.R SOLUTION, pll 5.0,
POR NON-ALKAI.INIi WAS'll-S
0.5 N ACUTIC ACIO
(pll=.50)
ASTM TYI'P. IV RF.AfiP.NT WATER
0.7 M SODIUM CITRATE
(plUS.O)
ACETIC AQD
2 MI-Q/R
INORGANIC 0.02 MEQ/G
ORGANIC DISTILLI-D WATER
Dl WATER
DISTILLED WATER
ACETIC ACID
IIUITRU.plM.5
211:1
IK HOURS
16:1 DURINO EXTRACTION
10:1 PINAI. DILUTION
JO. I
I O.I
20:1
10:1
10:1
4:1 9R
2:1
9.5 mm
AS IN ENVIRONMENT
2.0 mm
AS IN ENVIRONMENT
GROUND
9.5 mm
(••HOUND
9.5 mm
VARIAIH.F.
24 HOURS
I! HOURS
48 HOURS
24 HOURS
24 HOURS
16 HOURS
7 DAYS
24 HOURS
-------
00
CT
METHOD (MATERIAL
CHACTEREATION
CENTRE-2) ^
C. SEQUF.NTIAL CHEMICAL EXTHACTIONTtSTS
TA111.E 1 • I'X'lllACnON 11;STS (continued)
TEST METHOD
MATERIAL CHAR ACTEK-
IZATION CEN1RE-4
(MATERIAL CHARACTER-
IZATION CEN1RE)
OILY WASTE
(1330)
SYNTHETIC PRECIPI-
TATION LEACHING
PROCEDURE (1312)
EQUILIBRIUM
LEACH TEST
LEACIIINO FLUID
CHOICE
SOX LET WITH TIIFAND
TOLUENE LP ON
REMAINING SOLIDS
VARIABLE
DISTILLED WATER
NUMBER OF
L1QUID:SOIJD RATIO MAXIMUM PARTICLE SIZE EXTRACTIONS . TIME OF EXTRACTIOI
10:1 2 FRACTIONS 1 20 DAYS TO
74 - 149 mm 10 YEARS
150 -425 mm
IIXXltinOML 9.5mm 3 24 HOURS (CP)
20:1
20:1 9.5mm 1 l» HOURS
4:1 ISn.im 1 7 DAYS
n. NON-AGITATED EXTRACTION TESTS
TEST METHOD
STATIC LEACH
TEST METHOD
(MATERIAL CHACTEIt-
IST1C CENTRE- 1)
Iliail TEMPERATURE
STATIC LEACH TEST
LEACHING FLUID
CAN nn srn- SPECIRC
SAMP. AS Anovi-
I1UTATIOO°C
NUMRF.ROP , '
LIQUID:SOIJD RATIO MAXIMUM PARTICLE SIZE EXTRACTIONS TIME OF EXTRACT!'
VOL/SURFACE 10 urn 40 mm: SURFACE AREA 1 >7 DAYS
VniVSUKFACI! lOum 40 mm7 SURFACI- AltliA 1 >7 DAYS
I
TEST METHOD
SEQUENTIAL
EXTRACTION TESTS
LI-ACHING FLUID
0.04 M ACirnc ACID
!.IO.UII):SOI.II) RATIO
50:1
MAXIMUM PAIU1CI.F. SIZE
9.5 r
NUMIIER OF
EXTR ACTIONS TIME OF EX1RACI1
15
24HOUKSPF.
F.XIVACTKV
-------
TAIU.I: I - EXTRACTION TESTS (cominncd)
D. CONCENTRATION BUILD-UP TEST
•TEST METHOD
SEQUENTIAL
CHEMICAL EXTRACTION
STANDARD LEACH
TEST. PROCEDURE C
(UNIVERSITY OF
WISCONSIN)
LEACHING FLUID
nvn LEACHING SOLUTIONS
INCREASING ACIDITY
Dl WATP.R
SYNI.ANOni.1.
I.IQUID:SQUD RATIO
VARIES ITCOM
10:1,5:1
1.5:1
MAXIMUM PARTICLE SIZE
1501
AS IN I'.NVIIIONMI'.NT
NUMBER OF
EXTRACTIONS
TIMF. OF EXTRACTIONS
VAR1PSFROM7
TO 74 HOURS
3 OR HDAYS
II. DYNAMIC TESTS (LEACHING FLUIO RENEWED)
A. SERIAL MATCH (PARTICLE)
I
TEST METHOD
MULTIPLE
EXTRACTION
PROCEDURE
(1320)
MWEP
(MONOF1LL WASTE
EXTRACI1ON PROCEDURE)
GRADED SERIAL HATCH
(U.S. ARMY)
SEQUENTIAL DATCH
ASTM D4793-88
WASTE RESEARCH
UNIT LEACH TEST
(HARWELL LAD-
ORATORY. UK)
STANDARD LEACHING
TEST: CASCADE TEST
SOSUV. NETHERLANDS
LEAGUING PI.UID
SAME AS EPTOX.THEN
WITH SYNTHETIC ACID
RAJN(SULFURJCACID:
NITRIC ACID IN 60:40%
MIXTURE)
DISTILLED/DGIONIZED
WATER Oil OTHER TOR
DISTILLED WATP.H
TYPE IV REAGENT WA1T:R
ACETIC AOD
nUITCREDpll =
nisni.Lno WATER
UNO] I'M 4.0
I.IQUlD:SOl.m RATIO
20:1
10:1 PP.R
EX'lllACnON
SI'liCIFIC SI'll:
INOtRASES ITIOM
J:IT096:I
70:1
I ni:D VOL 5 EI.UTIONS
inni;nvoL>6
El.imONS
70:1
MAXIMUM PARTICLE SIZE
9.5 mm
9.6 mm OR
MONOLITH
N/A
AS IN ENVIRONMENT
CRUSHING
CRUSHING
NUMPI-ROP
P.XIXACnONS
9 (OR MOKE)
>7
10
TIMEOPEXTRACTIOh
74 HOURS PER
EX1HACTION
18 HOURS PER
P.XIHACnON
UNTP. STEADY
18 HOURS
7 TO 80 HOURS
23 HOURS
-------
J-S
I
K>
do
TAIII.Ii I • EXTRACTION 1V.STS (coiuiiiueil)
II. FLOW AROUND TESTS
TEST METHOD
IAEA DYNAMIC LEACH
TEST (INTERNATIONAL
ATOMIC UNEIIGY AGENCY)
ISO LEACH TEST
(INTERNATIONAL
STANDARDS ORGANI-
ZATION)
ANSIMNS 16.1
(AMERICAN NATIONAL
STANDARD INSTITUTE/
AMERICAN NUCLEAR
SOCIETY)
DLT
LEACHING FLUID
Dl WATER/SITE WATER
Dl WATER/SITE WATP.R
DI WATER
Dt WATER
C. FLOW THROUGH TESTS
TEST METHOD
STANDARD LEACHING
TEST: COLUMN TEST
(SOSUV.TIIE
NETHERLANDS)
COLUMN ASTM D4874-89
LEACHING FLUID
Dl WATI-It
IIN03p1l=.4
TYIT: IV REAGENT W ATI-It
I.IQUin:SOUD RATIO
N/A
N/A
N/A
N/A
I.IQUID:SOUn RATIO
10:1
ONI- VOID VOI.UMF.
MAXIMUM PARTICLE SKI-
ONF.FACF. rUF-PARRD
SURFACE POLISHING
SURFACE WASHING
SURFACE WASHING
MAXIMUM PARTICLE SI7.fi
AS IN ENVIRONMENT
AS IN ENVIRONMENT
NUMBER OF
EXTRACTIONS
18
NUMREROF
EXTRACTIONS
TIME OF nXTRACTIC
>6 MONTHS
>IOODAYS
90 DAYS
1 96 DAYS
TIME OP EXTRACT
20 DAYS
24 HOURS
-------
I
III.
OTIIFJl TESTS
TEST METHOD -
LEACHING F1.UID
TAIII.E I • KX'lllACIlON 'HiSTS (coniiniicil)
NUMDER OP
LIQUID:SOLID RATIO MAXIMUM PARTICLE SI7.E EXTRACTIONS TIMF. OF EXTRACTIONS
MdC-JSSOXHLETTEST DI/SITE WATER 100:1
(MATERIAL CHARACTER-
ISTIC CENTER)
ACID NEUTRALIZATION UNO. SOLUTIONS OP 3:1
CAPACITY INCUI-ASINO STUENfiTII
CUT AND WASHED
I SO mil
0.2 M1./MIN
48 HOURS PER
F.XTRACTION
cr
REFERENCES:
I. Cornpendiiim of Wnsic Lc.nlinR Tcsn, Wnsic Waicr Technology Ccnirc. l-nvirnnineni Ciniailii. Final Diall May 27. I9R9
2. Private discussions wilh Gail ll.niiscn.Ofnccof Solid Waste. U. S. P.PA
-------
PREDICTING THE ENVIRONMENTAL IMPACT OF OILY MATERIALS:
SCIENTIFIC PERSPECTIVE
Larry P. Jackson
INTRODUCTION
This paper is intended to stimulate discussion into new or better ways to evaluate the
potential release of regulated substances from oily wastes. The paper discusses some options
to the currently approved procedures to determine the concentrations of regulated organic
chemicals released into the groundwater regime from improperly managed oily waste. The
paper also describes a proposed method to evaluate the fraction of an oily waste which is
flowable under the influence of gravity or overburden pressure if the material is improperly
disposed in a landfill. The options presented cover, in part, some of the major technical
concerns of the Environmental Engineering Committee of the Environmental Protection -
Agency's (EPA) Science Advisory Board (SAB) in their October, 1991 recommendations to the
EPA Administrator 1
This paper is prepared from the perspective that accurate, reliable, and cost-effective
analytical procedures can be developed to properly characterize and manage potentially
hazardous oily wastes. The paper accepts the premise that the regulatory community must
proceed carefully and the "worst case scenario" will be considered in any proposed solutions.
The paper seeks to incorporate some of the suggestions of the EPA Science Advisory Board
that methods should take into consideration real world factors such as:
• source matrix properties,
• contaminant properties,
• leachant properties,
• fluid dynamics,
• chemical and physical properties of the waste,
• temporal/spatial dependence,
• measurement methods, and
• physical models.
Presented on July 14,1992 at EPA Workshop n Page 20
on "Predicting the Environmental Impact of Qfly Materials"
-------
TECHNICAL ISSUES
Neither the regulatory nor the regulated community has successfully proposed
methods to properly characterize the potential for environmental impact for oily wastes.
Existing leaching tests are known to be technically and mechanically deficient, and no
method exists to measure the amount of flowable, oily material which may be released from
a waste. Solutions to these problems have not been discussed to any extent in the published
literature nor in the proceedings of symposia and workshops. These issues are recognized as
the major unaddressed problems in evaluating the pollution potential of oily wastes. Any
scenario which proposes to assess the pollution potential of this class of wastes must address
these issues. This section describes the current state of the technology in these areas.
Tne Oily Waste Extraction Procedure (OWEP, EPA Method 1330A)2 is designed to
evaluate the potential for an oily waste to release metals under aqueous leaching conditions.
OWEP separates the solid material from the oil by solvent extraction. The solid phase is then
leached by Method 1310A, Extraction Procedure Toxicity Test2 and the extracted oil analyzed
directly for the metals of interest. The results of the analyses of the two fractions are
combined mathematically. It is generally conceded that this overestimates the leaching
potential of the waste. If the method is applied to the analysis of regulated organic
constituents, all of the analyte will be deemed leachable which is incorrect. It should be noted
that the OWEP has never been suggested as appropriate for organic constituents.
The current approach for analyzing the leaching potential of solid waste, EPA Method
1311, Toxicity Characteristic Leaching Procedure CTCLP)2 differs from the OWEP in that TCLP_
attempts to determine the aqueous leachabuity of the waste for both inorganic and organic
constituents in a single leach test It is very difficult to conduct in a reproducible manner.
Mechanical problems with the test make it time consuming to perform and frequent
reanalysis is required. Precision between replicate tests is very poor. Equipment cleanup is a
major obstacle to laboratory productivity. Costs can run to several thousand dollars per
sample for difficult-to-handle samples. The major problems found in conducting the TCLP
are:
• Handling of the sample is messy, effecting weighing of proper amounts into
the extraction vessels. Loss of volatiles occurs.
• Proper sub-sampling of multi-phasic materials is difficult. Samples frequently
contain oil, water, and solids. Isolation of solids for extraction is arduous.
• The tumbling action of the two liter extraction vessels forms emulsions making
isolation of the aqueous leachate difficult
• Separation of the leachate from the solid residue after extraction is frequently
impossible because the oily material clogs the filter. This is especially serious
when using the zero headspace extractor (ZHE) since the test must be repeated
if this happens.
Presented on July U, 1992 at EPA Workshop H Page ZL
on "Predicting 'the Environmental Impact of Oily Materials"
-------
• Oily wastes frequently yield aqueous leachates and free organic material which
must be separated and analyzed separately, doubling or tripling the analytical
costs.
• Equipment cleanup is very time consuming, minor amounts of residual organic
material can carry over and contaminate succeeding samples.
These problems are sufficiently severe that both regulators and regulated community
have lost confidence in the utility of the method to estimate the potential environmental
hazard of oily wastes.
PROPOSED APPROACHES
This section discusses four proposed approaches to improving the technical and/or
procedural methods for determining the potential environmental impact of oily materials.
They are:
• Adopt a flowable materials test
Modify the TCLP.
• Adopt a new method of contacting the leach medium with the waste.
• Devise a new model for determining the amount of a regulated substance
released from an oily waste by aqueous leaching mechanisms.
Approach 1 - Flowable Materials Test
The EPA has laid the groundwork for a Flowable Materials Test (FMT) in the 1991
proposed rule making for the Liquid Release Test (LRT), EPA Method 90963. The Agency has
published two reports describing the test for its original application, namely to detect the
release of any free liquid from material destined for land disposal*-5. The test places a 76mm
diameter by 10mm high sample in a confined chamber under a 50 psi load for ten minutes to
force the release of free liquids.
If the device is modified to provide an tight fitting piston/barrel arrangement
(identical to the design of the zero headspace extractor, the ZHE) and the indicator paper
holder is replaced with a reinforced screen and fluid collection vessel, it will be capable of
applying the necessary degree of pressure to the sample necessary to simulate overburden
pressure. The screen will allow for the effective escape and collection of the flowable material
from the solid mass. Both the retained solids and the collected flowable material can be
analyzed separately using one or more of the suggested experimental changes described in
the following sections.
Presented an July 14,1992 at EPA Workshop H Page 22
on "Predicting the Environmental Impact of Oily Materials"
-------
Approach 2 - Modify the TCLP
Modification 1 - Addition of Inert Substrate.
One basic problem with the ability to conduct TCLP is the physical nature of oily
material and the impact that has on the conduct of the test as discussed above. The EPA has
addressed this type of problem in Methods 3540 and 35502, Soxhlet Extraction and Sonication
Extraction respectively, where inert adsorbents are added to the waste to provide a free
flowing material with sufficient permeability to allow for efficient extraction. Tne same
approach can be taken with the TCLP.
The addition of a high surface area, inert matrix like silica beads (or sand) will
effectively immobilize the free phase organic material and provide a free flowing medium for
sample preparation (sub-sampling) and extraction. The increased surface area will promote
solubilization of the organic components into the extraction medium. This approach will be
effective for both free liquids and oily solids. If an aqueous phase is also present, adsorption
of the oily material should facilitate separation of the aqueous material prior to extraction.
The presence of the substrate surface as a host site for oily material will minimize the
formation of emulsions during tumbling of the waste/leachant mixture, provided the
viscosity of the organic material is sufficiently high that the shear forces of the tumbling
action do not separate the liquid material from the solid. After the tumbling sequence, the
solid substrate and absorbed oily material will settle to the bottom of the leaching vessel and
eliminate or minimize the amount of free organic liquid floating at the surface of the
solution, making the filtration step much easier and clogging less likely.
This type of sorbent bed closely resembles the real world case of oily material spilled
onto or migrating through soil columns until it no longer moves under the force of gravity.
This model of oil coated soil represents the most common real world source of potential
pollutant release from oily wastes.
Modification 2 - Use of Fritted Stainless Steel Filter.
Regardless of whether or not the method is modified by the addition of an inert
substrate to immobilize the oily material, the filtration step of the method can be improved.
Agency funded research of improved filtration media led to the development of a sintered
stainless steel filter that overcame many of the dogging problems5. The modification has not
been added to the method at this time, but it has been used without formal regulatory
adoption, with some intractable wastes. Other approaches to improve filtering should be
examined, such as the use of thick pads (several mms) of non-woven glass or plastic fibers
and powdered filter aids as pre-filters. These are physical changes to the filter apparatus;
they should be permitted as long as the modifications can be shown not to alter the
composition of the filtrate by absorption of analytes or allow for the passage of particles with
a nominal size greater than 0.7 micron.
Presented on July 14,1992 at EPA Workshop U Page 23
on "Predicting the Environmental Impact of Oily Materials"
-------
Approach 3 - Adopt a New Leaching Technique
The mechanical forces that act on oily waste during the TCLP tend to separate the oil
from the substrate that was part of the original waste material or the inert material added in
Approach 2. This leads to the formation of emulsions and/or free liquid phases which coat
and dog the filters during the filtration step. Column leaching configurations that are less
physically aggressive than tumbling can be used as the leaching model for oily wastes. The
permeability of the waste material is the key property of the waste which must be controlled
if a column technique is to work (permeability also impacts the efficiency of any extraction
process). Use of inert sorbents, as in Approach 2, can provide the necessary permeability to
allow for uniform flow of the aqueous medium through the waste bed and promote effective
leaching. Uniform flow would be provided by pumping the leachant through the system.
Flow rates can be adjusted to minimize the shear forces which might dislodge oily
material from the waste. Flow direction can be changed based on the density of the organic
fluids. Downward flow for materials lighter than water and upward flow for materials
heavier than water will minimize the likelihood that oily material will separate from the
substrate during testing. If the fluids do separate, they will not find their way into the
leachate reservoir without passing through the substrate bed where they will re-deposit on
the surface. Minimum flow volumes per unit mass of waste will become the operational
control of the test rather than the tumbling time that is now used.
The dynamic flow conditions of the column test also allow for efficiencies in
subsequent sample analysis. Modern solid phase sorbents for both organic and inorganic
analytes can be placed between the pump outlet and the head of the column to collect and
pre-concentrate the analytes for future analysis. The use of these sorbents also allows the
introduction of "fresh leachant" to the top of the column of waste in a manner similar to the
way fresh ground or surface water would contact the waste in the real world scenario. This
would promote maximum release of the target analytes.
The column leach model proposed here resembles the real world case where ground
or surface water percolates through oily material that adheres to the soil, more closely than
does the rumbling action of the TCLP. The column leach approach can be extended to
evaluate the attenuation of solubilized materials by a representative soil, by placing a soil
layer in the same extraction column as the waste or by passing the leachate through a second
column placed in series with the waste containing column. This allows for the development
of a modular test sequence in which the same test used to characterize a waste leachate is
used as the source term for attenuation studies, which may be conducted as part of a site-
specific risk assessment. This strategy is in keeping with the SAB's recommendation to the
EPA.
Approach 4 - Use a Totally Different Leaching Model
The current TCLP and the two options previously discussed are alternative physical
models of the leaching process. Most problems resulting from these approaches center
around sample handling, leaching, and filtering the leachate. To avoid some of these
Presented an July 14,1992 at EPA Workshop E Page 24
on "Predicting the Environmental Imped of Ofly Materials"
-------
problems, the Agency should consider using well-developed, existing theoretical and
experimental models of the leaching of materials from oily matrices as well and the migration
and interaction of the soluble components with soils. Both the EPA and the American
Petroleum Institute (API) have published significant papers on the approach735-10-11. There
is ample experimental evidence that these models are a good first order approximation of the
amounts material actually found from aqueous leaching of oily materials. They apply to both
oily solids and flowable oily materials. The models depend on the amount of the target
analyte present in the waste, the analytes physical/chemical properties, and the chemical
properties of the soil. Some of the more important features of these models are discussed
below.
The American Petroleum Institute (API) published a review of historical data relating
fuel composition to the aqueous solubility of its various components7. The review
investigated the relationship between the solubility of the pure hydrocarbon components in
water and the amount found in aqueous solutions that had been allowed to equilibrate with
fuels (1:10 fuel/ water ratio). The study defined the partition coefficient for this process Kfv
by equation 1:
where: Cf = concentration of the component in the fuel, g/L
Cv = concentration of the component in the water, g/L
This property is related to the solubility of the pure component in water, S ', for a
group of six aromatic compounds by equation 2 which has a correlation coefficient of r =
0.99:
Log Kfv =- 0.884 log S + 0.975 (2)
As should be expected, the relationship between S and Kfv is a function of the class of
organic compounds being considered (aromatic, aliphatic, olefinic, etc.). When six additional
compounds, one aromatic, two olefinic, and three aliphatic, were considered, the best fit
equation describing the relationship between S and Kfv became
Log Kfv =- 1.018 log S + 0.706 (3)
and the correlation coefficient, r , dropped to 0.87. Table 1 compares the experimental data
for eleven of the compounds for which data was experimentally determined with the data
derived from equation 3. Most of the data compare favorably with the normal range of
allowable differences between replicate analytical determinations.
Presented on July 14,1992 at EPA Workshop H Page 25
on "Predicting the Environmental Impact of Oily Materials"
-------
TABLE 1
Comparison of Observed and Estimated Hydrocarbon Concentrations
from a Standard Gasoline in Equilibrium with Water (1:10)
HYDROCARBON
Benzene
Toluene
2-Butene
2-Pentene
Ethylbenzene
o-Xylene
m-Xylene
Butane
1 ,2,4-Trimethylbenzene
2-Methylbutane
Pentane
CONCENTRATION
OBSERVED
58.7
33.4
2.4
2.4
4.3
6.9
11.0
2.7
1.1
3.7
1.0
ESTIMATED
58.8
37.8
3.2
1.7
3.2
4.7
9.2
5.2
1.8
6.2
2.2
This type of model works well for those cases where the oily waste matrix is the
primary determinate in the partition coefficient in the matrix/water distribution. The 1984
API report discusses the situation where the amount of oil is very small compared to the
total mass of organic carbon in the soil/sediment/waste matrix and in effect represents oil
absorbed on soil6. Equation 4 applies to these situations.
where:
K,
oc
Kp =
(foc)
(4)
= soil/water partition coefficient
= the organic carbon partition coefficient
= weight percent organic carbon in the substrate.
Presented on July 14,1992 at EPA Workshop U
on 'Predicting the Environmental Impact of Oily Materials"
Page 26
-------
The organic carbon partition coefficient, Koc , is related to the octanol water partition
coefficient, Kov , by equation 5.
= log Kw- 0.317 (5)
These models are based on the physical and chemical properties of the target analytes
and the substrates with which they are associated, be it a flowable liquid, solid waste, or soil.
Accurate and precise methods exist for experimentally determining the input variables to the
models. These variables include but are not limited to:
• analyte concentration in total waste,
• percent organic carbon in soil or waste matrix,
• partition coefficients (fuel/water, soil/water, octanol/water), and
• water solubility of target analytes.
As the data base is expanded, relationships among classes of organic compounds, water,
soils, and wastes will emerge. These relationships will lead to better empirical and theoretical
understanding of the physical and chemical factors controlling the release of materials to the
environment. New materials can be evaluated without detailed experimental studies by
analogy with similar compounds, wastes, and soils.
Use of this type of approach helps fulfill the SAB's recommendation that more rigorous
scientific procedures be used to determine the potential for release as well as environmental
impact. This approach also meets the recommendation that rugged tests that are less
susceptible to waste matrix effects be used. The approach also uses many of the same
parameters used in determining fate and transport and important measures of environmental
risk; therefore, a more unified model of environmental impact can be developed.
ROLE OF THE EPA AND PUBLIC SECTOR GROUPS
The EPA can serve as a catalyst for the necessary research studies for needed to improve
and develop reliable analytical methods. EPA also can lead in measuring the important
physical and chemical properties, of the analytes, wastes, and soils, that define analyte
behavior in the environment. Members of the public sector can contribute laboratory support
and technical expertise to developing the necessary methodology and demonstrating the
applicability and ruggedness of the methods.
These workshops are an ideal expression of how this should work.
Presented on July 14,1992 at EPA Workshop U Page 27
on "Predicting the Environmental Impact of Oily Materials"
-------
REFERENCES
1. EPA Science Advisory Board. October, 1991. Leachability Phenomena,
Recommendations and Rationale for Analysis of Contaminant Release by the
Environmental Engineering Committee, Report EPA-SAB-EEC-92-003.
Z EPA, Test Methods for Evaluating Solid Wastes, Physical/Chemical Methods, SW-846,
3rd Edition, Final Update 1, November, 1990
3. ^Hazardous Waste Management: Containerized Liquids in Landfills. October 29,1991.
Federal Register, VoL 56, No. 209, p. 55646.
4. Hoffman, P.A. et. al.. Development of the Liquid Release Test. Research Triangle
Institute Report
5. Background Document for the Liquid Release Test (LRT): Single Laboratory
Evaluation and 1988 Collaborative Study. EPA RCRA Docket £ F-91-CLLA-FFFFF.
6. Truesdale, R£. et. al.. April 1990. Evaluation and Modification of Method 1311 for
Determining the Release Potential of Difficult-to-Filter Wastes. EPA Contract No. 68-
01-7075, Research Triangle Institute.
7. Karickhoff, S.W. and Brown, DS. 1979. Determination of Octanol/Water Distribution
Coefficients, Water Solubilities, and Sediment/Water Partition Coefficients for
Hydrophobic Organic Pollutants, EPA Report EPA-600/4-79-031
8. Reinbold, K.A. et. aL 1979-Adsorption of Ejiergy-Rejated-Organic Pollutants: A
Literature Review. EPA Report EPA-600/3-79-086.
9. Hassett, JJ. eL al 1980. Sorption Properties of Sediments and Energy Related
Pollutants, EPA Report EPA/3-80-041.
10. Environmental Research and Technology, Inc. 1984. The Land Treatability of
Appendix VIII Constituents in Petroleum Industry Wastes, API Publication No. 4379.
11. TRC Environmental Consultants, Inc. 1985. Laboratory Study on Solubilities of
Petroleum Hydrocarbons in Groundwater. API Publication No. 4395.
Presented on July 14,1992 at EPA Workshop U Page 28
on "Predicting the Environmental Impact of Oily Materials"
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Appendix VI
Office of Solid Waste Methods Section
Memoranda #35, #36
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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
WASHINGTON. D.C. 20460
OFFICE OF
SOLID WASTE AND EMERGENCY RESPONSE
MEMORANDUM I 36
DATE: January 12, 1993
SUBJECT: Notes on RCRA Methods and QA Activities
From: Gail Hansen, Chief yU&d
Methods Section (OS-331)
This memo addresses the following topics:
o 1992 Symposium on Waste Testing and Quality Assurance
o Issue Discussion Groups
o Inorganic Methods Workgroup Meeting
o Organic Methods Workgroup Meeting
o QA Workgroup Meeting
o Miscellaneous Methods Workgroup Meeting
o ICP Discussion Group
o HPLC Methods Discussion Group
o SPA Methods Discussion Group
o SFE Methods Discussion Group
o SW-846 Update and TCLP Spike Recovery Correction Removal
Notice Update
o Total Analysis Versus TCLP.
Printed on Recycled Paper
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The instrument manufacturers are working with the Agency to
determine the optimum SFE conditions for the major classes of
semivolatile analytes. This input will help expedite development
of a broader scope for Method 3560.
For further information on SFE topics, please contact Barry
Lesnik at (202) 260-7459.
SW-846 and TCLP Spike Recovery Correction Removal Notice
The final SW-846 Update I rule and the proposed Update II rule
packages are both currently at the Office of Management and Budget
(OMB) review step in the regulatory process. It is not known how
long this review step will take. Once the review by OMB is
complete, it is expected that the promulgation of Update I and the
proposal of Update II will take at least 2 months.
The rule to delete the matrix spike correction requirement
from the TCLP which was finalized on June 29, 1990, has been
published (57 FR 55114-56117, November 24, 1992). This rule
withdraws the spike recovery correction requirements from the TCLP
and, except for a few technical and format changes made in the June
29, 1990 rule revising the TCLP, returns the QA provisions of the
TCLP to those promulgated on March 29, 1990 (55 FR 11796).
Specifically, this rule requires the method of standard -additions
as the quantitation method for" metallic contaminants when-
appropriate as specified in the method.
For further information on SW-846 updates or the TCLP rule,
please give Kim Kirkland a call at (202) 260-6722.
Totals Analysis Versus TCLP
Over the past year, the Agency has received a number of
questions concerning the issue of total constituent analysis with
respect to the TCLP. Section 1.2 of the TCLP allows for a
compositional (total) analysis in lieu of the TCLP when the
constituent of concern is absent from the waste, or if present, is
at such a low concentration that the appropriate regulatory level
could not be exceeded. A number of persons have contacted the MICE
Service and have requested clarification on this issue with respect
to a number of waste testing scenarios.
Wastes that contain less than 0.5% dry solids do not require
extraction. The waste, after filtration, is defined as the TCLP
extract. The filtered extract is then analyzed and the resulting
concentrations are'.compared directly to the appropriate regulatory
concentration.
19
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For wastes that are 100% solid as defined by the TCLP, the
maximum theoretical leachate concentration can be calculated by
dividing the total concentration of the constituent by 20. The
dilution factor of 20 reflects the liquid to solid ratio employed
in the extraction procedure. This value then can be compared to
the appropriate regulatory concentration. If this value is below
the regulatory concentration, the TCLP need not be performed. If
the value is above the regulatory concentration, the waste may then
be subjected to the TCLP to determine its regulatory status.
The same principal applies to wastes that are less than 100%
solid (i.e., wastes that have filterable liquid). In this case
however, both the liquid and solid portion of the waste are
analyzed for total constituency and the results are combined to
determine the maximum leachable concentration of the waste. The
following equation may be used to calculate this value.
[AxB] + [CxD] p
[20-- x D]
where: A = concentration of the analyte in liquid portion of the
sample (mg/L)
B = Volume of the liquid portion of the sample (L) .
C = Concentration of analyte in the solid portion of the
sample (mg/kg)
D = Weight of the solid portion of the sample (kg)
E = Maximum theoretical concentration in leachate (mg/L)
To illustrate this point, the following example is provided:
An analyst wishes to determine if a lead processing sludge
could fail the TC for lead. The sludge is reported to have a low
concentration of lead, and the analyst decides to perform a
compositional analysis of the waste instead of a full TCLP
evaluation. A representative sample of waste is subjected to a
preliminary percent solids determination as described in the TCLP.
The percent solids is found to be 75%. Thus, for each 100 grams of
this waste filtered, 25 grams of liquid and 75 grams of solid are
obtained. It is assumed for the purpose of this calculation that
the density of the filterable liquid is equal to one. The liquid
and solid portion of the sample are then analyzed for total lead.
The following dat4 are generated:
20
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Percent solids = 75%
Concentration of lead in the liquid phase = 0.023 mg/1
Volume of filtered liquid = 0.025 L
Concentration of lead in the solid phase = 85 mg/kg (wet weight)
Weight of the solid phase = 0.075 kg.
The calculated concentration is as follows:
x 0.025L] + [85-^2 x 0.075kg]
, _ kg _ _ mg
0.025 L+ [20~ x 0.075Jcg] L
kg
In this case, the maximum leachable concentration is below the
5 mg/1 regulatory concentration for lead, and the TCLP need not be
performed.
Non-aqueous based wastes (i.e., oily wastes) may be calculated
in-the same manner as described above, except the concentration of
constituents from the liquid portion of the waste (A in the above
formula) are expressed in mg/kg units. Volumes also would be
converted to weight units (kg). The final leachate concentration
is expressed in mg/kg units.
21
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I tW? 3 UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
\^y»y WASHINGTON, D.C. 20460
OFPICE OF
SOLID WASTE AND EMERGENCY RESPONSE
MEMORANDUM * 35
DATE: June 12, 1992
SUBJECT: Notes on RCRA Methods and QA Activities
From: Gail Hansen, Chief
Methods Section (OS-331)
This merao addresses the following topics:
• o 1992 Symposium on Waste Testing and Quality
Assurance
o sw-846 Update
- Final Rule for January 23, 1989 Proposed Rule
- Notice, Proposed Rulemaking for the Second Update to
the Third Edition
o Chlorof luorocarbon 113 (CFC-113) Solvent Replacement
Update
O Environmental Monitoring Methods Index (EMMI)
o Sampling Work Group Formation
o MICE Update
o Oily Waste Analysis
o Electronic SW-846 Availability.
Printed on Recycled Paper
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Oily Waste Analysis
One of the most frequently asked questions on the MICE
Service concerns the application of the TCLP, Method 1311, to
oily wastes. Many callers request technical guidance on the
extraction of oily wastes due to the difficulty in the filtration
on these types of waste. In many cases, an oily waste does not
filter completely due to premature clogging of the glass fiber
filter. This can result in the retention of standing liquid on
the glass fiber filter. Material that do not pass through the
glass fiber filter at the conclusion of the filtration step is
defined by the method as the solid phase of the waste. The solid
phase is then subjected to the leaching procedure of the TCLP.
For oily wastes, clogging of the glass fiber filter can result in
an overestimation of the amount of solid material available for
leaching.
To solve this problem, the Agency recommends a conservative
approach, one that probably will overestimate the amount of
leaching. Rather than performing the TCLP extraction on the
unfiltered portion of the oily waste, assume the waste is 100%
liquid (e.g., will pass through the glass fiber filter) and
perform a totals analysis on the oily waste to determine if the
oil exceeds the appropriate regulatory level.
Filterable waste oil generated during the TCLP must be
analyzed for a'-variety of organic and inorganic analytes. The
OSW recognizes the difficulty in achieving acceptable performance
for the analysis of waste oil using methods currently provided in
SW-846. As a result, the Agency will provide several new methods
for the preparation and analysis of oil samples to the Organic
Methods Workgroup in July. In addition, a microwave assisted
digestion procedure should improve the analysis of metals and
will be proposed as part of the Second Update of the Third
Edition of SW-846. Brief descriptions of these techniques are
provided below, for additional information on the organic
procedures contact Barry Lesnik at (202) 260-7459. For
additional information on microwave digestion contact Ollie
Fordham (202) 260-4778.
The use of purge-and-trap (Method 5030) for volatiles in oil
generally results in severe contamination of analytical
instrumentation. Traps, transfer lines and chromatography
columns may become contaminated with oil. This leads to elevated
baselines, hydrocarbon background in subsequent analyses, and
cross-contamination. Headspace (Method 3810) is currently
allowed only as a screening procedure in SW-846. The Agency is
evaluating the usfe of headspace in conjunction with isotope
dilution mass spectrometry for the quantitative analysis of
volatiles in oil. Headspace reduces interference problems
encountered with purge-and-trap. However, headspace quantitation
can be questionable because the distribution of analytes is not
10
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the same in different types of samples. That difficulty appears
to be minimized by the use of isotope dilution calculations.
Headspace/isotope dilution analysis will require the promulgation
of two new SW-846 methods: Method 5022, Volatiles by Automated
Headspace, and Method 8266, Volatiles by Isotope Dilution GC/MS.
Performance data for the analysis of motor oil will be presented
to the Organics Workgroup and during a platform talk at the July
Symposium. Draft methods should be available for limited
distribution by September.
Headspace/isotope dilution will require that laboratories
acquire hardware and provide additional analyst training.
Therefore, an alternate Solvent Dilution Direct Injection (Method
3585) option for Method 8260 is also being evaluated. While use
of the direct injection technique will result in more instrument
contamination, it may be appropriate for laboratories that
analyze only a limited number of oil samples. Method performance
data will also be presented for direct injection during the
symposium in July.
The analysis of semi-volatile target analytes is also
difficult with present methods. While gel permeation cleanup
(GPC) is effective, it can only be used for small oil samples
(<0.5 g). Work is in progress to evaluate partition and
extraction cleanup procedures for waste oil. Partitioning oil
between dimethyl formamide (DMF) and hexane or extraction of oil
with methanol/DMF followed by acid/base partitioning has proved
successful prior to the analysis of chlorophenols in waste oil.
A similar approach is being evaluated for the analysis of
organochlorine pesticides. Work to date has demonstrated that
steam distillation and vapor/vapor extraction procedures are not
appropriate for petroleum products.
The Agency will propose a new digestion procedure (Method
3051) for inorganic samples in the Second Update of the Third
Edition of SW-846. The procedure uses a microwave oven to heat
the acid during digestion of sediment, sludge, soil and oil
samples. The resulting digestate can be analyzed using atomic
absorption (AA) or inductively coupled plasma (ICP) methods in
SW-846. Microwave assisted digestion is suitable for all oils
including oils that contain particulates. The only current
inorganic preparation method suitable for oils is Method 3040, a
dissolution procedure. In contrast to Method 3051, Method 3040
is suitable only for metals dissolved in oil. Method 3040 can be
used to show that an oil is hazardous based on the concentrations
of dissolved metals.
Electronic SW-846
0
SW-846 now can be purchased from private vendors in an
electronic format. A brief description of each known package and
information on how to obtain copies of each are given below.
11
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The SW-846 Authority is published in electronic format by
Virtual Media Corporation. The SW-846 Authority is an
comprehensive electronic publication designed to track and manage
regulatory issues. By using IQTP (Intelligent Query Text
Processor), the SW-846 Authority utilizes a comprehensive index,
allowing users full text and retrieval capabilities. Users have
access to thousands of EPA generated regulatory documents and
official notices, including the full text of Federal Register
Preambles. Other features of the SW-846 Authority include:
• RCRA Act (SWDA)
• RCRA 40 CFR Parts 260-265, 270-272
• SW-846 Solid Waste Test Methods Manual
• RCRA Inspection Manual.
For information on the SW-846 Authority call (800) 645-4130
or write to:
Virtual Media Corporation
14455 North Handen Road, Suite 201
Scottsdale, AZ 85260
Electronic E.P'.A. Methods*0 1.1 is offered by Chemsoft*3
Corporation as--an electronic database of all EPA methods. This
program is designed for rapid search and retrieval of EPA methods
by method number, analyte, title, type of instrumentation, or CAS
number. Each program contains the full text of the methods as
they appear in the appropriate EPA manual. Use of this software
requires Windows 3.0. The following programs are available
either separately or may be purchased as a single package:
• EPA SW-846 Series Methods
• EPA 500 Series Methods
• EPA 600 Series Methods
• EPA Water and Waste Methods.
For further information on Electronic E.P.A. Methods, call
(800) 536-0404 or (707) 864-0845 or write to:
WindowChem Software, Inc.
1955 West Texas Street, Suite 7-288
Fairfield, CA 94533-4462
The Methods Section will provide additional information in
future memoranda on other sources of electronic SW-846 media when
we become aware of them.
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Appendix VII
Recommendations and Rationale for Analysis of
Contaminant Release by the Environmental
Engineering Committee
Science Advisory Board
October 1991
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United States Science Advisory Board EPA-SAB-EEC-92-003
Environmental Protection (A-101F) - October 1991
Agency
ve/EPA Leachability
Phenomena
Recommendations and
Rationale for Analysis of
Contaminant Release by the
Environmental Engineering
Committee
A) Printed on Recycled Paper
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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
WASHINGTON. D.C. 20460
EPA-SAB-EEC-92-003
OFFICE OF
THE ADMINISTRATOR
October 29, 1991
Honorable William K. Reilly
Administrator
U.S. Environmental Protection Agency
401 M Street, E.H.
Washington, D.C. 20460
Subject: Leachability: Recommendations and Rationale
for Analysis of Contaminant Release
Dear Mr. Reilly:
The Leachability Subcommittee (LS) of the Science Advisory
Board's Environmental Engineering Committee (EEC) has prepared
the attached recommendations and rationale on leachability, an
important release term related to solid wastes and contaminated
soils, for your consideration.
Over the past decade, the EEC has reviewed a number of EPA
issues involving leachability phenomena and noted several
problems relating to this release term that were common to a
variety of EPA offices. The Committee believed that these common
problems would be best called to the Agency's attention through a
general review of leachability phenomena.
Drafts of this report on leachability have been reviewed at
a series of Subcommittee, Committee, and Executive Committee
meetings over the past 18 months. This included both a session
on February 26, 1990, devoted to assessing the Agency's varied
needs on leachability-related information, and a Technical
Workshop on May 9, 1990. The workshop assisted in determining
how leachability phenomena should be used to determine how a
waste will leach when present under various scenarios in the
environment.
The following recommendations have been developed. First,
in regard to leachability test development we recommend:
a) incorporation of research on processes affecting
leachability into EPA's core research program to better define
and understand principal controlling mechanisms,
b) development of a variety of contaminant release tests,
rather than focusing on mimicking a single scenario,
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c) development of improved release and transport-
transformation models of the waste matrix to complement the
leaching tests/ and
d) field validation of the tests and models, and
establishment of release-test accuracy and precision before tests
are broadly applied.
Next, in regard to the application of such tests and models/
ve recommend:
e) use of a variety of contaminant release tests and test
conditions which incorporate adequate understanding of the
important parameters that affect leaching in order to assess the
potential release of contaminants from sources of concern. A
medical analogy is that no physician would diagnose on the basis
of one test showing only one aspect of the problem/
f) development of a consistent/ easily applied/ physical/
hydrologic/ and geochemical representation for the phenomenon or
vaste management scenario of concern/
g) identification and application of appropriate
environmental conditions for tests in order to evaluate long-term
contaminant release potential as required under varying statutes/
and
h) coordination between the Agency's programs which develop
leachability tests with those that develop the environmental
models in which the release terms are used.
Finally/ we recommend:
i) establishment by the Agency of an inter-office/ inter-
disciplinary task group/ including ORD to help implement these
recommendations/ and
j) development of an Agency-wide protocol for evaluating
release scenarios, tests/ procedures/ and their applications.
These recommendations are made with the anticipation that an
improved understanding of the fundamental scientific principles
that control contaminant release and transport within a waste
matrix will allow better regulatory and technical decisions to be
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made in cases where the potential exists for leaching of
contaminants into the environment.
We are pleased to be of service to the Agency, and hope that
you will find this effort useful. We look forward to your
response to the recommendations cited above.
Dr. Raymond C. Loehr, Chairman Kr. Richard A. Conway, Chairman
Executive Committee Environ. Engineering Committee
Dr. C. H. Ward, Chairman
Leachability Subcommittee
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ABSTRACT
The Leachability Subcommittee (LS) of the Environmental
Engineering committee (EEC) of the EPA Science Advisory Board
(SAB) conducted a self-initiated study and prepared a report on
the topic of leachability phenomena. The intent of this report
is to provide recommendations and rationale for analysis of
contaminant release to the staff in the various offices of the
Environmental Protection Agency (EPA). The nine recommendations
from the report are highlighted as follows:
1) A variety of contaminant release tests and test condi-
tions vhich incorporate adequate understanding of the important
parameters that affect leaching should be developed and used to
assess the potential release of contaminants from sources of
concern.
2) Prior to developing or applying any leaching tests or
models/ the controlling mechanisms must be defined and
understood.
3) A consistent, replicable and easily applied/ physical,
hydrologic, and geochemical representation should be developed
for the vaste management scenario of concern.
4) Leach test conditions (stresses)- appropriate to the
situations being evaluated should be used for assessing long-term
contaminant release potential.
5) Laboratory leach tests should be field-validated/ and
release test accuracy and precision established before tests are
broadly applied.
6) More and improved leach models should be developed and
used to complement laboratory tests.
7) To facilitate the evaluation of risk implications of
environmental releases/ the Agency should coordinate the
development of leach tests and the development of models in vhich
the release terms are used.
8) The Agency should establish an inter-office/ inter-
disciplinary task group, including ORD to help implement these
recommendations and devise an Agency-vide protocol for evaluating
release scenarios, tests, procedures/ and their applications.
9) Core research on contaminant release and transport vithin
the vaste matrix is needed.
Key Words; leachability, leachability phenomena/ leach tests and
methods, leaching chemistry, leaching models
ii
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I. EXECUTIVE SUMMARY
In vaste management, including managing the effects of
spills or other releases which are sources of underground
contamination, a critical issue is the assessment of the
potential for constituents to leach to the environment. The
Environmental Engineering Committee (EEC) of the Science Advisory
Board (SAB) undertook a study of this issue because it noted
several common problems relating to this release term as it
reviewed, over the past decade, various leaching tests and risk
models for several EPA offices. Tests such as the Extraction
Procedure (EP) and the Toxicity Characteristic Leaching Procedure
(TCLP) had, and continue to have, scientific limitations, yet
were being inappropriately and in some cases widely used. Often
tests were developed without rigorous review. A self-initiated
study seemed appropriate to define the leachability problem
better and to offer advice on its resolution.
The EEC established a Leachability Subcommittee (LS) that
addressed:
1) Needs of the Agency and regulated communities to
quantify leachability (releases) of contaminants to the
environment.
2) State-of-the-art and science related to fundamental
principles and practice in predicting leaching of constituents
from wastes, contaminated soils, and other sources.
3) Recommendations to improve the scientific understanding
and application of leaching tests.
Workshops were held, literature was analyzed, and
findings were discussed over an 18-month period leading to the
preparation of this report.
The various needs for tests and models to predict leaching
are defined. Tests developed and used in the U.S. and Canada are
summarized. The scientific considerations important in design
and interpretation of leachability tests are presented. This
information, expert advice and analysis by workshop participants,
and reviews by SAB members, resulted in guidance which should, if
progressively implemented, significantly strengthen the Agency's
ability to assess appropriately leaching of contaminants from
hazardous wastes, contaminated soils and other sources.
This guidance, in the form of nine recommendations, is
summarized as follows:
»
t
1) A variety of contaminant release tests and test
conditions which incorporate adequate understanding of the
important parameters that affect leaching should be developed
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and used to assess the potential release of contaminants from
sources of concern.
2) Prior to developing or applying any leaching tests or
models, the controlling mechanisms .must be defined and
understood.
3) A consistent, replicable and easily applied, physical,
hydrologic, and geochemical representation should be developed
for the vaste management scenario of concern.
4) Leach test conditions (stresses) appropriate to the
situations being evaluated should be used for assessing long-term
contaminant release potential.
5) Laboratory leach tests should be field-validated, and
release test accuracy and precision established before tests are
broadly applied.
6) More and improved leach models should be developed and
used to complement laboratory tests.
7) To facilitate the evaluation of risk implications of
environmental releases, the Agency should coordinate the
development of leach tests and the development of models in which
the release terms are used.
8) The Agency should establish an inter-office, inter-
disciplinary task group, including ORD, to help implement these
recommendations and devise an Agency-vide protocol for evaluating
release scenarios, tests, procedures, and their applications.
The task group should also be charged vith recommending vhat the
appropriate focal point(s), responsibilities, and organizational,
budgetary and communication links should be vithin the Agency for
the most effective, continued and ongoing support and pursuit of
the research, development and utilization of methods and
procedures.
9) Core research on contaminant release and transport vithin
the vaste matrix is needed.
II. INTRODUCTION
In both hazardous and non-hazardous vaste management, one of
the most critical issues is the assessment of the potential for
constituents contained in the source material to leach or
otherwise be released to the environment. Approaches to estimate
potential release of organic and inorganic constituents and their
subsequent environmental migration and associated health risks
are important in many situations (e.g., pollution prevention,
risk reduction, restoration-remediation and hazard identi-
fication) .
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Appendix VIII
USEPA Region II
Special Analytical Services Request
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SAS Number
U.S. ENVIRONMENTAL PROTECTION AGENCY
CLP Sample Management Office
P.O. Box 818 - Alexandria, Virginia 22313
Phone: (703) 557-2490 - (FTS) 557-2490
SPECIAL ANALYTICAL SERVICES
Client Request
EH '
1 ' Regional Transmittal ' ' Telephone Request
A. EPA Region/Client:
B. RSCC Representatives:.
C. Telephone Number: (_
D. Date of Request:
E. Site Name:
Please provide below description of your recent request for
Special Analytical Services under the Contract Laboratory
Program. In order to most efficiently obtain laboratory
capability for your request, please address the following
considerations, if applicable. Incomplete or erroneous
information may result in a delay in the processing of your
request. Please continue response on additional sheets, or
attach supplementary information as needed.
1. General Description of Analytical Service Requested:
Analysis of soil samples by TCLP for TC analytes.
Analysis of aqueous blanks for TC analytes.
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2. Definition and number of work units involved (specify
whether whole samples or fractions; whether organics or
inorganics; whether aqueous or soil and sediments; and
whether low, medium, or high concentration):
Number of Samples
Matrix
Concentration
Analysis
Soil
Low
TCMplus
pyridene
and m-
cresol),
TAL,
2,4-D and
2,4,5-TP
by TCLP
Water
Field
Blank
Low
TCL(plus
pyridene
and m-
cresol),
TAL,
2,4-D and
2,4,5-TP
3. Purpose of analysis (specify whether Superfund (Enforcement
or Remedial Action), RCRA, NPDES, etc.):
4.
Estimated date(s) of collection:
5. Estimated date(s) and method of shipment:
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6. Number of days analysis and data required after laboratory
receipt of samples:
Environmental samples must undergo TCLP extraction within
the following time periods after sample receipt:
Mercury 26 days
Other Metals 178 days
Volatiles 12 days
Pest/Herb/BNA 12 days (7 additional days
from TCLP extraction to
preparative extraction)
Environmental TCLP sample extracts must be analyzed within
the following time periods after extraction:
Mercury 28 days
Other Metals 180 days
Volatiles 14 days
Pest/Herb/BNA 40 days
Field and trip blanks must be analyzed within the following
time periods after sample receipt:
Mercury 26 days
Other Metals 6 months
Volatiles 10 days
Pest/Herb/BNA 5 days to extraction,
40 days to analysis
The complete data package containing all the sample delivery
groups (SDG) associated with this case must be submitted as
one data package in its entirety within 35 days from the
verified time of receipt of the last sample in this case.
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7. Analytical protocol required (attach copy if other than a
protocol currently used in this program):
Parameter
TCLP Metals
TCLP VOAs
TCLP BNAs
TCLP Pest
TCLP Herb
Metals
VOAs
BNAs
Pest
Herb
Matrix
soil
soil
soil
soil
soil
water
water
water
water
water
Preparation
57 FR 55114
57 FR 55114
57 FR 55114
57 FR 55114
57 FR 55114
Analysis
CLP ILM03.0
CLP OLM01.8
CLP OLM01.8
CLP OLM01.8
SW-846 8150A
CLP ILM03.0
CLP OLM01.8
CLP OLM01.8
CLP OLMQ1.8
SW-846 8150A
Only the 39 TC analytes shall be reported.
Revision l of Method 8150A, dated November 1990, shall be used to
analyze herbicides.
8. Special technical instructions (if outside protocol
requirements, specify compound names, CAS numbers, detection
limits, etc.):
All Fractions
If dilutions are necessary due to an analyte being out of
calibration range, they must be done in increments of 10.
The raw data of all the dilutions must be provided; the
final result of the analyte shall be calculated from the
least dilution that would bring the analyte concentration
within the calibration range.
A TCLP blank must be carried through the extraction,
digestion, and analytical procedures.
The maximum number of samples in a sample delivery group
(SDG) is 20.
Field blanks and trip blanks do not require MS/MSB. The
matrix spike shall be added to the TCLP extract, not the
environmental sample.
Metals
All of the TC metals, except mercury, shall be analyzed on
the TCP. The CRDLs for the TC metals shall be twenty times
the CRDL in the current SOW, except for mercury, which will
be two hundred times higher. The matrix spike analytes will
be spiked at five times the contract specified
concentrations.
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The TCLP Section 8.4 criteria for method of standard
additions shall be followed.
Organics
Volatile and semi volatile TCL fractions will be diluted
five times before analysis, which will increase the CRQLs by
a factor of five. Pesticides will be diluted ten times .
before analysis, which will increase the CRQLs by a factor
of ten. The TCL surrogates will be spiked at five times the
contract specified concentrations. The TCL matrix spike
analytes shall consist of all the TC analytes except
toxaphene, and shall be spiked at ten times the contract
specified concentrations.
When analyzing BNA samples, the 2/88 CLP extraction
procedure must be used. Initial and continuing
calibrations are required for pyridine and m-cresol.
There are no calibration acceptance criteria for pyridine or
m-cresol.
Herbicides
Follow requirements in 8150A and 8000A.
Analytical results required (if known, specify format for data
sheets, QA/QC reports. Chain of Custody Documentation, etc). If
not completed, format of results will be left to program
discretion.
The following TCLP deliverables shall be supplied:
1. The TCLP and preparative extraction dates and analyses
dates. Data to justify selection of TCLP extraction
fluid.
2. A physical description of the samples.
3. The sample weights and the extraction fluids weights.
4. The final volume of TCLP extract and the volume of
extract analyzed.
5. The calculations used to compute percent dry solids and
the weight of the liquid phase (if applicable).
6. Extraction logs for each sample, indicating the volume
and pH of acid added. Were inorganic sample extracts
properly preserved?
7. A description of the materials of construction for
extraction vessels, filtration devices, and ZHE
extraction devices (i.e. glass, Teflon, PVC, stainless
steel etc.).
8. The calculations used to compute TCLP extract
concentrations for multiphasic samples.
9. When VOA samples consist of oily waste that cannot be
filtered, describe how the TCLP extract is separated
from the oily waste.
10. A copy of the sampling log.
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11. Any evidence of leakage in the ZHE device.
A TCLP bank must be analyzed in addition to method blanks.
The following analytical results shall be submitted for
Method 8150 A analysis:
The laboratory must submit all documentation including: SAS
packing lists, traffic reports, chain of custody forms, and
sample preparation information. Analytical and QC results
shall be submitted on the following modified CLP/SOW
pesticide forms: Form I (Analytical Results), Form II
(Surrogates), Form III (Matrix Spikes), Form IV (Method
Blank), Form VI (Initial Calibration), Form VII (Calibration
Verification), Form VIII (Analytical Sequence) and Form X
(Identification Summary). All QA/QC information, including
laboratory generated standards and sample chromatograms,
must be submitted. A written narrative describing problems
encountered in receipt or during analysis and corrective
actions taken (including telephone logs, etc.) must be
provided. All documents (modified CLP forms, raw data,
etc.) related to re-extraction/re-analysis must also be
submitted in its entirety.
10. Other (Use additional sheets or attach supplementary
information, as needed):
The following requirements apply to method 8150A:
The laboratory must supply any information required to
reproduce, during independent data review, all results
reported by the laboratory. The laboratory must supply a
detailed example calculation that clearly demonstrates the
manner in which the initial and final results were derived.
Where applicable, each component of the calculation must be
explained (e.g., if the calculation include a dilution
factor, it must be specified how each dilution occurred).
11. Name of sampling/shipping contact:
Phone: ( )
12. Data Requirements
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For VOAs, BNAs, pesticides and metals, follow CLP criteria.
The following requirements apply to 8150A herbicide
analysis:
Parameter
2,4-D
2,4,5-TP
Detection Limit
As per method
8150A
Precision Desired
As per method
8150A
Estimated Quantitation Limits (EQL) can be computed from
Table 1 & 2 of method 8150A for various parameters.
13. QC Requirements
For VOAs, BNAs, pesticides, and metals, follow CLP criteria.
The following requirements apply to 8150A herbicide
analysis:
Audits Required
Initial Calibra-
tion
Continuing(mid-
level std) Cal-
ibration
Surrogate
Method Blank
Duplicate
Matrix Spike
Frequency of Audits
See Method 8000A
Every 10 samples
All samples, etc.
1 per 20 samples
1 per 20 samples
1 per 20 samples
Limits
(% or Concentration)
%D
50-120% Recovery
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14. Action Required if Limits are Exceeded
For VOAs. BNAs. pesticides, and metals, follow CLP protocol
For 8150A. reextract and reanalyze.
Please return this request to the Sample Management Office as
soon as possible to expedite processing of your request for
special analytical services. Should you have any questions, or
need any assistance, please contact your Regional representative
at the Sample Management Office.
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•o
•o
m
z
D
X
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Appendix IX
Office of Solid Waste Methods Section
Required Uses of SW 846
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The following information regarding required uses of SW-846
was compiled by the Methods Section, OSW, U.S. EPA Headquarters:
Several of the hazardous waste regulations under Subtitle c
of RCRA require that specific testing methods described in SW-846
be employed for certain applications. Any reliable analytical
method nay be used to meet other 'requirements in 40 CPR Parts 260
through 270. For the convenience of the reader, the Agency lists
below a number of the sections found in 40 CPR Parts 260 through
270 that require the use of a specific method for a particular
application, or the use of appropriate SW-846 methods in general:
(1) S 260.22(d>(1)(i) - Submission of data in support of
petitions to exclude a waste produced at a particular
facility (j..e. . delisting petitions) ;
(2) § 261,22(a)(l) and (2) - Evaluation of waste against
the corrosivity characteristic;
(3) § 261.24(a) - Leaching procedure for evaluation of
waste against the toxicity characteristic;
(4) SS 264.190(a), 264.314(C), 265,190(a), and 265.314(d) -
Evaluation of waste to determine if free liquid is a
component of the waste;
(5) § 266.112(b)(1) - Certain analyses in support of
exclusion from the definition of a hazardous waste of a
residue which was derived from burning hazardous waste
in boilers and industrial furnaces;
(6) § 268.32(i) - Evaluation of a waste to determine if it
is a liquid for purposes of certain land disposal
prohibitions;
(7) §§ 268,40(a), 268.41(a), and268.43(a) -Leaching
procedure for evaluation of waste to determine
compliance with Land Disposal treatment standards;
(8) SS 270.19(c)(1)(iii) and (iv), and 270.62(b)(2)(i)(C)
and (D) - Analysis and approximate quantification of
the hazardous constituents identified in the waste
prior to conducting a trial burn in support of an
application for a hazardous waste incineration permit;
and
(9) SS 270.22(a) (2) (ii) (B) and 270..66(c) (2) (i) and (ii) -
Analysis conducted in support of a destruction and
removal* efficiency (ORE) trial burn waiver for boilers
and industrial furnaces burning low risk wastes, and
analysis and approximate quantitation conducted for a
trial burn in support of an application for a permit to
burn hazardous waste in a boiler and industrial
furnace.
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