QUALITY ASSURANCE MANUAL FOR
WASTE MANAGEMENT BRANCH INVESTIGATIONS
Prepared by the Regional Quality Assurance Management Office
USEPA Region 10, in cooperation with the
Waste Management Branch
February, 1986
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To Users of the Quality Assurance Manual For Waste Management Branch Investigations:
The following is an initial list of errata found in the initial copies of this manual. If,
in use or review of this document, additional ones are found, please notify Roy R. Jones in
the Regional Quality Assurance Management Office so they may he corrected with the
first revision tentatively scheduled for May or June, 1986. If major changes or new
references should be noted, please give the RQAMO as much lead time as possible for
inclusion and/or further errata notice. Thank you for your patience, cooperation and
assistance in developing this manual.
Errata as of 2/12/86
Sect. V, pg 1, last sentence; change " Sample Management Office (SMO)" to Regional
Sample Control Center (RSCC)
Sect VIII, pg 2, 1 st. paragraph; should read "...found in Section XVI."
Sect.X, pgs.4 & 5, part E.; should read "RSCC NOTIFICATION AND REPORTING", with
RSCC replacing "laboratory" in subsequent 2 paragraphs. ALSO, delete SS from SSQAP in
last sentence of 2 nd. paragraph.
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SECTION
I.
n.
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IV.
V.
VI.
VII.
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IX.
X.
XI.
XII.
XIII.
XIV.
XV.
XVI.
XVII.
XVIII.
XIX
Appendix A:
Appendix B:
Appendix C:
Section No.
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TABLE OF CONTENTS
TITLE
Title
Table of Contents
List of Tables
List of Figures
Introduction
Project Description
Project Organization and Responsibilities
Objectives for Measurement Data
Sampling Procedures
Sample Custody and Documentation
Calibration Procedures and Frequency;
Preventative Maintenance
Analytical Procedures
Data Reduction, Validation, and Reporting
Internal Quality Control Checks
Performance and System Audits
Specific Routine Procedures Used to Assess Data
Precision, Accuracy, and Completeness
Corrective Action
Quality Assurance Reports to Management
Safety
Glossary of Terms
40 CFR Part 261
Model Quality Assurance Project Plan (QAPP)
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1 LIST OF TABLES
TABLE # TITLE
1 Persons Responsible for QA Activities
2 Example of Data Quality Objectives
for RCRA Measurement Data
3 Example of Sample Container and
Preservation Methods
4 Example of Methods for RCRA Analysis
5 Level of Effort for QA Samples
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SECTION PAGE
VII 3
VIII 3
IX 4
XII 2
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Section No. IV
IV. LIST OF FIGURES
FIGURE # TITLE
1 Project Organization
2 Chain of Custody Record
3 Examples of Custody Seals
4 Analysis Required Sheet-Water
5 Analysis Required Sheet-Sediment
6 Field Sample Data Sheet,
with Chain of Custody
7 Metals Analysis Required-Water
8 Pesticide Analysis Required-Water
9 Organics Traffic Report
10 Inorganics Traffic Report
11 High Hazard Traffic Report
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Section No. V
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V. INTRODUCTION
The Environmental Protection Agency (EPA) Region 10, Waste Management Branch
(WMB) administers implementation of the Resource Conservation and Recovery Act
(RCRA, see Appendix B, "40 CFR Part 261) and oversees compliance monitoring of
hazardous waste handling facilities. This includes on-site technical and field investigation
aimed at assessing compliance with permit requirements. An effective multidisciplinary
technical and field investigation program requires a definitive quality assurance (QA)
program coupled with efficient scheduling of all resources. The nature of the field
investigation as well as the combination of sampling and laboratory activities make QA of
all collected data critical. To obtain quality data that are scientifically and legally
defensible, and to have the requisite levels of precision and accuracy with minimum
expenditures of resources, requires the development of a comprehensive and
well-documented Quality Assurance Project Plan (QAPP).
The guidelines and procedures for quality assurance of data gathering, analysis, and
reporting under the RCRA Program are covered in this Quality Assurance Manual. This
manual describes those procedures which ensures the collection of data of adequate
quality to meet project objectives.
Specific guidelines and activities that are addressed include: sampling procedures;
sample custody; calibration procedures; analytical procedures; and data
analysis/reduction, validation, and reporting. The plan also addresses internal quality
control checks; performance and system audits; quality assurance reports to management;
preventive maintenance; corrective actions; and assessment of data precision, accuracy,
and completeness.
It will be necessary to prepare a WMB/RCRA specific QA project sampling plan for
each project that includes monitoring and measuring activities that generate and process
environmental data. Appendix C provides an example of format for preparing all types of
QAPPs. It can be utilized by simply "filling in the blanks" for routine and screening
efforts or expanded for developing a comprehensive plan for major data acquisition
efforts. This model addresses all essential elements called for in national agency
guidance and regulations
Each QAPP will be reviewed by appropriate Environmental Services Division (ESD)
peer revicwer(s), and when concurred with by the Regional Quality Assurance
Management Office (RQAMO), will serve as an authorization to assign Laboratory sample
numbers and other ESD resources. It cannot, be too strongly emphasized, that, except for
unique emergency response situations, the QAPP must be completed prior to the
initiation of sample collection. Finally, the QAPP will serve as the basic tracking
document for the project managers, the RQAMO, and the Sample Management Office
(SMO).
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Section No.
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VI. PROJECT DESCRIPTION
Data generated from the samples that are analyzed using the QA procedures
described in this manual will primarily he used for RCRA and solid waste permits,
compliance and enforcement cases. Data generated will he used for monitoring activities
related to:
Generation
Treatment
Storage
Disposal
Closure (e.g. specific sites)
Unregulated Discharges (e.g. spills)
PA/SI's
Permit Development
Case development
Corrective Action Development
SWMU's
Data will also he generated from hoth compliance, enforcement, and routine
surveillance activities covering hazardous waste facilities. These data will he used for
facility plan evaluation, and information, education and technical assistance in
professional development programs.
Under 40 CFR Part 261 (Appendix B) of the RCRA regulations, a listing of hazardous
materials is provided. This part also requires analyses to he performed by methods
provided in SW-846 "Test Methods for Evaluating Solid Waste; Physical/Chemical
Methods" . However, SW-846 does not provide methods of analysis for every material
listed as hazardous in 40 CFR Part 261. As new procedures are added to SW-846, the
laboratory will develop procedures the same as in SW-846 to perform these analyses. All
groundwater sampling and analysis procedures also currently follow either SW-846, the
EPA 600 series, or SW-611. This will be continued until such time as EPA promulgates
groundwater monitoring in SW-846.
The specific parameters addressed by this plan are as follows:
Ignitability
Corrosivity
Reactivity
EP Toxicity
Volatile Organics-
Semi-volat ile Organics
Polynuclear Aromatic
Hydrocarbons
Total and Amenable Cyanide
TOX
Su I fides
pH
Antimony Halogenated Volatile Organics
Arsenic Nonhalogenated Volatile Organics
Barium Aromatic Volatile Organics
Cadmium Acrolein, Acrylonitrile, Acetonitrile
Chromium Phenols
Lead Phthalate Esters
Mercury Organochorine Pesticides and PCBs
Nickel Nitroaromatics and Cyclic Ketones
Selenium Polynuclear Aromatic Hydrocarbons
Silver Chlorinated Hydrocarbons
Organophosphorous Pesticides
Other parameters may be measured as part of the overall RCRA program. These
parameters include, but are not necessarily limited to: TOC, polar organics, viscosity,
chlorides, specific gravity, BTU, proximate and ultimate analysis.
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Section No. VII
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PROJECT ORGANIZATION AND RESPONSIBILITIES
The WMB is organized under the Branch Chief into three Sections. Out of these
three Sections, the compliance section and the permit section are responsible for
conducting monitoring activities. The functions of this Section are described as follows:
Provides technical assistance to Federal, State, and local agencies and industry.
Conducts compliance inspections and takes enforcement actions as appropriate.
Overviews state program monitoring activities.
Project organization and individuals responsible for quality assurance are shown in
Figure I. Responsibilities of these personnel are summarized in Table I
FIGURE I
PROJECT ORGANIZATION
Hazardous Waste
Division Director
WMB
Branch Chief
Chief, RCRA Compliance Section
Project Officer
Environmental Services
RQAMO and Peer Review
State Operations Offices
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Section No. VII
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Table 1, Personnel Responsible For Quality Assurance Activities
Personnel
Responsibilities
WMB Chief
RCRA Compliance Section
Chief
Project Officer
ESD Peer Reviewer(s)
RQAMO
Provides oversight of all program
activities; consult with section chief on
policy decisions and major QA problems.
Reviews final-project QA needs,
problems, and requests; approves
appropriate QA corrective actions as
needed. Sign-off responsibility for
Section on QAPPs.
Coordinates both internal and external
technical operations with appropriate
State or local agencies. Liaison with
RQAMO. Ensures that QAPP is
prepared and adhered to: by proper
handling of logs, sample receipts,
custody records and all other required
documentation; through careful
instrument calibration and
maintenance; that internal quality
control measures are implemented; that
corrective action is taken and RQAMO
is notified when problems occur; that
data, QA information, and reports are
produced in a timely manner.
Provides technical QA assistance to
ensure compliance with approved or
recommended sample collection
policies and procedures.
Reviews and has sign-off authority for
Region on all QAPPs; provides
teclmieal QA assistance and audits in
relation to EPA QA policies and
procedures.
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Section No. VIII
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Vffl. OBJECTIVES FOR MEASUREMENT DATA
The overall QA objective is to develop and implement procedures for field sampling,
chain of custody, laboratory analysis and reporting that will provide sound scientific data
and legally defensible results in a court of law. Specific procedures to be used for
sampling, chain of custody, calibration, laboratory analysis, reporting, internal quality
control, audits, preventative maintenance and corrective actions are described in other
sections of this QA Manual. The purpose of this section is to define QA goals for
detection limits, precision, accuracy and completeness where possible and presented in a
tabular format similar to table 2. Such a table should be prepared by the project officer-
in consultation with the QA coordinator, laboratory director and reviewed by the RQAMO
prior to initiating sampling efforts.
All measurements will be made so that results are consistent and representative of
the media and conditions measured. All data will be calculated and reported in units
consistent with other RCRA investigations to guarantee comparable data bases.
Establishment of these goals allows the project manager to judge the adequacy of the
results obtained and either use them or take corrective action if necessary.
Data quality objectives recommended by WMH for RCRA analyses are described
below:
Detection Limits - The detection limits most commonly used for the pur-pose of
RCRA analyses are presented in Table 4 in Section XII.
Accuracy - The QA accuracy objectives for quantitative analysis are expressed in
terms of recovery of surrogate compounds or recovery of spiked analytes. Recovery
of a surrogate compound added to a sample will be defined as follows:
Recovery, % = Grams of Surrogate round in Sample x 100%
Grams of Surrogate Added to Sain pie
The recovery of a spiked analyte is defined as follows:
Recovery, % = Total Analyte Found - Analyte Originally Present x 100%
Analyte Added
QA objectives for these recoveries are given in Table 2.
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Section No. VIII
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Precision - The objective for precision where duplicates or replicate analyses have
been performed are as follows:
• Analysis of Surrogate or Analyte Spikes: One of the QA objectives is that the
standard analysis of surrogate compounds or analyte spikes in duplicate samples
from a given sampling point be within the limits specified in Table 2.
• Analysis of Duplicate Samples or Replicate Analytes : One of the QA
objectives is that the results or quantitative analysis for duplicate or replicate
samples be within the limits specified in Table 2.
A more thorough discussion of, and the equations used to calculate precision are to be
found in Section 15.0.
Completeness - Completeness is defined as the degree to which the number of
activities initiated are actually finished. The degree of completeness is the total
number of samples for which acceptable analytical data are generated divided by the
total number of samples collected times 100%. As shown in Table 2, the QA data
objective for the completeness of WMB projects is 95%.
Comparability - To ensure a coherent data base, all results should be reported in the
same units of quantification. Measurement units most commonly used for the
purpose of RCRA analyses are presented in Table 4 in Section XII.
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Section No. VIII
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TABLE 2
EXAMPLE OF DATA QUALITY OBJECTIVES FOR RCRA MEASUREMENT DATA
Technique or
Parameter Matrix Precision Accuracy Completeness
Characteristics
Ignitability Solid, Liquid ,sludge ±20% 97-103% 95%
Corrosivity Liquids, sludges ±10% 90-110% 95%
KPToxicity Solids ±30% 70-130% 95%
Composition
GC or GC/MS Aqueous ±20% ±3 SD 95%
Volatile Solids
Organics and Biota ±50% ±3 SD 95%
Base neutrals
Acids
Pesticides
Atomic Absorption Solid, liquid, sludge ±30% 70-130% 95%
for
spikes
±2SD
for QC 95%
samples
Cyanide Solid, liquid, sludge ±20% 80-120% 95%
Sulfides Solid, liquid, sludge ±20% 80-120% 95%
pH Aqueous phase of 20%
total volume
TOX Drinking & Ooundwaters ±20% 80-120% 957c
'o
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Section No. VIII
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Following is a list of documents that provide information concerning statistical
procedures for measurement data:
Cochran, W.G. 1977. Sampling Techniques. 3rd edition
John Wiley & Sons, Inc. New York, NY. 428 pp.
Finney, D.J. 1964. Statistical methods in biological assay.
Hafner Publishing Co. New York, NY.
Green, R.H. 1979. Sampling design and statistical methods for enviornmental biologists.
John Wiley & Sons, N.Y. 257 pp.
U.S. Environmental Protection Agency, 1984.
Calculation of Precision, Bias, and Method Detection Limit for Chemical and Physical
Measurements.
Keith, L, W. Crummett, J. Deegan, Jr., R. Libby, J. Talor and G. Wenther. 1983.
Principles of environmental analysis. Analytical Chemistry, Vol. 55. pp. 2210-2218.
Sokal, R.R., and F.J. Rohlf. 1969. Biometry. W.H. Freeman and Co., San Francisco, CA.
776 pp.
Tetra Tech. 1985. Bioaccumulation monitoring guidance: Selection of target species and
analytical detection limits prepared for U.S. Environmental Protection Agency,
Washington D.C.
U.S. Environmental Protection Agency. 1979a. Handbook for analytical quality control in
water and waslewater laboratories. EPA-600/4-79-019. Environmental Monitoring and
Support Laboratory, Cincinnati, OH.
U.S. Environmental Protection Agency. 1982a. Handbook for sampling and sample
preservation of water and wastewater. EPA-600/4-82-029. Environmental Monitoring
and Support Laboratory, Cincinnati, Oil. 402 pp.
U.S. Environmental Protection Agency. 1983b. Environmental measurement method
performance data for establishing achievable data quality goals. Environmental
Monitoring Systems Laboratory Research, Triangle Park, NC.
Additional references for methods and associated measurement objectives are given
in Section 7 - Sampling Procedures, and Section 10 - Analytical Procedures.
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Section No. IX
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K. SAMPLING PROCEDURES
Ultimate accuracy of any data generation begins with a sampling procedure that is
well conceived and implemented. Prior to sample collection, a detailed QAPP (see
Appendix C for example of format) specifying sampling procedures and equipment, sample
container type and preparation, sample preservation methods and holding times and
shipping requirements will be prepared.
The sampling procedures to be used by the HWMB for RCRA investigation are based
on those described in the following references:
• "Test Methods for Evaluating Solid Waste Physical/Chemical Methods",
SW-846, 2nd Edition, U.S. Environmental Protection Agency, 1982.
• "Sampling at Hazardous Materials Incidents", U.S. Environmental Protection
Agency, Office of Emergency and Remedial Response, April 1984.
• "Field Sampling Workbook", Prepared by Region 10, U.S. environmental
Protection Agency, Nov. 1984.
Before sampling of any site is performed, the Project Officer will meet or talk with
the Compliance Section Chief or the RCRA QA Coordinator. The purpose of the meeting
will be to establish the sampling objectives, sampling methodology to be employed and the
analytical test which will be performed on the samples. Where possible, the QA
coordinator and the field sampling team will establish the sensitivity required for the
analytical tests. All field activities and sampling will be documented in a stitched, bound,
and numbered field logbook. Modifications to approved or recommended sample
collection procedures will be described on the sample alteration checklist (Appendix C, pg
4) of the QAPP. Overall responsibility to see that field staff is properly trained in
sampling procedures rests with the WMB Chief.
The type of sample container and preservation method used will vary according to
the sample type and the parameters being measured. The field sampler is responsible to
assure proper preservation methods are employed.
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Section No. IX
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Table3
Example Of Sample Container And Preservation Methods
Parameter
Size and Tvoe of Container
Preservative*
Ignit ability
Corrosivity
Reactivity
EP Toxicity
Metals, except
Mercury and
Hexavalent Cr
Mercury
Hexavalent Cr
Volatile
Organ ics
Semi-volatile
Organics
Pesticides
Cyanide
TOX
Sul fides
pH
500 ml glass
1 liter plastic
1 liter plastic
1 quart glass
1 liter plastic
1 liter plastic
1 liter plastic
Purgeable vials (2 or more)
1 gallon glass
1 gallon glass
I liter plastic
Purgeable vials
I liter plastic
1 liter plastic
Iced or refrigerated
Iced or refrigerated
Iced or refrigerated
Iced or refrigerated
5 ml HN03/liter
20 ml (2.5% K2Cr207
in 25% HNO3)/liter and iced
Iced or refrigerated
Iced or refrigerated
Iced or refrigerated
Iced or refrigerated
1 ml 50% NaOH/litcr and iced
Iced or refrigerated
2 ml (2N) Zn(C2H302
per liter
Iced or refrigerated
* Preservation used only if sample is aqueous. Non-aqueous samples are placed in a
glass bottle and iced. If the sample is strongly alkaline or acidic, a preservative
should not be used. Volume of sample includes Quality Control effort.
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Section No.: X—ALL QAPs
Revision No.: 2
Date: March 1986
Page: I of 15_
X. SAMPLE CUSTODY AND DOCUMENTATION
The possession of samples must he traceable (i.e. their whereabouts must be
determinable at all times evidenced by paper to prove it) from the time the samples are
collected until they are introduced as civil or criminal evidence in enforcement
proceedings, because of the potential evidentiary nature of sample collecting
investigations. In addition, all information pertinent to field activities must be recorded
in various forms, including logbooks, sample tags, and photographs. Such information,
since it is required and used to refresh the investigators memory years later at trial will
support the introduction into evidence of a particular sample, and potentially provide
important or corroborative evidence relevant to the matters at issue. Therefore, each
field worker must keep detailed records of inspections, investigations, photographs taken,
etc., and thoroughly review all notes before leaving the site. Document control is
implemented to ensure that all documents for a specific project are accounted for when
the project is completed. Accountable documents include items such as logbooks, field
data records, and photos. Each document should bear a serial number and should be listed,
with the number, in a project document inventory assembled at the project's completion.
Waterproof ink should be used in recording all data in documents bearing serial numbers.
Under Rule 803(6) of the Federal Rules of Evidence written records of regularly
conducted business activities may be introduced into evidence as an exception to the
"hearsay rule" without the substantive oral testimony of the person(s) who made the
record, (IF the author can establish the proper foundation for admissibility (date, time,
place, who was there, identify that a document was authored by him (by signature,
initials, or handwriting) and be able to state that that type of document is kept in the
ordinary course of business). Although it is preferable, it is not always possible for the
individuals who collected, kept and analyzed samples to testify in court. In addition, if
the opposing party does not intend to contest the integrity of the sample or testing
evidence, admission under Rule 803(6) can save a great deal of trial time. For these
reasons, it is important to standardize the procedures followed in collection and analysis
of evidentiary samples to qualify for the requirement of "regularly conducted activity".
Whether or not the team members anticipate that various documents will be introduced as
evidence, they should make certain that all documents are as accurate and objective as
possible. THE SUCCESS OR FAILURE OF A COURT PROCEEDING COULD DEPEND ON
IT.
A. FIELD LOGBOOK
All information pertinent of field act i\i1 ies should be entered in ;i bound book with
consecutively numbered pages. At a minimum, logbook entries must include:
WHEN (date, time)
• WHERE (county, state, site address, sample location)
• WHO (those present directly involved)
• WHAT (sample numbers, descriptions of observations and actions)
• HOW (equipment used,or procedures followed)
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Section No.: X—ALL QAPs
Revision No.: 2
Date: Maroh 1986
Page: 2 of 15
Additional entries, of a WHY nature may he included, particularly if the sampler
feels they could act as collateral aids in refreshing his memory at a later date.
HOWEVER, caution should he exercised that these are essentially ohjective in nature as
they too would be considered as evidence. Such entries could include:
• Name and address of field contacts (federal, state, or local representatives
present hut not directly involved in activity)
• Type of process producing the material
• Type of media sampled (drinking water, wastewater, sediment, etc.)
• References such as maps or photographs taken or acquired of the sampling site
• Any field measurements made such as pH, total organic vapors, or
explosiveness
Because sampling situations vary widely, notes should he as descriptive and inclusive as
possible. Those reading the entries should he able to reconstruct the sampling situation
from the recorded information. Language must be objective, factual, and free of personal
feelings or opinions or any other inappropriate terminology. If anyone other than the
person to whom the logbook was assigned makes an entry, they must date and sign it.
Errors should he corrected with a single line drawn through the error; the correct data
filled in, and the correction entry initialed and dated.
B. PHOTOGRAPHS
Photographs can be the most accurate demonstration of the field worker's
observation. They can be significant to the field team during future inspections, informal
meetings, and hearings. A photograph should be documented withe the entries listed as
MUST listed in part A, above, if it is to be valid representation of an existing situation. It
is a good idea to sign and date the final print or1 transparency, (o aid in positive
identification at a future date. Comments should be limited to an objective description.
Photographs should be taken with a camera-lens system with a perspective similar to that
afforded by the naked eye.
C. SAMPLE LABELS
Each sample should be labeled using waterproof ink and sealed immediately after it
is collected. Labels should be filled out before collection to minimize handling of the
sample container. Records should be kept of the assignment of serial sample tags to field
personnel if such forms arc used. Sample tags must never be discarded. Lost, voided, or-
dain aged tags should be immediately noted in the logbook of the person to whom they
were assigned.
Labels must be firmly affixed to the sample containers . 'fags attached l>.\ string
arc acceptable when gummed labels are not available or- applicable, 'flu: container- must
he dry enough for a gummed label to be securely attached. The label must include at the
minimium the assigned sample number-. If supporting information, i.e. Name of collector-,
date and time of collection, place; of collection are not included on this label, such
information MUST be recorded in the bound field logbook at the time of actually taking
the sample and directly keyed to the assigned sample number and cross referenced to the
appropriate Field Data Sheet and Chain of Custody Form, and Analysis Requested form.
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Section No.: X—ALL QAPs
Revision No.: 2
Date: March 1986
Page: 3 of 15
D. CHAIN-OF-CUSTODY PROCEDURES
As in any other activity that may be used to support litigation, the sample collector
must he able to provide documentation of the chain of possession and evidence of the
continued custody of any samples which are offered for evidence. Written procedures
must be available and followed whenever evidentiary samples are collected, transferred,
stored, analyzed, or destroyed. The primary objective of these procedures is to create an
accurate written record which can be used to trace the possession and handling of the
sample from the moment of its collection through its analysis and to its introduction as
evidence.
A sample is considered to be in someone's "custody" if:
• It is in one's actual possession, or
• It is in one's view, after being in one's physical possession, or
• It is in one physical possession and then locked up so that no one can tamper
with it, or
• It is kept in a secured area, restricted to authorized and accountable personnel
only.
During sampling collection and shipment, specific procedures should be followed to
maintain proper chain-of-custody and accurate field inventory sheets, logbooks, and other
supporting documentation. DO NOT LOSE THEM!
1. Sample Collection, Handling, and Identification
The number of persons involved in collecting and handling samples should be kept to
a safe minimum. Field records should be completed at the time the sample is collected
and should be signed or initialed, including the data and time, by the sample collector(s).
Field records (in addition to those listed in Part A. of this section) should contain the
following information:
• Unique sampling or log number
• Custody form numbers, if supplied
• Preservative used
• Name of collector(s)
• Copies of Field Data Sheets, Chain of Custody documentation, Analysis
Requested, Airbill or Waybill documents if shipped by common carrier
It should he confirmed by the sampler writing in his or her field log that each sample
is identified by the approved pressure-sensitive gummed label or standardized tag on (lie
container, and if the individual container is scaled.
The sample con! ainer should t hen be place*I in a I runsport at ion case, along \\ it h t he
shipping copies of chain-of-custody record form, pertinent field records, and analysis
request forms as needed. The transportation case should be sealed or locked. A locked or
scaled ice chest eliminates the need for close oversight of the individual samples.
However, on those occasions when the use of an ice chest is inconvenient, tin; collector
should seal the cap of the individual sample container in such a way that any tampering
would be easy to detect.
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Section No.: X—ALL QAPs
Revision No.: 2
Date: March 1986
Page: 4 of 15
When samples are composited over a period of time, unsealed samples can he
transferred from one crew to the next. The transferring crew should list the samples and
condition and a memher of the receiving crew should verify the condition abd sign the
list. The receiving crew either transfers the unfinished composite samples to another
crew or treats the finished composite sample as described above for samples.
It is desirable to photograph the sample location or any visible pollution to facilitate
identification later. At the time the photo is taken, the photographer should record time,
date, site location, and a brief description of the subject in the Field Log book. If
Polaroid is used, the photographer should sign and date on the back of the photo. Film,
developed negatives, transparencies, photographs and written records that may be used as
evidence should be handled in such a way that chain-of-custody c;ui be established.
2. Transfer of Custody and Shipment
When transferring the samples, the transferee must sign and record the date and
time in the chain-of-custody record (Either Fig. 2 or Fig. 6). Custody transfers in the
field should be documented and account for each sample, although samples may be
transferred as a group (as long as each individual sample in the group is identified). Kvery
person who takes custody must note if the individual samples or the sealed shipping
container is correctly sealed and in the same condition as noted by the previous custodian;
and must fill in the appropriate section of the chain-of-custody record. To minimixe
custody records, the number of custodians in the chain-of-possession should bo minimized
(if possible).
All packages sent to the laboratory should be accompanied by the chain-of-custody
record and other pertinent forms. A copy of these forms should be retained by the
originating person. Have the designated agent of the common carrier sign and date the
field copy of the chain of custody form. Mailed packages can be registered with reI urn
receipt requested. For packages sent by common carrier, receipts, bills of lading, airbills
or waybills or copies of these documents must be retained as part of the permanent
chain-of-custody documentation. If the originals of such documents must be forwarded to
finance for payment, be sure to keep a true copy (a true copy is one made or photocopied
by an individual who signs and dates the copy to identify it as an accurate reproduction of
the original: "True copy of original. Made by John Doe, February 30, 1980.") for the chain
of custody documentation. Samples to be shipped must be packed so as not to break and
the package should be sealed or locked so that any tampering can be readily detected.
The FPA shipper and receiving personnel should both note the condition of the container
seals (brok(M) or unbroken) each time possession is exchanged. The preferred procedure
includes use of a custody seal (Figure 3) wrapped across filament tape that is wrapped
around the package at least twice. The custody seal is then folded over and stuck to itself
so that the only access to the package is by cutting the filament tape or- breaking the seal
to unwrap the tape. The seal is t hen signed. As an altcrnat ive, tamper proof t ape max, be
used to seal across the filimeiit tape.
Upon receiving the sample container the laboratory will verify the integrity of the
custody seals by noting in the "miscellaneous" section of the Field Data Shoot/Chain of
Custody sheet "seals intact" or "seal broken", initialed and dated. If containers arrive
with broken seals, the Laboratory will immediately notify the Project Officer and the
KQAMO.
-------
Section No.: X—ALL QAPs
Revision No.: 2
Date: March 1986
Page: 5 of 15
E. LABORATORY NOTIFICATION AND REPORTING
It is important to notify the Regional Sample Management Control Center (RSMCC)
by phone and verify the shipping schedule before sampling, whenever possible. The caller1
should indicate that it is a high priority situation (if appropriate) and verify that the lab
will be able to receive the samples. Queries about the sample arrival, position in the job
stream etc., should be directed to the RSMCC.
In an emergency situation, when the EPA RSMCC or laboratory cannot be notified
prior to sampling, the sampler must keep accurate records of sampling procedures and
locations. The sampler may use a physical description of the sample location, provided
that it is descriptive enough to differentiate between locations. As soon as possible
following the emergency response, a completed QAP will be submitted to facilitate
tracking and response.
All prospective sampler's or Project Officers should contact the Sample Control
Center prior to any sampling to obtain copies of their required forms. A list of the forms
often required by laboratories include:
• Chain of Custody Record (Figure 2)
• Examples of Custody Seals (Figure 3)
• Analysis Required: X-91,Priority Pollutants - Organies (Figure 4)
• Analysis Required Sheet: X-92, Metals (Figure 5)
• Field Sample Data Sheet, with Chain of Custody (Figure (>)
• Analysis Required: X-93, Physical and General Inorganics and Ion
Chromatograph (Figiu-e 7)
• Analysis Required: X-94, Oxygen Demand, Solids & Nutrients (Figure 8)
• Contract Lab Organic Traffic Report (Figure 9)
• Contract Lab Inorganics Traffic Report (Figure 10)
• Contract Lab High Hazard Traffic Report (Figure II)
Samplers should find out in advance which of these forms the laboratory requires.
F. CORRECTIONS TO DOCUMENTATION
If an error is made; on any accountable document assignee! to one individual, that
individual may make corrections simply by drawing a line through the error and enter-ing
t he correct information. The erroneous informal ion should not be obliterated. Any
subsequent error discovered on an accountable document should be corrected by 1 he
person who made the entry. All corrections must be initialed and dated.
-------
Section No.: X—ALL QAPs
Revision No.: 2
Date: March 1986
Page: 6 of 15
oEPA
United States
Environmental Protection
Agency
Region 10
1200 Sixth Avenue
Seattle WA 96101
CHAIN OF CUSTODY RECORD
PROJECT
LAB #
STATION
DATE
TIME
RELINQUISHED BY: ts
DATE
SAMPLERS: /Signature!
SAMPLE TYPE
WATER
SEDIMENT
TISSUE
X
o
r-
O
— *
I
m
3
NUMBER
OF
CONTAINERS
REMARKS
RECEIVED BY: ts,gn.wr,, DATE/TIME
RECEIVED BY: «*»«». DATE/TIME
RECEIVED BY: isynawm DATE/TIME
REC'V'D BY MOBILE LAB FOR FIELD DATE/TIME
ANAL.: ISipnelurei
'TIME
RECEIVED FOR LAB BY: isv-ww DATE/TIME
METHOD OF SHIPMENT:
Distribution. Original —Accompany Shipment
One Copy-Survey Coordinator Field Files
FIC.URE 2
Chain Of Custody Record
-------
Section No.: X—ALL CMPs
Revision No.: 2
Date: March 1986
Page: 7 of 15
^">"-v UNITED STATES
v *± V ENVIRONMENTAL PROTECTION AGENCY
* ,^^, 5 OFFICIAL SAMPLE SEAL
\ss;
*'-l ..<*'<•
SAMPLE NO.
DATE
SIGNATURE
PRINT NAME AND TITLE (Inspector. Analyst cr T)xhnician)
ISEAL BROKEN BY I
in
0
IA
P*
IS
2
-------
Section No.: X—ALL QAPs
Revision No.: 2
Hate: March 1986
Page: 8 of 15
EPA Region 10 Laboratory
Analyses Required
PRIORITY POLLUTANTS - ORGANICS
Project Name:
Project Code:.
Account Code:.
Matrix Codas larOe oni onlyl
10 Wner-Tolll
11 Water-Dissolved
40 Sediment/ Soil
45 Semi-Solid/Sludge
46 Sediment for EP Toxicity
70 Tissue
80 Oil/Solvent
00 Other
Sample Numbers
/Analy/Comp
Init/Daie
GC/MS Orgenic Scant
68 Base/Neutrals/Acids BIN/A
62 Base/Neutrals Only B/N
51 Volatile Organics VOA
65 Acids Only Acid
Specific IGC/MS) Organics List flrtow
GC Organic Scans
71 Pesticide/PCB's Pest/PCB
74 PCB's Only PCB
64 Purgeable Halocarbons Purg
S3 Trihalomethanes Tribal
73 HerbioOes Herb
70 Chlorinated Hydrocarbons
70 OrganophosDhate Pesticides
Specific (GO Organics LSI Booty
Specific Organics at
Other Miscellaneous
67 PolyAromHydro (HPLC) PAH
40 OH Identification Oil-Id
40 Pnenolics IAAP) Phenol
40 Oil 6 Grease Oil & Greas
40 Flashpoint Flashpt
Save samples after analysis? NONE, SOME or ALL. m sot/-, a
Soecial detection limits and comments
EPA X-t1 Ub Copy
FIGURE 4
Analysis Required: X-91, Priority Pollutants - Organics
-------
Section No.: X--ALL QAPs
Revision No.: 2
Date: March 1986
Page: 9 of 15
M<
We
W
EPA Region 10 Laboratory Analyses Required
Pmjort Name: P
Matrix Codes IcmM one onlyl
10 Water-Total
11 Water-Dissolved
40 Sediment/Soil
45 Semi-Solid/Sludoe
46 Sediment tor EP Touchy
70 Tissue
00 Oil/Solvent
00 Other
Uls IcirOf WC II
>rkgroup 30 - Standard Method
>rkgroup 34 - EP Toxicrty Method
Aluminum Al
Antimony Sb
Arsenic Ac
Barium Ba
Beryllium Be
Cadmium Cd
Calcium Ca
Chromium Cr
Chromium Hexavaient Cr •*• 6
Cooalt Co
Copper Cu
Iron Fe
Lead Pb
Magnesium Mg
Manganese Mn
Mercury Hg
Molybdenum Mo
Nickel Mi
Potassium K
Selenium Se
Silver Ag
Silicon Si
Sodium Na
Thallium T1
Vanadium V
Zinc Zn
//.
reject Co
de- Ar
:count Code:
METALS
/ Sample Numbers /
'',
I
/
/
^
'//
'/,
7////////
i
i
i
i
1
1
i i
\
; 1 i
!
i
: i i
; i : i ; i : •
1 \ . , 1 i
I I'll i i '
1 ' ' i ' : • . ,
Save samples after analysis? NONE,
Soecial limns, methods and comments
Analy/Comp
Init/Date
SOME Or ACL. (If SOM£. circit same* numoers .
Protect O'licfr Sifrwiurr U*fe
EPA X-S2 Ub Copy
Analysis KoquirtKi: X-92, Motals
-------
FIELD SAMPLE DATA AND CHAIN OF CUSTODY SHEET
p
s
c.
•J-.
s.
EPA B^oo 10
1200 Stnh AWHM
SMUta WA 96101
Prnjact Code: Account:
Name/ Location:
Prniart Officer:
D Enforcement/Custody
D Possible Taxin/Hmardnus Nntas:
n On'" Tnnf jHflntifll
n Data for Slnrn*
Samplers'
HecorHnr-
UJ
O
CC UJ
3Q
OO
C/1U
MATRIX
|
I
1
§
1
6
»C
ft
!
3
0
.£
?
r
Ml
3E
c?
2
I
4!
se
-
vlt
RV
rtS
.
LAB
NUMBER
Yr
-
Wk
Seq
STATION
NUMBER
DATE
Yr
Mo
Dy
Time
-
COMPOSITE ONLY
ENDING DATE
Mo
:
Dy
-
Tims
-
-
1
Fraq
-
-
STATION
DESCRIPTION
LAB
NUMBER
Yr
Wk
Seq
DEPTH
c
D
-
s
-
-
COL
MTD
CD
-
QA
CODE
-
TEMP
DEC
C
-
-
-
-
pH
CNDCTVTY
umho/cm
-
MISCELLANEOUS
CHAIN OF CUSTODY RECORD
RELINQUISHED BY:>s««u~<
RELINQUISHED >Y:Uv>i«il
RELINQUISHED BY:isit*wi
RELINQUISHED BY:tt*~i»'.;
RECEIVED BY:u«/i.ur./ DATE
RECEIVED BYu&twml DATE
RECEIVED BY:>5vo.nn/ DATE
REC VO BY MOBILE LAB DATE
FOR FIELD ANAL.: is*~n.l
RECEIVED FOR LAB BY:»*n.».>DATE
TIME
rnTST
TIME
TIME
/TIME
L»bo.lliVY Copy Pro)*cl Otlicv COPY f "•« w Ott*-» Copy
£°*
H* CS ft)
00 S- <
a a £
Si. O
O 3
P "
O
CC
CO
to
X
I
I
t-
r
-------
Section No.: X—ALL QAPs
Revision No.: 2
Date: March lf)86
Page: 11 of 15
EPA Region 10 Laboratory Analyses Required
f
n
i
i
«
4
4
7
a
0
PHYSIO
rnjort Name: Pi
Matrix Codes IcirOe one omyl
3 Water-Total
1 Water-Dissolved i
3 Sediment/Soil /
5 Semi-Solid/Sludge /
> Sediment tor EP Toxicity /
0 Tissue / /
0 Oil/Solvent / /
0 Other / /
Physical ft General
Inorganics WG 1101
Turbidity TURB
pH (Lab) pH
Conductivity COND
Total Alkalinity T ALK
Total Hardness T HARD
Bicarbonate HC03
Calcium Ca
Carbonate C03
Chloride CI
Fluoride F
Sulfate SO4-TOT
Surfide S
Cyanide CN
Acidity Acidity
Hardness CaC03
Color Color
Ion Chromaiograph we lea
Calcium Ca
Chloride O
Cyanide CN
Fluoride F
Magnesium Mg
Potassium K
Sodium Na
Surtate S04
Nitrate N03
Nrtme N02
Ortho Phosphorous O-Phos.
!
\L£r
oject Coi
GENERAL
IONC
ie:
INORG
HROM
Account Co
ANICS AND
ATOGRAPH
de:
/ Sample Numbers /
w/////////////
1 1
' 1
: '• 1
i ; 1
j
i !
i
1
i i r
1 1 • i
i
i ' '
i i ' ' i : i
; • |
1 i i
1 i '
I' ! ' • , i
: ! ' ' i
Save samples after analysis? NONE. S
Special detection limits and comments
Analy/Comp
/ Inn/Date
DME or ALL.
-------
Section No.: X—ALL QAPs
Revision No.: 2
Date: March 1986
Page: 12 of 15
1
t
4
A
1
(
EPA Region 10 Laboratory Analyses Required
OXYGEN L
'rojeet Name:
Matrix Codes ic,roe one oniyi
0 Waler-Totel
1 Water-Dissolved
10 Sediment/ Soil
5 Semi-Solid/Sludge
IE Sediment tor EP Touchy
ro Tissue
B Oil /Solvent
XJOther
Oxygen Demand ft Carbon WG tJBl
Bio. Oxygen Demand BOD/5 day
Bio. Oxygen Demand BOD/20 day
Bio. Oxygen Demand BOD/60 day
Bio. Oxygen Demand
(5-d»y) Carbonaceous BOD/5 day-C
Chem. Oxygen Demand COD
Total Organic Carbon TOC
Solids we 1151
Total Dissolved TDS
Total Sus. Solids SS
Total Solids TS
Volatile TVS
Volatile Suspended TVSS
Senieable Solids SetSlds
% Total Solids % Tot
% Volatile Solids % V Slds
Grain Size Gm S\z
Nutrients we 12OI
Ammonia NH3
•Nitrate N03
•Nrmte N02
Nitrate + Nitrite N03 + N02
Kieldahl Kjel-N
Total Phosphorous T-Phos
Dissolved Phosphorous D*Phos
•Ortho Phosphorous O-Phos
Dissolved Ortn. Phos. D-0 Phos
/
i
)EMAr
Project Code
JD, SOLIDS AND NUTRIENTS
• Account Code:
/ Sample Numbers /
//////////////// /*nal»r/ComP
/////////// ////// 'nit/Date
; i
1
i
!
i
i
I
!
1
1 1
1 1
i , I i
. i ' I i
I
1 1 i
i
i
i !
1
1 i;i
i i i 1 1 1
,
!
1 ' i '
: i
i
i
i : • • < ' i 1 i 'i
i : . i .
Save samples after analysis? NONE, SOME or ALL. >/r snu[ nrc/r- wnw nu/w.-.- >
Soecial derernnn limiis and comments •
ProtKI Ollmt Signature Ofie
=PA X-M Lab Couy
KKUJRKS
Analysis Required: X-94, Oxygen Demand, Solids and Nutrients
-------
Section No.: X—ALL QAPs
Revision No.: 2
Date: March 1986
Page: 13 of 15
U5.ENVIRONMENTRLPROTECnON AGENCY HWI Sample Management Office
P-O.Box818.Aiexandna.Vut5iiia22313-703 557.2490-FTS 557-2490 •--..-•
ORGANICS TRAFFIC REPORT
Sample Number
JB 102
T) Case Number
Sample Site Name/Code:
SAMPLE CONCENTRATION
(Check One)
Low Concentration
Medium Concentration
SAMPLE MATRIX
(Check One)
Water
Soil/Sediment
0 Ship To:
Attn:
Transfer
Ship To:
© Regional Office: _
Sampling Personnel:
(Name)
(Phone)
Sampling Date:
© For each sample collected specify numbei
of containers used and mark volume level
on each bottle.
Number of
Containers
Water
(Extractable)
(Begrn)
(End)
Water
(VOA)
® Shipping Information
Name of Carrier
Date Shipped:
Soil/Sediment
(Extractable)
Soil/Sediment
(VOA)
Other
Airbill Number:
® Sample Description
Surface Water
Ground Water
Leachate
Mixed Media
Solids
Other (specify).
Approximal
Total Volum
JB
1 JB
JB
JB
JB
JB
JB
JB
©SampleI JB
JB
102
102
102
102
102
102
102
102
Ib2
Iu2
- Water
(Em-actable)
-Water
(Extractable)
- Water
(Extractable)
- Water
(Extractable)
• Water
(VOA)
- Water
(VOA)
- Soil/Sediment
(Extractable)
-Soil/Sediment
(Extractable)
• Soil/Sediment
(VOA)
- Soil 'Sediment
I VOA I
(To) Special Handling Instructions:
(e.g., safety precautions, hazardous nature)
SMOCOPY
FICURI: y
Contract Laboratory Organic Traffic Report
-------
Section No.: X—ALL QAPs
Revision No.: 2
Date: March 1986
Page: 14 ofIs
.sa
U.S.ENVmONMENTALPROTECnON AGENCY HWI Sample Management Officef
P.O.Box818,Alexandria,VA22313-703/557-2490• FTS/557-2490^:'§vfx"; ;r£T^;l^^t~4hfr'
INORGANICS TRAFFIC REPORTER
Sample Number
MJA700
(7) Case Number:.
Sample Site Name/Code:
Sampling Office: _
Sampling Personnel:
(Name)
(Phone)
Sampling Date:
(Begin)
(End)
® Sample Description:
(Check One)
Surface Water
Ground Water
Leachnte
Mixed Media
__ Solids
Other
(specify)
MATC1IES ORGANIC SAMPLE NO.
© SAMPLE CONCENTRATION
(Check One)
Low Concentration
Medium Concentration
© SAMPLE MATRIX
(Check One)
Water
Soil/Sediment
(?) Shipping Information:
Name Of Carrier:
Date Shipped:
Airbill Number:
Mark Volume Level
On Sample Bottle
Check Analysis required
Task 1 & 2
- Task 3 Ammonia
Sulfide
Cyanide
SMOCOPY
Ship To:
Attn:
Transfer
Ship To:
|MJ A 700 -Ta*kl&2
J A 700 -Ta*kl&2
|MJ A 700 Ta.«k3
MJ A 700 -TaA3
MJ A 7 0 0 Task 3
MJ A 700 Task3
MJ A 700 -TaskS
l-KJURI- 10
Contract Laboratory Inorganics Traffic Report
-------
Section No.: X—ALL QAPs
Revision No.: 2
Date: March 1986
Page: 15 of 15
US. ENVIRONMENTaLH^aiBCTION AGENCY CLP Sample Management Ofine
PO. Box aiB-Afaomdna, Vigaa 22313 Phone 7D3/5572-»90-FT5/557-a«0 •. - . - • r
FIELD SAMPLE RECOPUD
-' Case Number:
Sample Site Name/Code:
i) Sampling Office:
Sampling Personnel:
(name)
(phone)
Sampling Date:
(begin) tend)
8} Shipping Information:
(name of earner)
(date shipped;
(airoiL TTjrrjDer)
(D Field Sample Description:
_ Drum
__ Aq-aeous Liquid
._. Siuage
Sohd
Q!
Othpr
(L1 Known or Suspected Hazards:
'Jj Preparations Requested:
(check beiow)
Sample Volume:
__ Volatile Qrganics
. Base/Neuiral, Add,
TCDD
_ Pestades, PCS
Inorganics
_ Total Metals
Total Mercury
._ Strong Acid Anions
^ Ship To:
AttTv
v§) Sample Location:
1 5152
' 5152
T 5152
J 5152 .;
1 C 4 r O
J 0 1 D £
Special Handling Instructions:
SMOCopy
I'KilJRl' II
High Iliixard TntlTic Report
-------
Section No. XI
Revision No. 0
Date
Page 1 of
XL CALIBRATION PROCEDURES, FREQUENCY; PREVENTAM MAITENANCE
The calibration procedures and frequencies for laboratory analytical methods will be
those specified in SW-846. If field measurements are to be taken, all equipment and the
appropriate check and calibration procedures should be described by reference in the
QAPP.
Maintenance of equipment is an important part of every laboratory and field
operation. In the Regional Laboratory, contract laboratory, or field operations, the
responsibility of routine operating care lies with the analysts using the instruments.
Every manufacturer furnishes instrument maintenance manuals for their equipment.
These are kept on file in each laboratory for frequent reference; adjustments or repairs
which cannot be performed to satisfy these manuals are contracted to the manufacturer's
service department or representative.
Preventative maintenance procedures are discussed in detail in the Regional
Laboratory QA Manual.
Preventive maintenance and check procedures for field instrumentation will be
described separately for each instrument identified for use in the QAPP
-------
Section No. XII
Revision No. 0
Date
Page 1 of
ANALYTICAL PROCEDURES
Methods and references for most analyses are summarized in table 4.
Analysis of chemical and biological samples collected during field investigations will be
performed by the Regional laboratory or contract laboratory program with established
protocols and QA procedures described in SW-846 or contract requirements. When
approved or recommended EPA procedures are not available, a written description of the
procedure will be included as a reference to an EPA recommended method and what
modification have been made. Modifications to approved or recommended methods for
analytical methods will be described on the sample alteration checklist (in Appendix C,
page 4) of the QAPP.
-------
Section No. XII
Revision No. 0
Date
Page 2 of 3
Table 4
Methods and Minimum Detection Limits for RCRA Analysis
Parameter
SW-846 Method
Detection Limit
ug/L
Igiiitability 1010
Corrosivity 9040
Reactivity Sect.6
EPToxicity 1310
Antimony 7040,7041
Arsenic 7060
Barium 7080,7081
Cadmium 7130,7131
Chromium 7190,7191
Chromium, Hexavalent 7196,7197
Lead 7420,7421
Mercury 7470
Nickel 7520,7521
Selenium 7740
Silver 7760
Halogenated Volatile Organics 8010
Nonhalogenated Volatile Organics 8015
Aromatic Volatile Organics 8020
Acrolein, Acrylonitrile, Acetonitrile 8030
Phenols 8040
Pthalate Esters 8060
Organochlorine Pesticides and PCBs 8080
Nitroarornatics and Cyclic Ketones 8090
Polynuclear Aromatic Hydrocarbons 8100
Chlorinated Hydrocarbons 8120
Organophosphorus Pesticides 8140
Chlorinated Herbicides 8150
Volatile Organics (GC/MS) 8240
Semi-volatile Organics (GC/MS) 8270
Polynuclear Aroinatic Hydrocarbons (HPLC) 8310
Total and Amenable Cyanide 9010
Total Organic Halides (TOX) 9020
Su If ides 9030
pH 9040
N/A
N/A
N/A
N/A
200., 3.0
1.0
100., 2.0
5.0, 1.0
50., 1.0
verification
100., 1.0
0.2
40., 1.0
2.0
10.0
0.03-0.5*
1.0 ug/G sample
1.0 ug/G sample
1.0 ug/G sample
0.1-16.0*
0.29-3.0*
0.004-0.176*
0.06-5.0*
1.0 ug/G sample
0.03-1.19*
0.1-5.0*
0.1-200.0*
1.6-7.2
0.9-45.0*
0.4-2.3*
Not Defined
* Dependent on individual compound within group.
ug/L microgram per Liter
ug/G microgram per gram
-------
Section No. XII
Revision No. 0
Date
Page 3 of 3
Table 4 (Cont'd)
Parameter
Sample Preparation - Metals
Acid Digestion Procedure for Flame Atomic
Absorption Spectroscopy
Acid Digestion Procedure for Furnace Atomic
Absorption Spectroscopy
Acid Digestion of Oils, Greases, or Waxes
Dissolution Procedure for Oils, Greases or Waxes
Acid Digestions of Sludges
Alkaline Digestion
Sample Preparation - Organics
Separatory Funnel Liquid - Liquid Extraction
Continuous Liquid - Liquid Extraction
Acid-Base Cleanup Extraction
Soxhlet Extraction
Sonieation Extraction
Sample Introduction - Organics
Purge and Trap
SW-846 Method Number
3010
3020
3030
3040
3050
3060
3510
3520
3530
3540
3550
5030
-------
Section No. XIII
Revision No. 0_
Date
Page 1 of
DATA REDUCTION, VALIDATION AND REPORTING
Each QAPP will identify individuals responsible for handling data, and describe the
type of information to be transmitted with the data at each step. In general, laboratories
will provide verified data sets to the Project Officer and/or designated QA Coordinator
with adequate documentation to allow independent data validation. The Project Officer
and/or QA Coordinator is responsible for conducting checks for internal consistency,
transmittal errors, laboratory protocols, and finally, a check for complete adherence to
the quality control elements specified in Sections 6, 9, 10, and 12 of this manual.
Data storage needs unique to the WMB operations will be specified after
consultation with ESD data management staff. Such needs might include the way in which
data are referenced to original documents, particular data qualifiers to be used, the level
of detail with which sampling and analysis methods are to be described, and the inclusion
of certain types of descriptive information or additional data. Procedures and criteria for
evaluating both historical data and new data for completeness and comparability for
database inclusion should be developed by the WMB QA Coordinator in conjunction with
the ESD data management staff. Any other procedures or criteria used by the HWMB or
their contractors for assessing data validity must be described in the QAPP. All data
submitted by contractors must be in a form consistent with other WMB investigations and
compatible with the Regional Data Management System.
The data analysis scheme planned for collected data, including units, and statistical
tests to be used will be specified in the QAPP. While such specification may be by
citation from this guidance, the Project Officer should encourage a well thought out
project plan and should clearly identify additional data needs to ensure comparability with
study site reference data or historical comparisons
Each project officer is responsible for the accuracy of the reduction of data to
reports or final file inclusion. If precision or accuracy are outside of established
acceptance limits, data analyzed with that group of QA data must either be re-analyzed
or considered for corrective action. Where appropriate and defensible adjustments cannot
be made, the data should not be used. The Project Officer is also responsible for further
use or release of the data or derived project reports.
Standardized forms are to be used for data collection, analysis requests, reduction
and reporting. While data are entered into the computer system, the forms package will
be submitted to the WMB following QA acceptance.
On at least a yearly basis, WMB will cooperate with the SMO/RSCC, ESD in a
review and audit of the computer system records of analysis, etc. maintained on the
sample tracking and laboratory reporting systems.
-------
Section No.
Revision No.
Date
Page
XIV
0
1
of
XIV. INTERNAL QUALITY CONTROL CHECKS
Each measurement system shall have predetermined limits to identify when
corrective action is required, hefore data becomes unacceptable. The QAPP will specify
(from Table 4, Section XII) the analytical procedures to be used to identify that point.
The QAPP will address controls for accurate location of sampling stations, the
rationale used in selecting the number and location of those stations, for sample
collection, and for sample handling, and the type and frequency of QA/QC samples as set
forth in Table 5:
Table 5: Level Of Effort In QA Samplinj
Data Characteristic
Frequency*
Evaluated
Sample Type
Recommended
Field/Transport
Contamination
Field/Transfer
Contamination
Sampling Equipment
Laboratory
Contamination
Accuracy (Field
variability
Accuracy
Precision (Field
Variability)
Precision (Lab
Variability)
Container
Contamination
Field Blank
Field Blank
Field Blank
Lab (reagent)
Blank
Field Spiked
Standard
Addition (Spike)
and performance
evaluation samples
or standard reference
materials: One per
20 samples
Field
replicates
Laboratory
One per batch run
Empty
Container
One per 20 samples
One per 20 samples
As appropriate Final Rinse
One per batch nui
One per 20 samples
One per 10 Samples
One per 20 samples or
One per sample event
One per 10 samples or
One per sample event
One per container lot
Where two alternatives are cited, the recommended alternative is that resulting in
more frequent analysis. Where less than 20 samples are taken at a site, Transport
and/or Transfer blanks shall be taken to provide QA even to the minimum sampling
efforts.
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Section No.
Revision No.
Date
Page
XIV
0
I
of
XIV. INTERNAL QUALITY CONTROL CHECKS
Each measurement system shall have predetermined limits to identify when
corrective action is required, before data becomes unacceptable. The QAPP will specify
(from Table 4, Section XII) the analytical procedures to be used to identify that point.
The QAPP will address controls for accurate location of sampling stations, the
rationale used in selecting the number and location of those stations, for sample
collection, and for sample handling, and the type and frequency of QA/QC samples as set
forth in Table 5:
Table 5: Level Of Effort In QA Sampling
Data Characteristic
Frequency
Evaluated
Sample Type
Recommended
Field/Transport
Contamination
Field/Transfer
Contamination
Sampling Equipment
Laboratory
Contamination
Accuracy (Field
variability
Accuracy
Precision (Field
Variability)
Precision (Lab
Variability)
Container
Contamination
Field Blank
Field Blank
Field Blank
Lab (reagent)
Blank
Field Spiked
Standard
Addition (Spike)
and performance
evaluation samples
or standard reference
materials: One per
20 samples
Field
replicates
Laboratory
One per batch run
Empty
Container
One per 20 samples
One per 20 samples
As appropriate Final Rinse
One per batch run
One per 20 samples
One per 10 Samples
One per 20 samples or
One per sample event
One per 10 samples or
One per sample event
One per container lot
Where two alternatives are cited, the recommended alternative is that resulting in
more frequent analysis. Where less than 20 samples are taken at a site. Transport
and/or Transfer blanks shall be taken to provide QA even to the minim m sampling
efforts.
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Section No. XV
Revision No. 0
Date
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XV. PERFORMANCE AND SYSTEM AUDITS
Each QAPP will describe the internal and external performance and system audits
that will he required to monitor the capability and performance of the measurement
system(s).
Performance and system audits for WMB sampling and analysis operations will
consist of on-site reviews of field and laboratory quality assurance systems and equipment
for sampling, calibration, and measurement. This includes review of items such as
documentation of quality control data, completeness of field forms, field data storage and
filing procedures, and sample custody sheets. Environmental monitoring equipment will
be routinely maintained and calibrated during field use (see Preventive Maintenance).
Region 10 Laboratory and contract laboratories are required to take part in
performance evaluation studies conducted by the Environmental Monitoring and Support
Laboratory (EMSL) in Cincinnati, OH. and Las Vegas NV.. Results of these audits are
available from the RQAMO. For internal quality control applications, analytical
standards used in preparing performance evaluation samples and guidance for their use
can be obtained from:
Environmental Monitoring Systems Laboratory. U.S. Environmental
Protection Agency. Las Vegas, NV 89114
Environmental Monitoring Systems Laboratory. U.S. Environmental
Protection Agency. Cincinnati, OH 45268
The RQAMO in conjunction with the WMR QAC will develop and conduct system
audits based on this manual and also conduct optional site technical audits of operations
detailed in the QAPPs.
The WMB QAC ensures that each aspect of a project detailed in a QAPP will have
performed adequate internal audits of performance and systems before submitting quality
assurance reports to the management.
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Section No. XVI
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Date
Page 1 of
XVI. SPECIFIC ROUTIE PROCEDURES USED TO ASSESS DATA
PRECISION, ACCURACY, AND COMPLETENESS
The assessment of data precision, accuracy, completeness, and blanks will he made
by the HWMB project officer or QAC.
Assessment of Precision;
The mean, C, of a series of replicate measurements if concentration, C[, is
calculated as:
i = 1
where n = number of replicate measurements; C, Cj are both on mg/L or mg/Kg
The estimate of precision of duplicate measurements is expressed as the relative
percent difference (RPD):
RPD = Cg-Cj x 100
C
The RPD calculated will be compared with the respective goals identified in the
QAPP.
The estimate of precision of a series of replicate measurements (primarily used in
GC/MS analysis) is expressed as the relative standard deviation (RSD) where:
'n _
RSD = ±/I](C1-O)2
i = 1
n-l
Assessment of Accuracy:
Accuracy is monitored by analyzing standards, samples that have been spiked with
standard solutions, and control sain pies. Approximately 10% of all samples are
analyzed as spiked samples. The accuracy of new analytical methods is verified by
analyzing replicate spiked samples intermixed with routine samples.
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Section No. XVII
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Page 1 of
XVI CORRECTIVE ACTION
Corrective actions can fall into two categories:
1. Handling of sampling analysis, data processing, or equipment failures.
2. Handling of non-confonnance or non-compliance with the QA
requirements that have been set forth (objectives for measurement data).
Each QAPP will address the corrective measures to be taken for the method or
equipment failure type of problem. It will include predetermined limits of sample and
data acceptability, identification of the corrective action, and the organizational level
responsible for approval of action. Routine procedures for correcting and limiting data
processing errors will cover data coding, data entry, and data reporting. A formal
corrective actions program is difficult to define in advance for the non-conformance or
non-compliance type of problem. Each QAPP will list who is responsible for taking
actions, when actions are to be taken, and who ensures that actions taken produce desired
results. A special form is included with the example QAPP to facilitate such
documentation.
Corrective actions will be taken by the project officer when data are found to be
outside the predetermined limits of acceptability. The acceptable data range will be
listed on the corrective action form, which also provides a checklist for procedures to be
followed.
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Section No. XVIII
Revision No. 0
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XVE QUALITY ASSURANCE REPORTS TO MANAGEMENT
Reports to the WMB Branch Chief and the Project Officer will be made periodically
by the QA Coordinator. QAPPs will identify the mechanism of and the points to which
the reports will be made. QA reporting should be tied to the completion of various
elements of the QAPP rather than to general time periods. The reports will contain
information regarding data accuracy, precision, completeness, result of system mid
performance audits along with any reports of corrective action, sample alteration, or
other significant QA problems. Through this mechanism, effective solutions to project
problems may be developed and applied.
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Section No. XIX
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Page 1 of
XH. SAFETY
RCRA inspectors must occasionally deal with the risk of incurring illness or injury
while conducting investigations. They cannot anticipate every hazard, so they must take
precautions to prevent illness or injury to themselves, other workers, and the public.
Since RCRA inspectors cannot eliminate risk, they must reduce it to the lowest
feasible level. No set of rules can be uniformly applied to every situation. The Project
Officer must judiciously apply the guidelines of the EPA Standard Operating Safety
Guides (SOSG) at each site visited. The Project Officer must access those variables
peculiar to each investigation in order to establish appropriate safeguards. The EPA
Region 10 Safety and Health Officer (RSHO) is available at 442-0370 for consultation on
appropriate levels of protection, equipment, etc. to use for each investigation.
Generally, all RCRA site inspections requiring the collection of samples or potential
exposure to toxic materials will require a site safety plan. The Project Officer is
responsible for preparing the site safety plan. If the investigation is quite complex, the
RSHO will prepare or assist with the preparation of the plan. The site safety plan in
non-emergency situations must be written, posted, distributed and signed by all project
team members, and discussed with them prior to visiting the site. Emergency situations
may require verbal safety instruction and use of standard operating procedures until
specific protocols can be written. The SOSG will be used as standard operating procedure
in emergency situations.
Annex 9 and 10 of the SOSG are two examples of site safety plans. Examples of job
functions requiring to use of levels C and B are described on pages A9-2 and A9-3 of the
SOSG.
All RCRA inspectors must complete training as described in the Regional Policy on
Health, Safety and Proficiency Training before being allowed to participate in a RCRA
inspection or investigation.
Special safety considerations may be addressed as part of the QAPP. I3ecause a
formal safety plan is already required as separate documentation on any field activity,
such considerations would only address the possible effect of plan limits on achieving data
quality objectives.
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APPENDIX A
GLOSSARY OF TERMS
AUDIT
A systematic check to determine the quality of operation of some function or activity.
Audits may be of two basic types: 1) performance audits on which quantitative data are
independently obtained for comparison with routinely obtained data in a measurement
system, or 2) system audits of a qualitative nature that consist of an on-site review of a
laboratory's quality assurance system and physical facilities for sampling, calibrations,
and measurement.
CHAIN-OF-CUSTODY
Documentation that describes the physical control of a sample, measurement or document.
DATA QUALITY
The totality of features and characteristics of data that bears on its ability to satisfy a
given purpose. The characteristics of major importance are accuracy, precision,
completeness, representativeness, and comparability. These characteristics are defined
as follows:
- Accuracy - the degree of agreement of a measurement (or an average of
measurements of the same thing), X, with accepted reference or true value, T,
usually expressed as the difference between the two values, X-T, or the
difference as a percentage of the reference or true value, 100 (X-T)/T, and
sometimes expressed as a ratio, X/T. Accuracy is a measures of the bias in
the system.
Precision - a measure of mutual agreement among individual measurements of
the same property, usually under prescribed similar conditions. Precision is
best expressed in terms of the standard deviation. Various measures of
precision exist depending upon the "prescribed similar conditions."
Defensibility - ability to document the origin, chain of custody, matrix of
scientifically acceptable operations performed, reduction, and transcription of
data, so that their limitations, representativeness, and applicability are known.
- Completeness - a measure of the amount of valid data obtained from a
measurement system compared to the amount that was expected to be
obtained under correct normal conditions.
Representativeness - expresses the degree to which data accurately and
precisely represent a characteristic of a population, parameter variations at a
sampling point, a process condition, or an environmental condition.
Comparability - expresses the confidence with which one data set can be
compared to another.
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DATA VALIDATION
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, verification, certification, and review.
ENVIRONMENTALLY RELATED MEASUREMENTS
Terms used to describe essentially all field and laboratory investigations that generate
data involving I) the measurement of chemical, physical, or biological variables in the
environment, 1) the determination of the presence or absence of contaminants in waste
streams, 3) assessment of health and ecological effect studies, 4) conduct of clinical and
epidemiological investigations, 5) performance of engineering and process evaluations, 6)
study of laboratory simulation of environmental events, and 7) study or measurement of
pollutant transport and fate, including dispersion models.
PERFORMANCE AUDITS
Procedures used to determine quantitatively the accuracy of the total measurement
system or component parts thereof.
QUALITY ASSURANCE
The total integrated program for assuring the reliability of monitoring and measurement
data. A system for integrating the quality planning, quality assessment, and quality
improvement efforts to meet user requirements.
QUALITY ASSURANCE PROGRAM PLAN
An orderly assemblage of management policies, objectives, principles, and general
procedures by which an agency or laboratory outlines how it intends to produce data of
known and accepted quality.
QUALITY ASSURANCE PROJECT PLAN
An orderly assembly of detailed and specific procedures which delineates how data of
known and acceptable quality are produced for a specific project. (A given agency or
laboratory would have only one quality assurance plan, but would have a specific Quality
Assurance Project Plan(QAPP) for each of its projects.)
QUALITY CONTROL
The routine application of procedures for obtaining prescribed standards of performance
in the monitoring and measurement process.
STANDARD OPERATING PROCEDURE (SOP)
A written document that details an operation, analysis, or action whose mechanisms are
thoroughly prescribed and that is commonly accepted as the method for performing
certain tasks.
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APPENDIX B
CODE OF FEDERAL REGULATIONS
TITLE 40: PROTECTION OF THE ENVIRONMENT
Part 261: Identification and Listing of Hazardous Waste
as amended through July 1, 1984
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Environmental Protection Agoncy
PART 261— IDENTIFICATION AND
LISTING OF HAZARDOUS WASTE
Sec.
261.1 Purpose mnd icope.
261.3 Definition of solid wute.
261.3 Definition of hazardous waste.
261.4 Exclusions.
261.5 Special requirements for hazardous
waste generated by small quantity gen-
erators.
261.6 Requirement* for recyclable materi-
als.
261.7 Residues of hazardous waste In
empty containers.
Urlifict *f HawsWi Wmto «nd fw U»H«fl
Wmtot
261.10 Criteria for Identifying the charac-
teristics of hazardous waste.
261.11 Criteria for listing hazardous waste.
SofcfM
261.20
261.21
261.22
261.23
261.24
General.
Characteristic of Instability.
Characteristic of corroslvity.
Characteristic of reactivity.
Characteristic of EP toxlclty.
Sufcp
Ucta *f H«ur4*v* W««M
261.30 General.
261.31 Hazardous wastes from non-specific
sources.
261.32 Hazardous wastes from specific
sources.
261.33 Discarded commercial chemical
products, off-specification species, con-
tainer residues, and spill residues there-
of.
APPENDICES
APPENDIX I—REPRESENTATIVE SAMPLING
MTTHODS
APPENDIX II—KP Toxicrrv TEST PROCE-
DURES
APPENDIX III—CHEMICAL ANALYSIS TEST
METHODS
APPENDIX IV—(RESERVED FOR RADIOACTIVE
WASTE TEST METHODS]
APPENDIX V—(RESERVED FOB INFECTIOUS
WASTE TREATMENT SPECIFICATIONS]
APPENDIX VI—[RESERVED FOR ETIOLOOIC
AGENTS]
APPENDIX VII—BASIS FOR LISTING HAZARD-
OUS WASTE
APPENDIX VIII—HAZARDOUS CONSTITUENTS
APPENDIX IX—WASTES EXCLUDED UNDER
1(260.20 AND 260.22
§261.1
Sec.
APPENDIX X—METHOD OF ANALYSIS FOR
CLORINATED DIBENZO-P-DIOXINS AND Di-
BENZOFUIIANS
AUTHORITY: Sees. 1006, 2002(a), 3001 and
3002 of the Solid Waste Disposal Act. as
amended by the Resource Conservation and
Recovery Act of 1076. as amended (42 U£.C.
6005. 6«12(a). 6921. and 6022).
SOURCE 45 PR 33110, May 10. 1080. unless
otherwise noted.
Subport A—General
B 261.1 Purpose and scope.
(a) This part Identifies those solid
wastes which are subject to regulation
as hazardous wastes under Parts 262
through 26S and Parts 270. 271. and
124 of this chapter and which are sub-
ject to the notification requirements
of section 3010 of RCRA. In this part:
(1) Subpart A defines the terms
"solid waste" and "hazardous waste,"
Identifies those wastes which are ex-
cluded from regulation under Parts
262 through 265. 270, 271 and 124 and
establishes special management re-
quirements for hazardous waste pro-
duced by small quantity generators
and hazardous waste which is used, re-
used, recycled or reclaimed.
(2) Subpart B sets forth the criteria
used by EPA to identify characteris-
tics of hazardous waste and to list par-
ticular hazardous wastes.
(3) Subpart C identifies characteris-
tics of hazardous waste.
(4) Subpart D lists particular haz-
ardous wastes.
(b)(l) The definition of solid waste
contained in this part applies only to
wastes that also are hazardous for pur-
poses of the regulations implementing
Subtitle C of RCRA. For example, it
does not apply to materials (such as
non-hazardous scrap, paper, textiles,
or rubber) that are not otherwise haz-
ardous wastes and that are recycled.
(2) This part identifies only some of
the materials which are solid wastes
and hazardous wastes under Sections
3007, 3013, and 7003 of RCRA. A mate-
rial which is not defined as a solid
waste in this part, or is not a hazard-
ous waste identified or listed in this
part. Is still a solid waste and a hazard-
§261.2
ous waste for purposes of these sec-
tions If:
(I) In the case of Section* 3007 and
3013. EPA has reason to believe that
the material may be a solid waste
within the meaning of Section
1004(27) of RCRA and a hazardous
waste within the meaning of Section
1004(5) of RCRA: or
(ii) In the case of Section 7003, the
statutory elements are established.
(c) For the purposes of (| 261.2 and
261.6:
(DA "spent material" Is any materi-
al that has been used and as a result
of contamination can no longer serve
the purpose for which it was produced
without processing;
(2) "Sludge" has the same meaning
used in f 260.10 of this chapter:
(3) A "by-product" Is a material that
Is not one of the primary products of a
production process and Is not solely or
separately produced by the production
process. Examples are process residues
such as slags or distillation column
bottoms. The term does not Include a
co-product that is produced for the
general public's use and Is ordinarily
used in the form It is produced by the
process.
(4) A material is "reclaimed" If it Is
processed to recover a usable product,
or if it is regenerated. Examples are
recovery of lead values from spent bat-
teries and regeneration of spent sol-
vents.
(5) A material is "used or reused" if
It Is either
(1) Employed as an ingredient (In-
cluding use as an Intermediate) in an
industrial process to make a product
(for example, distillation bottoms
from one process used as feedstock In
another process). However, a material
will not satisfy this condition if dis-
tinct components of the material are
recovered as separate end products (as
when metals are recovered from
metal-containing secondary materials);
or
(11) Employed in a particular func-
tion or application as an effective sub-
stitute for a commercial product (for
example, spent pickle liquor used as
phosphorous precipitant and sludge
conditioner in wastewater treatment).
(6) "Scrap metal" is bits and pieces
of metal parts (e.g..) bars, turnings.
40 CFR Ch. I (7-1-M Edition)
rods, sheets, wire) or metal pieces that
may be combined together with bolts
or soldering (.e.g.. radiators, scrap auto-
mobiles, railroad box cars), which
when worn or superfluous can be recy-
cled.
(7) A material Is "recycled" If It is
used, reused, or reclaimed.
(8) A material IB "accumulated spec-
ulatively" If it Is accumulated before
being recycled. A material Is not accu-
mulated speculatlvely, however, if the
person accumulating it can show that
the material Is potentially recyclable
and has a feasible means of being recy-
cled; and that—during the calendar
year (commencing on January 1)—the
amount of material that Is recycled, or
transferred to a different site for recy-
cling, equals at least 75 percent by
weight or volume of the amount of
that material accumulated at the be-
ginning of the period. In calculating
the percentage of turnover, the 75 per-
cent requirement Is to be applied to
each material of the same type
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Environmental Protection Agency
(U) Recycled, as explained in para-
graph (c) of this section; or
(ill) Considered inherently itxute-
lUce, as explained In paragraph (d) of
this section.
(b) Materials are solid waste If they
are abandoned by being:
(1) Disposed of; or
(2) Burned or incinerated: or
(3) Accumulated, stored, or treated
(but not recycled) before or in lieu of
being abandoned by being disposed of,
burned, or Incinerated.
(c) Materials are solid wastes if they
are recycled—or accumulated, stored.
or treated before recycling—as speci-
fied in paragraphs (cKl) through
Materials listed In paragraph
(d)(l) of this section.
(f) Documentation of claim* that
materials are not tolid wattes or an
conditionally exempt from regulation.
Respondents in actions to enforce reg-
ulations implementing Subtitle C of
RCRA who raise a claim that a certain
material Is not a solid waste, or Is con-
ditionally exempt from regulation.
must demonstrate that there is a
known market or disposition for the
material, and that they meet the
terms of the exclusion or exemption.
In doing so, they must provide appro-
priate documentation (such as con-
tracts showing that a second person
uses the material as an ingredient in a
production process) to demonstrate
that the material is not a waste, or is
exempt from regulation. In addition,
owners or operators of faculties claim-
ing that they actually are recycling
materials must show that they have
the necessary equipment to do so.
[60 FR 604, Jan. 4. 1985)
Emcrmt DATI Nore At 50 PR «64, Jan.
4, 1885. | 261.2 was revised, effective July 5.
196S (except for paragraph (e) which was ef-
fective December 20. 1984). For the conven-
ience of the user, the superseded text Is set
out below:
40 CFR Ch. I (7-l-a5 E«Uti«i)
IMU Definition of *olU wuU.
(a) A Mild WMU Is city garbage, refuse.
sludge or any other waste material which U
not excluded under I 361.4(a).
(b) An "other waste materlaT U any solid,
liquid. semi-solid or contained gaseous mate-
rial, resulting from Industrial, commercial.
mining or agricultural operation*, or from
community activities which:
(1) b discarded or Is being accumulated.
stored or physically, chemically or biologi-
cally treated prior to being discarded: or
(2) Has served Its original Intended use
and sometimes Is discarded; or
(3) Is a manufacturing or mining by-prod-
uct and sometimes Is discarded.
(c) A material Is "discarded" U It U aban-
doned (and not used, re-used, reclaimed or
recycled) by being:
(1) Disposed of: or
O) Burned or Incinerated, except where
the material Is being burned as a fuel for
the purpose of recovering usable energy; or
(» Physically, chemically, or biologically
treated (other than burned or Incinerated)
In Ueu of or prior to being disposed of.
(d) A material ls "disposed or U It ls dis-
charged, deposited. Injected, dumped,
spilled, leaked or placed into or on any land
or water so that such material or any con-
stituent thereof may enter the environment
or be emitted Into the air or discharged Into
ground or surface waters.
(e) A "manufacturing or mining by-prod-
uct" Is a material that Is not one of the pri-
mary products of a particular manufactur-
ing or mining operation. Is a secondary and
Incidental product of the particular oper-
ation and would not be solely and separate-
ly manufactured or mined by the particular
manufacturing or mining operation. The
term does not Include an Intermediate man-
ufacturing or mining- product which results
from one of the steps In a manufacturing or
mining process and Is typically processed
through the next step of the process within
a short time.
1260 Definition of hazardous waste.
(a) A solid waste, as defined in
1201.2. la a hazardous waste U:
(1) It is not excluded from regula-
tion as a hazardous waste under
I 2«1.4(b); and
(2) It meets any of the following cri-
teria:
(1) It exhibits any of the characteris-
tics of hazardous waste identified in
Subpart C.
(11) It is listed In Subpart D and has
not been excluded from the lists In
Subpart D under f{ 200.20 and 200.22
of this chapter.
353
354
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vlronmtintal Protection Agoncy
111) It is a mixture of a solid waste
d a hazardous waste that is listed in
ibpart D solely because It exhibits
e or more of the characteristics of
.zardous waste identified in Subpart
unless the resultant mixture no
ager exhibits any characteristic of
.zardous waste identified in Subpart
;iv) It is a mixture of solid waste and
.e or more hazardous wastes listed In
ibpart D and has not been excluded
3m this paragraph under || 260.20
id 260.22 of this chapter; however,
e following mixtures of solid wastes
id hazardous wastes listed In Sub-
j-t D are not hazardous wastes
xcept by application of paragraph
)(2) (1) or (U) of this section) if the
nerator can demonstrate that the
ixture consists of wastewater the dls-
iarge of which is subject to regula-
3n under either Section 402 or See-
in 307(b) of the Clean Water Act (in-
jding wastewater at facilities which
we eliminated the discharge of
istewater) and:
(A) One or more of the following
>ent solvents listed in 8261.31—
j-bon tetrachloride, tetrachloroethy-
ne, trichoroethylene—provided that
ie maximum total weekly usage of
lese solvents (other than the
nounts that can be demonstrated not
* be discharged to wastewater) divld-
1 by the average weekly flow of
astewater into the headwords of the
^clltty's wastewater treatment or pre-
•eatment system does not exceed 1
art per million; or
(B) One or more of the following
>ent solvents listed in i 261.31— meth-
,ene chloride. 1.1.1-trlchloroethane,
ilorobenzene. o-dichlorobenzene, cre-
ils, cresyllc acid, nitrobenzene, tolu-
ne. methyl ethyl ketone, carbon dl-
ilfide. isobutanol, pyridlne. spent
olorofluorocarbon solvents—provided
lat the maximum total weekly usage
[ these solvents (other than the
mounts that can be demonstrated not
3 be discharged to wastewater) dlvid-
d by the average weekly flow of
•a&tewater into the headworks of the
icillty's wastewater treatment or pre-
reatment system does not exceed 25
arts per million; or
(C) One of the following wastes
ated in i 261.32—heat exchanger
§ 261.3
bundle cleaning sludge from the petro-
leum refining Industry (EPA Hazard-
ous Waste No. KOSO); or
(D) A discarded commercial chemi-
cal product, or chemical Intermediate
listed In ( 261.33, arising from at mini-
mis losses of these materials from
manufacturing operations in which
these materials are used as raw mate-
rials or are produced In the manufac-
turing process. For purposes of this
subparagraph. "de minimi*" losses In-
clude those from normal material han-
dling operations (e.g. spills from the
unloading or transfer of materials
from bins or other containers, leaks
from pipes, valves or other devices
used to transfer materials); minor
leaks of process equipment, storage
tanks or containers; leaks from well-
maintained pump packings and seals;
sample purgings; relief device dis-
charges; discharges from safety show-
ers and rinsing and cleaning of person-
al safety equipment; and rinsate from
empty containers or from containers
that are rendered empty by that rins-
ing; or
(E) Wastewater resulting from labo-
ratory operations containing toxic (T)
wastes listed In Subpart D, provided
that the annuallzed average flow of
laboratory wastewater does not exceed
one percent of total wastewater flow
into the headworks of the facility's
wastewater treatment or pre-treat-
ment system, or provided the wastes,
combined annualized average concen-
tration does not exceed one part per
million in the headworks of the facili-
ty's wastewater treatment or pre-treat-
ment facility. Toxic (T) wastes used in
laboratories that are demonstrated
not to be discharged to wastewater are
not to be Included In this calculation.
(b) A solid waste which is not ex-
cluded from regulation under para-
graph (aXI) of this section becomes a
hazardous waste when any of the fol-
lowing events occur:
(1) In the case of a waste listed in
Subpart D. when the waste first meets
the listing description set forth in
Subpart D.
(2) In the case of a mixture of solid
waste and one or more listed hazard-
ous wastes, when a hazardous waste
listed in Subpart D is first added to
the solid waste.
§ 261.4
(3) In the case of any other waste
(Including a waste mixture), when the
waste exhibits any of the characteris-
tics Identified in Subpart C.
(c) Unless and until It meets the cri-
teria of paragraph (d):
(1)A hazardous waste will remain a
hazardous waste.
(2X0 Except as otherwise provided
in paragraph (c)(2)(ll> of this section,
any solid waste generated from the
treatment, storage, or disposal of a
hazardous waste. Including any sludge,
spill residue, ash, emission control
dust, or leachate (but not including
precipitation run-off) is a hazardous
waste. (However, materials that are re-
claimed from solid wastes and that are
used beneficially are not solid wastes
and hence are not hazardous wastes
under this provision unless the re-
claimed material is burned for energy
recovery or used in a manner consti-
tuting disposal.)
(U) The following solid wastes are
not hazardous even though they are
generated from the treatment, stor-
age, or disposal of a hazardous waste,
unless they exhibit one or more of the
characteristics of hazardous waste: (A)
Waste pickle liquor sludge generated
by lime stabilization of spent pickle
liquor from the iron and steel industry
(SIC Codes 331 and 332).
(d) Any solid waste described in
paragraph (c) of this section is not a
hazardous waste if It meets the follow-
ing criteria:
(1) In the case of any solid waste. It
does not exhibit any of the character-
Istlcs of hazardous waste identified in
Subpart C.
(2) In the case of a waste which is a
listed waste under Subpart D, contains
a waste listed under Subpart D or is
derived from a waste listed in Subpart
D. it also has been excluded from
paragraph (c) under |( 260.20 and
260.22 of this chapter.
[46 FR 33118, May 19. 1080. u amended at
46 FR 56588, Nov. 11, 1981; 60 FR 14218.
Apr. 11, 1985}
Erncnvi DATI Norr At 60 FR 664, Jan.
4. 1986. and corrected at 60 FR 14219. Apr.
11. 1985, |261.3(cK2) was revised, effective
July 5, 1985. For the convenience of the
user, the superseded text Is »et out below:
40 CFR Ch. I (7-1-15 Edition)
I Ml 4 DeflnHlM of haaardaw waste.
(C)' * *
(2X1) Except as otherwise provided In
paragraph
-------
Environmental Protection Agency
recovery furnace and then reused In
the pulping proceu, unleu It Is accu-
mulated ipeculatlvely as defined In
I 261.KO of this chapter.
(7) Spent sulfurtc acid used to
produce virgin sulfurtc acid, unless It
is accumulated speculatlvely as de-
fined In | 261.Kc) of this chapter.
(b) Solid wutet which art not hat-
ardout vxutei. The following solid
wastes are not hazardous wastes:
(1) Household waste, including
household waste that has been collect-
ed, transported, stored, treated, dis-
posed, recovered (e.p.. refuse-derived
fuel), or reused. "Household waste"
means any waste material (Including
garbage, trash and sanitary wastes In
septic tanks) derived from households
(Including single and multiple resi-
dences, hotels and motels, bunk-
houses, ranger stations, crew quarters,
campgrounds, picnic grounds, and day-
use recreation areas).
(2) Solid wastes generated by any of
the following and which are returned
to the soils as fertilizers:
(1) The growing and harvesting of
agricultural crops.
(11) The raising of anim^iy, Including
animal manures.
(3) Mining overburden returned to
the mine site.
(4) Fly ash waste, bottom ash waste,
slag waste, and flue gas emission con-
trol waste generated primarily from
the combustion of coal or other fossil
fuels.
(5) Drilling fluids, produced waters.
and other wastes associated with the
exploration, development, or produc-
tion of crude oil, natural gas or geo-
thermal energy.
(6X1) Wastes which fail the test for
the characteristic of EP toxiclty be-
cause chromium is present or are
listed In Subpart D due to the pres-
ence of chromium, which do not fall
the test for the characteristic of EP
toxicity for any other constituent or
are not listed due to the presence of
any other constituent, and which do
not fall the text for any other charac-
teristic, if it is shown by a waste gener-
ator or by waste generators that:
(A) The chromium in the waste is
exclusively (or nearly exclusively) trt-
valent chromium; and
§ 261.4
(B) The waste Is generated from an
Industrial process which uses trivalent
chromium exlcuslvely (or nearly exclu-
sively) and the process does not gener-
ate hexavalent chromium; and
(C) The waste Is typically and fre-
quently managed In non-oxidizing en-
vironments.
(II) Specific wastes which meet the
standard in paragraphs (b)(6)UMA),
(B) and (C) (so long as they do not fall
the test for the charactrtstlc of EP
toxiclty. and do not fall the test for
any other characteristic) are:
(A) Chrome (blue) trimmings gener-
ated by the following subcategories of
the leather tanning and finishing In-
dustry; hair pulp/chrome tan/retan/
wet finish; hair save/chrome tan/
retan/wet finish; re tan/wet finish; no
beamhouse; through-the-blue; and
shearling.
(B) Chrome (blue) shavings generat-
ed by the following subcategories of
the leather tanning and finishing In-
dustry: hair pulp/chrome tan/retan/
wet finish; hair save/chrome tan/
retan/wet finish; retan/wet finish; no
beamhouse; through-the-blue; and
shearling.
(C) Buffing dust generated by the
following subcategories of the leather
tanning and finishing Industry; hair
pulp/chrome tan/retan/wet finish;
hair save/chrome tan/retan/wet
finish; retan/wet finish; no beam-
house; through-the-blue.
(D) Sewer screenings generated by
the following subcategories of the
leather tanning and finishing indus-
try: hair pulp/crome tan/retan/wet
finish; hair save/chrome tan/retan/
wet finish; retan/wet finish; no beam-
house; through-the-blue; and shear-
ling.
(E) Wastewater treatment sludges
generated by the following subcategor-
ies of the leather tanning and finish-
Ing industry: hair pulp/chrome tan/
retan/wet finish; hair save/chrome
tan/retan/wet finish; retan/wet
finish; no beamhouse; through-the-
blue; and shearling.
(F) Wastewater treatment sludes
generated by the following subcategor-
ies of the leather tanning and finish-
Ing Industry: hair pulp/chrome tan/
retan/wet finish; hair save/chrome-
§ 261.4
tan/retan/wet finish; and through-
the-blue.
(O) Waste scrap leather from the
leather tanning Industry, the shoe
manufacturing Industry, and other
leather product manufacturing Indus-
tries.
(H) Wastewater treatment sludges
from the production of TiO, pigment
using chromium-bearing ores by the
chloride process.
(7) Solid waste from the extraction.
beneficlatlon and processing of ores
and minerals (including coal), includ-
ing phosphate rock and overburden
from the mining of uranium ore.
(8) Cement kiln dust waste.
(9) Solid waste which consists of dis-
carded wood or wood products which
falls the test for the characteristic of
EP toxiclty and which is not a hazard-
ous waste for any other reason If the
waste is generated by persons who uti-
lize the arsenical-treated wood and
wood products for these materials' In-
tended end use.
(c) Hazardous wastes which are ex-
empted from certain regulations. A
hazardous waste which is generated in
a product or raw material storage
tank, a product or raw material trans-
port vehicle or vessel, a product or raw
material pipeline, or In a manufactur-
ing process unit or an associated non-
waste-treatment-manufacturing unit,
is not subject to regulation under
Parts 262 through 265. 270. 271 and
124 of this chapter or to the notifica-
tion requirements of Section 3010 of
RCRA until it exits the unit In which
It was generated, unless the unit Is a
surface Impoundment, or unless the
hazardous waste remains In the unit
more than 90 days after the unit
ceases to be operated for manufactur-
ing, or for storage or transportation of
product or raw materials.
(d) Samples. (1) Except as provided
In paragraph (d)(2) of this section, a
sample of solid waste or a sample of
water, soil, or air, which Is collected
for the sole purpose of testing to de-
termine its characteristics or composi-
tion, is not subject to any require-
ments of this part or Parts 262
through 267 or Part 270 or Part 124 of
this chapter or to the notification re-
quirements of Section 3010 of RCRA,
when:
40 CM Ch. I (7-1-C5 Edition)
(1) The sample Is being transported
to a laboratory for the purpoae of tast-
ing; or
(II) The sample Is being transported
back to the sample collector after test-
ing; or
(111) The aample Is being stored by
the sample collector before transport
to a laboratory for testing; or
(Iv) The aample is being stored In a
laboratory before testing; or
(v) The sample Is being stored In a
laboratory after testing but before It Is
returned to the aample collector or
(vl) The aample Is being stored tem-
porarily In the laboratory after testing
for a specific purpose (for example,
until conclusion of a court case or en-
forcement action where further test-
Ing of the aample may be necessary).
(2) In order to qualify for the ex-
emption In paragraphs (dXl) (1) and
(11) of this section, a sample collector
shipping samples to a laboratory and a
laboratory returning samples to a
aample collector must:
(1) Comply with U.S. Department of
Transportation (DOT). U.S. Postal
Service (USPS), or any other applica-
ble snipping requirements: or
(11) Comply with the following re-
quirements if the sample collector de-
termines that DOT, USPS. or other
shipping requirements do not apply to
the shipment of the sample:
(A) Assure that the following Infor-
mation accompanies the sample:
(1) The aample collector's name.
mailing- address, and telephone
number
(2) The laboratory's name, mailing
address, and telephone number
(J) The quantity of the sample;
(4) The date of shipment; and
(5) A description of the sample.
(B) Package the sample so that It
does not leak, spill, or vaporize from
Its packaging.
(3) This exemption does not apply If
the laboratory determines that the
waste Is hazardous but the laboratory
is no longer meeting any of the condi-
tions stated in paragraph (dXl) of this
section.
(45 PR 33119. May 19, 1880. as amended at
46 PR 72037, Oct. 30. 1980; 45 PR 70620
Nov. 19. 1980; 45 PR 78931. Nov. 25. 1980: 45
PR 80287. Dec. 4, 1980: 46 PR 27476. Hay
20. 1981; 46 PR 47429, Sept. 25. 1981; 48 PR
357
358
-------
Environmental Protection Agency
14293. Apr. 1. 1883; 48 PR 10116. June 30.
1983; 49 FR 44980, Nov. 13. 1984: 80 PR 645.
Jut. 4. 1986: 60 FR 14219. Apr. 11. 1986]
Emcrivc DAT* NOTE At BO FR 686. Jan.
4. 1986. as corrected at 60 FR 14219. Apr. 11.
1986. |281.4(3).
or 266.36 is not Included in the quanti-
ty determinations of this section and
is not subject to any requirements of
this section. Hazardous waste that is
subject to the requirements of {261.6
(b) and (c) and Subparts C, D. and F
of Part 266 is included in the quantity
determination of this section and is
subject to the requirements of this
section.
(d) In determining the quantity of
hazardous waste he generates, a gener-
ator need not include:
(1) His hazardous waste when it is
removed from on-site storage; or
(2) Hazardous waste produced by on-
slte treatment of his hazardous waste.
(e) If a small quantity generator
generates acutely hazardous waste in a
calendar month in quantities greater
than set forth below, all quantities of
that acutely hazardous waste are sub-
ject to regulation under Parts 262
through 265 and Parts 270 and 124 of
this chapter, and the notification re-
quirements of Section 3010 of RCRA:
(DA total of one kilogram of acute
hazardous wastes listed in {{ 261.31.
261.32. or 261.33(e).
(2) A total of 100 kilograms of any
residue or contaminated soil, waste or
5 261.5
other debris resulting from the clean-
up of a spill, into or on any land or
water, of any acute hazardous wastes
listed in if 261.31, 261.32. or 261.33(e).
(f) A small quantity generator may
accumulate hazardous waste on-site. If
he accumulates at any time more than
a total of 1000 kilograms of his haz-
ardous waste, or his acutely hazardous
wastes In quantities greater than set
forth in paragraph (eXl) or (e)(2) of
this section, all of those accumulated
wastes for which the accumulation
limit was exceeded are subject to regu-
lation under Parts 262 through 265
and Parts 270 and 124 of this chapter,
and the notification requirements of
Section 3010 of RCRA. The time
period of | 262.34 for accumulation of
wastes on-slte begins for a small quan-
tity generator when the accumulated
wastes exceed the applicable exclusion
level.
(g) In order for hazardous waste gen-
erated by a small quantity generator
to be excluded from full regulation
under this section, the generator must:
(1) Comply with {262.11 of this
chapter,
(2) If he stores his hazardous waste
on-site. store It in compliance with the
requirements of paragraph (f) of this
section: and
(3) Either treat or dispose of his haz-
ardous waste in an on-site facility, or
ensure delivery to an off-site storage,
treatment or disposal facility, either of
which is:
(1) Permitted under Part 270 of this
chapter;
(il) In interim status under Parts 270
and 265 of this chapter;
(ill) Authorized to manage hazard-
ous waste by a State with a hazardous
waste management program approved
under Part 271 of this chapter;
(Iv) Permitted, licensed or registered
by a State to manage municipal or in-
dustrial solid waste; or
(v) A facility which:
(A) Beneficially uses or re-uses, or le-
gitimately recycles or reclaims his
waste; or
(B) Treats his waste prior to benefi-
cial use or re-use, or legitimate recy-
cling or reclamation.
(h) Hazardous waste subject to the
reduced requirements of this section
may be mixed with non-hazardous
§ 261.6
waste and remain subject to these re-
duced requirements even though the
resultant mixture exceeds the quanti-
ty limitations Identified in this section.
unless the mixture meets any of the
characteristics of hazardous wastes
Identified In Subpart C.
(1) If a small quantity generator
mixes a solid waste with a hazardous
waste that exceeds a quantity exclu-
sion level of this section, the mixture
is subject to full regulation.
(45 FR 70823, Nov. 19. 1980. as amended at
48 FR 34687. July 2. 1981: 48 FR 14294. Apr.
1, 1983; 80 FR 886. Jan. 4. 1985: 80 FR 1999.
Jan. 14. 1988: 50 FR 14219. Apr. 11. 19881
Emcrm D*« Wore: At 50 FR 885. Jan.
4. 1985. aa corrected at 60 FR 14219. Apr. 11.
1986. I 261.6(c) wa* revised, effective July 6.
1986. Al 60 FR 1999. Jan. 14. 1985. | 201.5
-------
Environmental Protection Agoncy
3010 of RCRA. except as provided in
paragraph (a) of this section.
(cKl) Owners or operators of facili-
ties that store recyclable materials are
regulated under all applicable provi-
sions of Subparts A through L of Parts
264 and 265 and Parts 270 and 124 of
this chapter and the notification re-
quirement under Section 3010 of
RCRA, except as provided In para-
graph (a) of this section.
(2) Owners or operators of facilities
that recycle recyclable materials with-
out storing them before they are recy-
cled are subject to the following re-
quirements, except as provided in
paragraph (a) of this section:
(I) Notification requirements under
Section 3010 of RCRA:
(11) Sections 265.71 and 265.72 (deal-
ing with the use of the manifest and
manifest discrepancies) of this chap-
ter.
[50 FR 885. Jan. 4. 1985]
Emcerrvc DAW None At 60 FR 666. Jan.
4, 1886. I 261.6 waa revised, effective July 6.
1086. For the convenience of the uier. the
superseded text Is set out below:
IM1.C Special requirement! for haxardoui
waste which li med, re-iued, recycled or re-
claimed.
(a) Except u otherwise provided in para-
graph (b) of this section, a hazardous waste
which meets any of the following criteria Is
not subject to regulation under Parts 262
through 266 or Parts 270, 271. and 124 of
this Chapter and Is not subject to the notifi-
cation requirements of Section 3010 of
RCRA until such time as the Administrator
promulgates regulations to the contrary:
(1) It Is being beneficially used or re-used
or legitimately recycled or reclaimed.
(2) It Is being accumulated, stored or
physically, chemically or biologically treat-
ed prior to beneficial use or re-use or legiti-
mate recycling or reclamation.
(3) It is one of the following materials
being used, reused, recycled or reclaimed In
the specified manner
(I) Spent pickle liquor which is reused In
wastewater treatment at a facility holding a
National Pollutant Discharge Elimination
System (NPDES) permit, or which is being
accumulated, stored, or physically, chemi-
cally or biologically treated before such
reuse.
(b) Except for those wastes listed in para-
graph (a)(3) of this section, a hazardous
waste that is a sludge, or that Is listed In
I 261.31 or | 261.32, or that contains one or
more hazardous wastes listed In | 261.31 or
I 261.32: and that Is transported or stored
§ 261.7
prior to being used, re-used, recycled, or re-
claimed Is subject to the following require-
ments with respect to such transporatlon or
storage:
(1) Notification requirements under Sec-
tion 3010 RCRA.
(2) Part 262 of this chapter.
(3) Part 263 of this chapter.
(4) Applicable provisions of Subparts A
through L of Part 264 of this chapter;
(6) Applicable provisions of Subparts A
through L of Part 26S of this chapter
(6) Parts 270 and 124 of this chapter, with
respect to storage facilities.
[45 FR 33110. May 10, I960, as amended at
46 FR 44973. Sept. 8, 1981; 48 FR 2532. Jan.
20, 1983; 48 FR 14294, Apr. 1. 1983]
B 261.7 Residues of hazardous waste In
empty containers.
(a)(l) Any hazardous waste remain-
ing in either (1) an empty container or
(11) an Inner liner removed from an
empty container, as defined in para-
graph (b) of this section. Is not subject
to regulation under Parts 261 through
265, or Part 270 or 124 of this chapter
or to the notification requirements of
Section 3010 of RCRA.
(2) Any hazardous waste in either (1)
a container that is not empty or (il) an
Inner liner removed from a container
that is not empty, as defined In para-
graph (b) of this section. Is subject to
regulation under Parts 261 through
265, and Parts 270 and 124 of this
chapter and to the notification re-
quirements of Section 3010 of RCRA.
(b)(l) A container or an inner liner
removed from a container that has
held any hazardous waste, except a
waste that is a compressed gas or that
Is Identified as an acute hazardous
waste listed in {{261.31. 261.32, or
261.33(e) of this chapter is empty if:
(1) All wastes have been removed
that can be removed using the prac-
tices commonly employed to remove
materials from that type of container,
e.g., pouring, pumping, and aspirating,
and
(11) No more than 2.5 centimeters
(one inch) of residue remain on the
bottom of the container or Inner liner,
or
(1I1XA) No more than 3 percent by
weight of the total capacity of the
container remains In the container or
inner liner If the container is less than
or equal to 110 gallons In size, or
§261.10
(B) No more than 0.3 percent by
weight of the total capacity of the
container remains In the container or
inner liner if the container Is greater
than 110 gallons In size.
(2) A container that has held a haz-
ardous waste that is a compressed gas
is empty when the pressure in the con-
tainer approaches atmospheric.
(3) A container or an Inner liner re-
moved from a container that has held
an acute hazardous waste listed In
|| 261.31, 261.32, or 261.33(e> is empty
If:
(I) The container or Inner liner has
been triple rinsed using a solvent capa-
ble of removing the commercial chemi-
cal product or manufacturing chemi-
cal Intermediate;
(II) The container or Inner liner has
been cleaned by another method that
has been shown in the scientific litera-
ture, or by tests conducted by the gen-
erator, to achieve equivalent removal;
or
(111) In the case of a container, the
Inner liner that prevented contact of
the commercial chemical product or
manufacturing chemical Intermediate
with the container, has been removed.
(45 FR 78529. Nov. 25. 1080. as amended at
47 FR 36097, Aug. 18, 1082: 48 FR 14204,
Apr. 1.1083: 50 FR 1099. Jan. 14. 1985]
EFFTCTTVX DATE NOTE At 50 FR 1999, Jan.
14. 1985, |261.7(b)U> and (3) Introductory
texts were revised, effective July 15. 1985.
For the convenience of the user, the super-
seded text Is set out below:
IZ61.7 Residues of haiardoiu waste In empty
container*.
(bKl) A container or an inner liner re-
moved from a container that has held any
hazardous waste, except a waste that Is a
compressed gas or that Is Identified in
I 261.33(0 of this chapter, is empty if:
(3) A container or an Inner liner removed
from a container that has held a hazardous
waste identified In I 261.33(c) of this chap-
ter Is empty if:
40 OR Ch. I (7-145 Edition)
Subpart R—Criteria for Identifying
Hi* Characteristics of Hazardous
Watt* and for Lifting Hazardous
Wast*
1261.10 Criteria for identifying the char-
acteristic* of hazardous waste.
(a) The Administrator shall identify
and define a characteristic of hazard-
ous waste in Subpart C only upon de-
termining that:
(DA solid waste that exhibits the
characteristic may:
(1) Cause, or significantly contribute
to, an Increase in mortality or an in-
crease in serious irreversible, or inca-
pacitating reversible. Illness: or
(11) Pose a substantial present or po-
tential hazard to human health or the
environment when It Is improperly
treated, stored, transported, disposed
of or otherwise managed; and
(2) The characteristic can be:
(1) Measured by an available stand-
ardized test method which Is reason-
ably within the capability of genera-
tors of solid waste or private sector
laboratories that are available to serve
generators of wild waste; or
(11) Reasonably detected by genera-
tors of solid waste through their
knowledge of their waste.
• 261.11 Criteria for listing hazardous
waste.
(a) The Administrator shall list a
solid waste as a hazardous waste only
upon determining that the solid waste
meets one of the following criteria:
(1) It exhibits any of the character-
istics of hazardous waste identified in
Subpart C.
(2) It has been found to be fatal to
humans in low doses or, in the absence
of data on human toxicity, it has been
shown in studies to have an oral LD 50
toxicity (rat) of less than 50 milli-
grams per kilogram, an inhalation LC
50 toxicity (rat) of less than 2 milli-
grams per liter, or a dermal LD 50 tox-
icity (rabbit) of less than 200 milli-
grams per kilogram or is otherwise ca-
pable of causing or significantly con-
tributing to an Increase In serious Irre-
versible, or incapacitating reversible,
illness. (Waste listed In accordance
with these criteria will be designated
Acute Hazardous Waste.)
361
362
-------
Environmental Protection Agency
(3) It contaiiu any of the toxic con-
stituents listed in Appendix VIII
unless, after considering any of the
following factors, the Administrator
concludes that the waste is not capa-
ble of posing a substantial present or
potential hazard to human health or
the environment when improperly
treated, stored, transported or dis-
posed of. or otherwise managed:
(I) The nature of the toxiclty pre-
sented by the constituent.
(11) The concentration of the constit-
uent in the waste.
-------
Environmental Protection Agoncy
or a Class B explosive as defined in 49
CFR 173.88.
(b) A solid wute that exhibits the
characteristic of reactivity, but Is not
listed as a hazardous waste In Subpart
D. has the EPA Hazardous Waste
Number of D003.
I 261.24 ChBracteriitic of EP toxtclty.
(a) A solid waste exhibits the charac-
teristic of EP toxiclty U. using the test
methods described In Appendix II or
equivalent methods approved by the
Administrator under the procedures
set forth in 1(260.20 and 260.21. the
extract from a representative sample
of the waste contains any of the con-
taminants listed In Table I at a con-
centration equal to or greater than the
respective value given In that Table.
Where the waste contains less than 0.5
percent filterable solids, the waste
Itself, after filtering. Is considered to
be the extract for the purposes of this
section.
(b) A solid waste that exhibits the
characteristic of EP toxlcity, but is not
listed as a hazardous waste In Subpart
D, has the EPA Hazardous Waste
Number specified In Table I which cor-
responds to the toxic contaminant
causing It to be hazardous.
TABLE I—MAXIMUM CONCENTRATION OF CON-
TAMINANTS FOR CHARACTERISTIC OF EP
Toxtcrrv
§ 261.30
EPA
hatardou*
•nut*
numbar
PO04 . ,
O005
DOOfi
0007
DOOO
DOTJ8 '.
D010
D011
0012
0013
0014
001 S
Contammam
Bcnun,
f^aWtatMMIt
Chromum _...
\.mfrt
Marcury
SDvar _.
Endnn (1.2,3.4, 10,104i*nach'
1 .4.4a.$.e,7.64*«cuhydn>
1,4 *ndo. aodo-S.»-Om»ttv
•nc-naphthalan*.
Und*n* (1^.3.4. 5,Ww«». chlor-
ocydoh*v*n*. gamm* aiomar.
Matnonychlor (1,1.1-Thchkxo-
Z3-U* (p4n*tho«y-
ptwnyl ] •ttiovw) .
Touphana (C-H^X. Tachnical
cnkxiniiad camphana, 87-6*
Barcant ehkirinal.
Manrwn
ton
(makgnm*
5.0
100.0
1.0
S.O
6.0
0.2
1.0
S.O
0.02
0.4
10.0
0.6
TABLE I—MAXIMUM CONCENTRATION OF CON-
TAMINANTS FOR CHARACTERISTIC OF EP
TOXICITY—Continued
EPA
hanrdou*
number
0016
DOI7
Conunwwrt
2.4-D. (2.4.Dcnlarophanoiyaca-
KICK)).
2 4.5-TP SitMl (2 4 S-Tncnto-
fOphanoKypropionic Kid).
Maiknum
lion
(iMhgnimi
par Mar)
10.0
1 0
Subpart D—LUli of Hazardous
Wattot
G 261 JO General.
(a) A solid waste is a hazardous
waste If it Is listed In this subpart.
unless it has been excluded from this
list under }| 260.20 and 260.22.
(b) The Administrator will Indicate
his basis for listing the classes or types
of wastes listed in this Subpart by em-
ploying one or more of the following
Hazard Codes:
IgnnablaWaM*..
CorroaM* Wist*
R««ctr«« WUM_
EPtcndc Wn»*_
Acutt Huantoui Wttta..
TodC Wa*ta..
(E)
IH)
m
Appendix VII Identifies the constitu-
ent which caused the Administrator to
list the waste as an EP Toxic Waste
(E) or Toxic Waste (T) in f{ 261.31
and 261.32.
(c) Each hazardous waste listed in
this subpart Is assigned an EPA Haz-
ardous Waste Number which precedes
the name of the waste. This number
must be used in complying with the
notification requirements of Section
3010 of the Act and certain record-
keeping and reporting requirements
under Parts 262 through 265 and Part
270 of this chapter.
(d) The following hazardous wastes
listed in i 261.31 or { 261.32 are subject
to the exclusion limits for acutely haz-
ardous wastes established in {261.5:
EPA Hazardous Wastes Nos. FO20.
FO21. PO22, PO23. PO26. and FO27.
§2*1.31
[45 FK 33110. May 19. 1980. u amended »t
48 FR 14894. Apr. 1. 19§3; 60 PR 2000. Jan.
14, 198S1
EmcTtvc DATE NOTE At M FR 2000. Jan.
14. 198S. I 261.30(d) wu revised, effective
July 16, 1988. For the convenience of the
u§er. the iupewded text Is §et out below:
410 CHI Ch. I (7-1-M WHi.n)
IMIJt
(d) The following hatardous wwtes listed
In I 261.31 or 1361.32 are lubject to the ex-
clusion HmlU for acutely haurdoiu wutes
established In I 261.8: (Reserved)
B 261.31 Huardoui waitei from non-ipeelfle (ouree*.
The following solid wastes are listed hazardous wastes from non-specific
sources unless they are excluded under II 260.20 and 260.22 and listed In Appen-
dix IX.
Induny and EPA hasardou*
•MM No.
Ganarie:
F001...
F002...
F003_.
F004...
FOOS...
Fooe..
F018..
F007._
FOM_
FON_
F010._
F011-.
F012_
F024._
FO20
FO21..
; and •>• tM boaom*
Th* toaoamg apart haloganaiad autnanai u*ad In
trioMoroathytana, nwhylan* Ontario*. 1.1.1-McNoroaliana. carbon MncHond*.
and chKxmalad nuorocarbona, and akidaa* Irom t» racowvy ol n*M KUnnt* in
dagraaang opanbon*.
Th* tottMtog apart hdoganatad njHamt l*t»eMoroa«i»l«na, mathytan* cNnrid*.
>lLl. »an*«aMr, Haatamlar u»auiKm Hudg**, apant cualytt
•ran** kltad in | 2C1.3Z).
WattM (awapl msWMIar and •pant carbon Irom hydraptn cMorlda pachtoroph*n* (rom highly purlnad 2.4.5-
BichlQrophanol.1.
Wuta* lanapt »a«n»*»i and apart carbon Dam hydrogon chtono* puWcatlon)
from VM production or manuaKturing u*a (a* I raaclant chamical Marmadial*. or
component In • lormuH»ng proeaai) ol DamaoMorophanol. or ol Mamtadialai
u**d to product to dartnuba*.
366
m
(D
II. TJ
m
(H.T»
(R.T)
(B.H
-------
environment*! Protection Agoncy
§261.32
9201.32
40 CHI Ok. I (7-145 ftUtloti)
nduaty and EP*.
i No
FO2t
TOM-
TOM.
F027..
FO2S..
tromVM iMnutaculnp, uee (a* a reectanl Chun
• tormuteeng piucnei> ol Mr*-, penta-, or IM
hlorti>» putticaepn)
*, Of oomponant in
Wuw (now* imrtiiatef md «Mrt carbon Irom hydrogen entente purthcakon)
Irom *M production ol nMHrnH on •qupmwil pmvtomr/ uMd to to production
or mmuuicluring UM (M • nueunt chemical Marmaduita. or componanl In •
tormuMng prooaaa) of ki- and tatracMorophanoli. fThn kakng doaf not mduda
wtMm Irom aoupmanl uaad only tor the producbon or uee of Haucnloropnana
kom r«gnry purthad 2,4.6-kioMorophanol.).
INaMai (aioapl waalawatar and apant carbon kom hydrogen chtonda purMicakon)
kom aia producton of inamali on eo^pmani prevnuHy uaed lor »a manulactur-
ing uaa (a* a raadant. chamcal ntarmeoiaia. or componenl in • lonnulatng
nronn) of Mm-, penu-, or hauchlorobaniana under akabne oondram.
tacafoed unuaed tormulaboni comairang t>. Ian-, or pantaoMorophanol or de-
canted unuaed (onnulatona oontanng compoundi den»ad kom meae chlorophan-
oH (Trw eMng doei not tnduda ttxmuujbora containing Haiachlorophena lytha-
aHed kom prapurHied 2.4.S-ktchk>rDphano! a> tna aola componanl).
fleaduaa reaumng rrom me Ironeiaton or thermal keatment of aoH oonumnaujd
««n EPA Hasardoua w«ua No*. FO20, FO21. FO22. FO23, FO». and FO27.
Haiard
(M)
(H)
(H)
(H)
(T)
(4« FR 4617. Jan. 16. 1B81. u amended at 46 PR 27477. May 30. 1981; 49 FR 5312. Feb. 10.
1984; 49 FR 37070. Sept. 21. 1984: BO FR 666. Jan. 4. 1985; 50 FR 2000. Jan. 14. 1985]
Erracnvc DAT* NOTE At 50 FR 665. Jan. 4. 1985, the hazardous waste listings for F007
P008. P009. F010. P011. and P012 were revised, effective July 5. 1985. At 50 FR 2000. Jan. 14
1985. the hazardous waste listings for F020. F021. P022. F023. FQ26. F027. and F028 were
added, effective July 15, 1986. For the convenience of the user, the superseded text is set
out below:
0 261.31 Hazardous wastes from non-specific sources.
Induety and EPA hazardous
waataNo
Haiardout Mate
Hazard
coda
FOO? Spent cyanide plating bath aokitom kom el»iuuuls»ig operation* (except tor (R. T>
preotou* metal* aleeiiuulaiing (pent cyanide plating bath eolubon*).
Plaeng bath Nudges kom th* bonom ol plating bath* from eUr.nupl.um operation* (R, T)
where cyanide* are ueed In the procee* (except tor precious metal* aoctiuununtf
Plaeng ban aludgae).
FOOS Spent »ii»x«ng and cmmng bath solutions kom eiectiuuHliiig operations where (A. T)
cyarade* are ueed In the procee* (except for precious metal* electroplating *P*nt
*UMJ«IU and deanng bath sotutioos)
FOIO Ouencnmg bath tludge from o* battw from metal heat keeong operation* where (R. T)
cyanide* are uaed n tha prcceea (except tor precnu* metal* heat-treaMig
ojuancnng bath aludgea)
F011 Spent cyarad* aokjton* from sen bath pot cleaning kom metal heal keatmg
operabun* (except lor preoou* metal* heat keatmg spent cyanide eokikon* from
«alt bath pot cleaning)
F012 Quenching wealewater treetment aludgea from metal heal treating operations where (T)
cyanide* are uaed ki th* process (except tor preooua metal* heat keatmg
quenctwig waatewaler teaknent dudge*)
0 261.32 Hazardous wastes from specific sources.
The following solid wastes are listed hazardous wastes from specific sources
unless they are excluded under {( 260.20 and 260.22 and listed in Appendix IX.
Induatry and EPA hazardous
watt* No.
Wood pra*arvaiion: K001
Hazardous wait*
Bottom aeoVnent sludge kom the treatment ol waitewalen from wood preserving
prooe**e* that ua* creoaote and/or pentachloroprienol.
367
Hazard
code
ro
Induety end EPA nezarOoua
WaWaaV Nfi
KON
KOM... -
KOOS
Organic Chen ems*.
K010
K011 ,,.,„... :: „„
K013
KOM
KOI 6
K017
K01B
KOI a
KQ20 , I.....,,,...,,...,,,.
Koa
KO94
fctnoa
xntu
KOX
KQZ7 , ,
iron
toot
KMS ..._
KOM
Knao
KM3
K109
KDM
Kins
icriTi ,,.
icon
K10B
K031
K032
K033
K034
K0g7
K035
KOM
K037
KOM _
K040 .._ „
K041 ..
KOM
Hazardous waeu
eajmanta.
Waaneaur treatment abdne Irom tie produeeon el xlnc yi«»» pigment*
Waatawaiar iraatmant tfudpa from Via producton of chroma O.** groan plgmanti
(tvinydroua «* tiydratad).
WMtawatar boatman! •ludaa from Vw fntduoton oflronb.ua ptgman.*
Ovan raaMua from Via producton of chroma o*da groan aajmami..
DMMaHon aMa outi from tha producton of •oataJdahyda from atnytana
Bottom *.ra.vn from lha »a.na.va*ar abtpnar m Via producton of aorytonartla.
fiotnvn atmaun Inpn *>• .M^terttriU eok|fiHi kn MM pnMfud.fn of may****** „ , .
Bottom* from VM acalonHytfca purMcaton column in Via producton of auy.tii.lbia
Btfl bottom* from tha Tftffton of banxyl chtorfda
producton.
Haavy andt from Via aiBMMon of vinyl chtortda in vfnyt cMoftda rfoonai
producton.
Aquaoua ipaot anilmonv calatVH waat* from ftonmaViana.. emdueilnn
D.*tHtatlon bottom tan from Via producton of phanol/aMtona from oumana
Diatttaton bottom* from tha producton of nUiobamaiia by Via ntttton of banMna
S^pf.i*ig rw tart* from Vit producton of mathy athyt pyrtrf.naa
Cantrtruoja and dwittatoon rvtMuaa from tohiana olaoryvnala p^nrvrttm
oattiana.
Haavy anoa from tha haavy andi ookimn from Via producton of 1,1,1«chtoroa«v
ana.
and parcriiorcpairiytana.
of chiorobantanat.
Brin*. .HV • iH. (.-
aaparatary prapurMad brina it not uaad.
proca« uaing grvphrt* anodat In cNorina producton.
Byproduct aalt* generated In tie production of MSMA and cacooVfe add
Wanawater treatment aludoe from th. production of chtordana
WaMawatar and ecrub water Irom the chtomaeon of cyOopentadMn* hi ma
production of chtordana.
™er "olid* from Uu nn.tlki.i ol heiecntaucyclupenuuleii* kt tie producton of
cnioroana.
V^ilordan.W" '*"*"*' hl>nl ™ enlon»n» enwtntlor ki IM producton of
Watlewater keatment »ludge* generated ki the producton ol creoaou
S« bonom* from toluene redamation OKWujbon ki the producton of diauiiolon_
Waateweter gaatmenl ^udoea kom the production ol dtouNolon
waaiawater from me waahng and (tripping of phonMo production . _
rVIW CaWa (IWTI DM flrUalKM) Of dMthytCatipani^*vortflr|ifja»; mr^t tgt H^ mnA— IL-. «»J
phorata. '••— t- —• ~" « •• proounon 01
".«-.--...-, ^aaim.Kii jMuoga rioin tha pfoductw. of lomaptiaiia
Hazard
coda
(T)
(D
ID
(T)
(T)
(T)
(H, T)
(R,T)
(T)
m
rn
ro
(T)
O)
(T)
fO
CD
ro
ro
ro
ro
ro
ro
ro
ro
ro
ro
ro
ro
ro
ro
ro
ro
ro
ro
368
-------
Environmental Protection Agency
6261.33
todunry and EPA huwtiou
MSMlll Ite
KOM -.
EnHoaNaa:
K046
Patroiaurn fanrvngi
K050 — ~_.™~—
fron and staat
K061 _
K062 — -.— —
Secondary toad
KOM
K100
VataftftaiY pTOTtaoautca.*:
K1Q1
KIM
Ink tofmutaaon: KOM
Coking:
KWW
"ft*7
Hazardous waata
production of 2,4.5-T.
2 A-DchlarQptwfKri wat** from ttw producton of 2.44)
UntMtad wastawatar from ths producaon of 2.4-0 . .
Waatawatw traatmant akjdgaa from tha manufacturing, tormulaaon and toadmg of
laad-toaaad «Mtmg compounds.
pjoaorrtd air Aotabon (OAF) float from f» pitrolaum rafnng industry
Stop o»J amulsion tottta from lh» patroiaum rahning industry „.„„....„_„ ,
Haat axchangar bundt* daanng atudga from tha palrotaum raftfwig Industry
API Mpantof atudoa from lha patroiaum rafwwig induatry _ „
Tank bottom* (taadad) from lha patroiaum raArang •ndustry „„
EfiMaton control duat/akudga from tha primary production of sta* in alicaic
lumaoaa.
Spant ptoUa •guor from ataai fmNnQ oparattona . _
Emataton control duat/akidga from aaoondary taad amarang...
Waata •aach.ng aotoaon from aod (aactang of amaann oonlrol duat/aludga from
aaoondary toad antarang.
oaufecat* from arwrac or organo-araanc compounds,
DistMabon la/ raaiduaa from Vts drsOUtoon of anthna-baaad compounds in ttta
pounds
Raariut frtrn fftt utt of acfevatad cartwn to* daootonzaVon in tot produeaon of
Soivant waahas and aludgaa. caua&c waahaa and aludoas, or waiar waahaa and
aiudgaa from tiaaning uba and aqupmani usad In ma formulation of r* from
0*r>n1Mr Iv4f tar t^nlQt twn w¥ "'^ opvnlmnt
Huart
ood*
(1)
0)
(A)
(R)
(T)
("1
(T)
rn
0)
(T)
(T)
m
(C. T)
rn
(T)
fn
(T)
m
(T)
(T)
[46 FR 4618. Jan. 16. 1B81. u amended at 46 FR 27476-27477. May 20. 1B81; 49 PR 37070.
Sept. 21. 19843
6 261.33 Discarded commercial chemical
producti, off-ipeclfleation ipeciet, con-
tainer residue*, and iplll reilduei
thereof.
The following materials or Items are
hazardous wastes when they are dis-
carded or Intended to be discarded as
described In { 261.2(a)(2)(i), when they
are burned for purposes of energy re-
covery In lieu of their original Intend-
ed use, when they are used to produce
fuels In lieu of their original Intended
use, when they are applied to the land
In lieu of their original intended use,
or when they are contained In prod-
ucts that are applied to the land In
lieu of their original Intended use.
(a) Any commercial chemical prod-
uct, or manufacturing chemical inter-
mediate having the generic name
listed in paragraph (e) or (f) of this
section.
(b) Any off-specification commercial
chemical product or manufacturing
chemical intermediate which. If It met
specifications, would have the generic
name listed In paragraph (e) or (f) of
this section.
(c) Any container or Inner liner re-
moved from a container that has been
used to hold any commercial chemical
product or manufacturing chemical in-
termediate having the generic names
listed In paragraph (e) of this section.
or any container or inner liner re-
moved from a container that has been
used to hold any off-specification
chemical product and manufacturing
chemical Intermediate which, If It met
specifications, would have the generic
name listed In paragraph (e) of this
$261.33
section, unless the container Is empty
as defined in | 261.7(b)(3) of this chap-
ter.
(Comment- Unleu the residue Is being bene-
ficially used or reused, or legitimately recy-
cled or reclaimed: or being accumulated,
stored, transported or treated prior to such
use. re-use, recycling or reclamation, EPA
considers the residue to be Intended for dis-
card, and thus a hazardous waste. An exam-
ple of a legitimate re-use of the residue
would be where the residue remains In the
container and the container Is used to hold
the same commerlcal chemical product or
manufacturing chemical product or manu-
facturing chemical Intermediate It previous-
ly held. An example of the discard of the
residue would be where the drum Is sent to
a drum recondlttoner who reconditions the
drum but discards the residue.]
(d) Any residue or contaminated soil,
water or other debris resulting from
the cleanup of a spill Into or on any
land or water of any commercial
chemical product or manufacturing
chemical Intermediate having the ge-
neric name listed In paragraph (e) or
(f) of this section, or any residue or
contaminated soil, water or other
debris resulting from the cleanup of a
spill, into or on any land or water, of
any off-specification chemical product
and manufacturing chemical Interme-
diate which, If It met specifications,
would have the generic name listed In
paragraph (e) or (f) of this section.
[Comment- The phrase "commercial chemi-
cal product or manufacturing chemical In-
termediate having the generic name listed
In ..." refers to a chemical substance
which Is manufactured or formulated for
commercial or manufacturing use which
consists of the commercially pure grade of
the chemical, any technical grades of the
chemical that are produced or marketed,
and all formulations In which the chemical
Is the sole active ingredient. It does not
refer to a material, such as a manufacturing
process waste, that contains any of the sub-
stances listed In paragraphs (e) or (f).
Where a manufacturing process waste Is
deemed to be a hazardous waste because It
contains a substance listed In paragraphs (e)
or (f). such waste will be listed In either
II 261.31 or 261.32 or will be Identified as a
hazardous waste by the characteristics set
forth In Subpart C of this part.)
(e) The commercial chemical prod-
ucts, manufacturing chemical interme-
diates or off-specification commercial
chemical products or manufacturing
40 CM Ch. I (7-145 Edition)
chemical Intermediate* referred to In
paragraphs (a) through (d) of this sec-
tion, are Identified a* acute hazardous
wastes (H) and are subject to be the
small quantity exclusion defined in
I 261.6(e).
(Comment- For the convenience of the regu-
lated community the primary hazardous
properties of these materials have been Indi-
cated by the letters T (Toxlclty). and R (Re-
activity). Absence of a letter Indicates that
the compound only Is listed for acute toxlcl-
ty.)
These wastes and their correspond-
ing EPA Hazardous Waste Numbers
are:
I No.
P023
foot
POST
POSS
coot.
•*»»•
2-feofO-
Aodte MM. SUXO-. ndun Hit
acid. N-{(nM4-2-4Nour»«
Aldhn
Alyliloohal
Ammonun pKnu (R)
Animonium vanadMa
Anmc (HI) <**••
Ancric (V) end*
Aiwnfc
avwn cysnM*
, 4-flMfD*
4-I1-hydn>iy-2-
-------
Environmental Protection Agency
§ 261.33 § 2*1.33
40 CHt Ch. I (7-1-«5 SdhHon)
HUWOOM
MM* NO
POX _...
P031
POM
PO36
P037
POM
PO39
P040
PM3..._ _
P044
PO4S
P071
POBZ... —
PO47 _
P034. _..
P048
P020 „
PO85
PQ39
P04B
P1M
POM
POU
POS1 _
PO12
PO46
P10I
POM
POB7
pose
P057
pose
PO65
pose
POS1
PO37
P060...._
POM
poeo_ _.
POM
P1 16
POM
P083
P096
P064
P007
PO92
P085
P016
P112
P1 18 ....
post
POS6
P087
SutMUno*
CyiradM IK*** cyvnd* uta). not i
wMn«MC«Md
Cywngm
Ik^dm
CMhylaran*
O.O-Owttiyl S-t2-(«OV»X)»«h»() ptmpd
d«M»U
OMOpropyl fkioaxitvMpW*
OmthocU
3.3-Dim«hy*-Hm«fiynNo(-2-«>uUnon«.
O.O-Orrwthyl CVfMvtraplMnyt pho^h
IhKMlt
t.^Omm-ocnttf md MM
2.4-Orttrophral
DmoMb
DwMMon
2.44MNotmm
EndcMUlin
EfldOttMl
Endm
EprapMni
Elhy.«xo-
^ydfUra, fiMVi)4.
HyOrocyinic Kid
*••
oro-
O-
om-
•n-
Itocyinc Kid. nwffiyl nur
3(2H|-liouiolan<. S-4imnoiTMV)y<>-
Mwcixy. I«c«««o-O)p4wi»1-
Mcrcwy lulnwMI* (R,T)
Mrturx. or»tt»-3«.4.7.7*-Mlratiydn>-
M*0xxnyl
2-McffMuiridifW
Methyl ryoraw
UMnyl aHcyenala
2-MWiytoctor.We
•Ipht-Naphttiymiioura*
NBkal caitonrl
Nickel cyanide
Nickel|ll) cyanide
Nickel utrK*ft>ony<
Nicotine and aata
Nnropen dxmde
Nltrooenomafia.2J-d«nalhanol. 1,«.5.6.7.7-he«-
achtoro. cyckceulMa
Ooameftytpyiutjiiuephoramida
Oamun onda
Oamum latroad*
7-Oub«rcto[2^.1 )lMpUna-2.:
Phenol, 2-cydonaxyM.6-drt*o-
Phenol, 2.44kratiD-
Phenol. 2,4-dmliie-a^ietfiyt-
Pnenol. 2.4.8-*n»o-. ammonun un (R)
Phenyl dicnloioereni
N-PnwiyntwwM
Pnorau
Phoepnoric acid, dMtiyf p-rt»optieny( euer
PnoaphoreoWiioc acid. O.O-dmemyl S-C2-
(m«iyl«mno|-2-OK>ettiyl)eB«
Pnoepnorolluoric aod. tw(1-melhyta«ixl)-
Phoepftorottwic acid, O.O-dMhyl S-
(eViy»M»metriyl eater
Phoaphorotticci acid. O.Cntvn^ CMp-rt«o-
Phoephorolhloic abd. O.Oxtethyl O- pyraHnyl
Phoaphoraffiioe aod. O.O-dvnelhyl O-1HI*-
Plumturx.
PoUMwm cyvwto
PaUMum «*v»t cyinidt
PraMral. 2-m«ttiyt-2-)ci>t>ony<)aiin*
Prap«n«n«rii*
mnnrale- (R)
2'Propanona, Hnoflio-
Propargyl alcohol
2-Prapenal
2-Propan-l4l
1.2-Propylenimne
2-Piopyiv1 0.1% or taM
2-AMiyivnnolluaran*
AcMyt cMaridi (C.R.T)
•(2-eWo
•• L-
«no > CH«mnuc«r>»ooy1) oiy)m*B)yl]-
BentlclKridne
3.4-aenacrtdne
Benzal cNartde
U-Bcnonvnocn*
1 j-BmnMrrann*. 7.12-dlm«>iyt-
N.N -JtrmlX)! -«-ph»n
O.T)
1.8 0«iu»n«dic»itim»lc Kid inhydnd.
Kid. (lM(2-«ttiyl-
1^-a«iu«n»diMrbo«ytle add. dtanyl MUr
1^-8*rmn*dKaitoiiylie Kid. dMKyt nMr
B«i»iw. 1.4-dkrtoro-
BMOOT*. (dkM
BvnMiw. 1.3-dMocywiiKXMIhyl- (R.T)
^ cfDortd* (C.R)
0«n»»o«, 1.2.4,5-tofrMtto'O-
B*nno*. (MenianKMttiy1)-
-------
Environmental Protection Agoncy
§ 261.33
§261.33
40 CFR Ch. I (7-1-M EdHion)
WuwNo.
0234...
0021...
0202..
O120..
O022.
0022
O187..
0050 .
O065 .
O021..
1X173..
0081..
0085..
O024..
0027..
0244..
0028..
0246..
022S..
O030-
O128...
0172-.
0035-
OO31...
0158 _
0063.
0074 _
O031.
0136..
O238-
017*..
0177..
O218-
U087..
021S-
0156 _
0033.
O211-.
O033-
O034..
O03S-.
O036...
O026..
O037...
O038...
O041...
O042...
O044...
0046...
0047-.
O048...
OO48...
O032...
O050...
OOS1...
OOS2...
0052...
0053...
0055...
O246...
0187...
O056...
O057...
0130...
UOM.
O240...
O058...
Sutwunc*
Himdom
WuWNo
B««nn*. IJ,Wrin*o- (R,T)
. I.t
3.4-Bantopyrana
p-8ansoqunona
BvuotncMondt (C.R.T)
1.2-BauphanarHrnna
i. 3.3 -d«**orO-
i. S.S'-dmatttoxy-
3.3-o«iw(fly(.
Btt(2-Ca>ilorM|thovy) nwttiww
BaX2-ehloro»opro0yl) tHm
Biacarbainoyl)d»ullida
Bronx* cyanida
4-Bromophanyl pltanyl <
1.3-Bula<*«na. 1
1-Buunamna. N-outyt-N-rtwao-
bcnmw-
t-auunol(q
2-BuMnoni (I.T)
2-Buunant
2-Butaiwl
add. 4-CBia(2-cNoioMiyqa>rino]
n-6utyi afchcnol (t)
Cacodyic add
IH.T)
O.T)
Cvbamic add. a«iyl aatar
nwtti)4nim&-. Mnyf 4
i. N attiyl N r
N-niatfiyl NH*'
wtrtMtioyf craorkto, i
Cotonic lad. iMnJUnQ) uH
Cxtioiiochtondtc «cM. rnMiyt«
Cwton aiyfluond* (H.T)
Caiton minjiiuitu*
drDanyl «uortd» (B.T)
CNoral
r(lT)
4-Chkxo-nxrMol
>po«>i
viny1i0Mr
CNoromMriyl rnMhyl •«•
o-ChloraprMnol
QvyMO*
CrcoaoU
Cnwll
Cyinogwi bound*
1.4-Cycfc»M>adi«n«tio
CycJohuwM (I)
Cydorwunon* (I)
1.3-Cydopwrodry1) dnopfOpytltnoc«(t)«m«l»
O-OcMorobcn *n«
m-DictilorotwnnrM
p-DJCtilorobwmn*
3 J -OcMoiotKi
DcrHorodifluoromtthtnt
DcNoro rtprnnyl tfBNoroMhww
DicNoro d^rwnyl tncrHoroMWM
1.2-Oichtoro«ltiyH»«
UMM^'OAttiyl VtfMf
2.4-Oietiloroprnnul
2(V-OcMuruptwnol
2.4-Oicrik>ropr»»nu.y»
1 i3.4-O*OCTmlt)inlhnom
•Ipntjlplu-OniMhytwnzylriydropOTOiiid* (R)
Dnwthytoftwnoyl cNomto
1.1-Onwihylnydruin*
1 ^-OntMhylriydnzirw
2.4-Dmwlhylprwnol
Dmttiyl phth4KU
OnMlhyl iurliu
2.4-OntrotokMn«
2.6-OnilrotoltMn*
Dnvoctyl ptithaKU
1.4-OioniM
Opropyumni (I)
[VN-propylflilnwamin*
Ettwfwl (I)
Emwurnn*.
Etron*. 1,2--
1^-EmarwdiyttncaitwmodnhMc «od
EitutM. l.1,l.2.2.2-h.x«c«oTO-
Elrun*. 1.1'-[nwltiyl«n«bn(oiy)lbltl2-ctikin>-
Ettnn.nrtrt« (I. T)
Etlunt.l.V^nylm- (I)
EttwM. 1.1 -OJtytmU-otHoro-
Elhvw, p*nl»ctuoro-
0208.,
0208.,
0216.,
0247...
O227.,
O043.,
O042...
O076.,
O078.,
O210...
0173.,
UOM...
uoo*.
U112,
0113.,
0236.,
0038,.
0114...
O087,.
0077.,
0116.,
0116...
O117...
O076.,
0116,
0118,
0138,
0120..
0122,
0123,
0124,
0125.
0147..
0213,
0125..
0124-
0206..
012«.
0183.
0127-
0128.
0128.
0130-
U131,
O132.
0243.
0133-
0086.
0088.
0088.
0108,
0134..
0134.
0135.
OO86.
O138.
0116.
O137.
0138.
O140.
0141.
0142.
0143.
0144.
0146.
0146.
0128.
O147.
0148.
O148..
Subwnc*
. 1,1.1.2-latractHoro-
Emana. 1,1.2.2-tatiactiloro-
Elhanamoainda
Ethana. l.1.1.-*icrrloro-2.2-tM(P-ma1rK»y
ErXana. 1.1.2-rnchioro-
Elhana. crUoro-
Elhana. 2-eMoroa«Kny-
Elrwna. 1.1-dKMoiD-
Ethana, lrana-1 J-dcMoro-
Ethana. 1.1.2.2-MtaeNoro-
Etrnnoi. 2.2'HrmreauiiiniuHiia-
Enanona. 1-prianyl-
Elhanoyt cMonda (C.H.T)
EBiyl aoaiata (I)
EBV acrylala (I)
Eltiyl cafbamau (urathan)
Ethytonabtaldrihiocaroanc aod)
Etytana dibromida
Ettiytana dctilonda
EMana onto (I.T)
Elhytana VMuraa
Ethylaiharll)
Etriytidana deNortda
EdyUnathacrylala
(0
0160,
0151,
0162,
U092
O028.
O045..
O046,
0068..
0080..
O075-
0119..
0121..
0226-
O044,
0121..
0123..
O036..
O164...-
Fwric dmrwi
FluorantriKM
Forme aod (C,T)
Finn (I)
2-furanciftould*hydt
2.5^irand»xw
Fur«n. Mrahydro- (I)
Furhnl (I)
Furturan(l)
D-GtucopyranOM, 2-o»oiy-2(3-m«tn>t-3-r»-
•ouraUo)-
Guin«Jn«. N-nltro«o-N^n«l»ni6»(2-cMoio«n*i«)
M«nyl^» c«orid«
(I.T)
.(H.T)
KftMfayiigabiityl hMoiv (I)
Mdhyl rmlwcryM* (I.T)
U Milhyl If 1*11 N iiilnanuiaiHrtm
uli»u»i«i»
2-tMpt10-N4
373
374
-------
Environmental Pr*tacti*n Agency
9261.31
WMMNo.
U17l_
U1W.
U1S1-
uiss.
uocs.
U041
U1S2
U1S3
U1S4
HIM
SeeF027.
U1SS
U1M.
U101
O1TO
SeeROT.
Do
U1S7.
U14S.
UOS7_
U1M_
U180-
U1I1-
U1*2-
U1B4_
U110-
uoee.
U14t_
U171.
U027.
U193.
U002-
UOOT.
UOS4.
U243..
UOOB.
U1S2-
U113
U11S
0162
See ROT.
U1»4
UOB3
•U1M
U1S5
U17S
U191
U1S4
U1M-
U200-
U201-
U202.
U203-
U204_
U204.
pbendn
U018_
«Mn
e«i>llam>iollaliah>*o-,
OdranelLT)
PaniacnlanMhani
rtlrobi
Pemaonlotaphenol
U213 —
Phenol 2«-iiia
Phenol 2.4-dichlon>
Phenol 44*R>.
U220-
Pnenol 2.4.W1enlon>
1,10-(1J-i)henylene)oyrana
Phoephonc add. LMd aaR
PhoapnoraoWWe add, 0,0-**h»t., s-me4ny
Phoepnt
(")
U22«
2-Ptooin*
U22S«
1^-iepanamlne (IT)
1-PfOoanamlna, N iBUpfl (I)
IJ-Otromo-O-dHon
Propane. 2-n*t>- (Q
Prepane. 2J-o«y««2-ertoro-
1>Propane autene
1-Pnpanol 2.3-dtjnmo-. ehoaphala (3:1)
t-fTopaool. 2>rapena. 1.1J
2-PnpenenlMe
2-PrapmnlMa. Z-metiji- (IT)
2'f^opMnoBC acid (I)
2^roptnoBC acsd, atttyt aalaf (1)
U24B
2-PrapenoJc add. 2^ne1hyl-. nMhyl eater fl.T)
Propionlc add. 2-(2.4.6-»ichloropheno>f>-
n*ropylen*» O.T)
Propvtene acntoide
4.4-4Mbene«ol alpha^lphi'^ieSiyt.
SuNunc add, dtme»V eater
fitrffur phoephkle (A)
SuHw wMraoe (R,T)
2.4.6-T
1.1.1 J-TekacNonethane
I.IAJ-TeeaUamoelliane
TeliaUiluueUiyterie
TYuNiunm) cMorttto
(I.T)
Thkam
Toluene
Tok>
>iyl-.
koro o( 10% or I
Pyrtdne
»TrTioBna,
mino)
2-(U-n>-.
Pmptortc aad. 2-<2,4,5-trtc**>ropt>.no«yK
U2M 2,4.«-TikMoraphennl.
U231 2,4^-TrtcHorephenol.
U230 2,4>TikMaroptMna>yw>e«c Mid.
Ammax. I—RXPRZSKIITATIVX SAMFUKO
MITHOM
The methods and equipment used for
..tripling watte 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 to be representative of the waste.
Extremely viscous liquid—ASTM Standard
D140-70 Crushed or powdered material—
ASTM Standard D346-76 Soil or rock-like
material—ASTM Standard D420-69 SoU-
llke material—ASTM Standard D1453-66
Fly Ash-like material—ASTM Standard
D2234-76 [ASTM Standards are available
from ASTM. 1916 Race St.. Philadelphia,
PA 19103]
Containerized liquid waste*-"COLIWASA"
described In 'Test Methods for the Eval-
uation of Solid Waste. Physical/Chemical
40 CFK Ch. I (7-145 Edition)
Methods." • U.S. Environmental Protec-
tion Agency. Office of Solid Waste. Wash-
ington, D.C. 20460. (Copies may be ob-
tained from Solid Waste Information. V£.
Environmental Protection Agency. 26 W.
Bt. Clalr St.. Cincinnati. Ohio 452681
Liquid waste in pits, ponds, lagoons, and
similar reservoirs.—"Pond Sampler" de-
scribed in "Test Methods for the Evalua-
tion of Solid Waste. Physical/Chemical
Methods." •
This manual also contains additional in-
formation on application of these protocols.
ATTENDEE II—EP Toxicnr TEST
PEOCKDUUS
JL Extraction Procedure (£/>>
1. A representative sample of the waste to
be tested (minimum site 100 grams) shall be
obtained using the methods specified In Ap-
pendix I or any other method capable of
yielding a representative sample within the
meaning of Part 260. [For detailed guidance
on conducting the various aspects of the EP
see "Test Methods for the Evaluation of
Solid Waste. Physical/Chemical Methods"
(Incorporated by reference, see I 260.11).]
2. The sample shall be separated Into its
component liquid and solid phases using the
method described In "Separation Proce-
dure" below. If the solid residue » obtained
using this method totals less than 0.5% of
the original weight of the waste, the residue
can be discarded and the operator shall
treat the liquid phase as the extract and
proceed Immediately to Step 8.
I. The solid material obtained from the
Separation Procedure shall be evaluated for
Its particle sixe. If the solid material has a
surface area per gram of material equal to.
or greater than. S.I cm* or passes through a
9A mm (0.375 inch) standard sieve, the oper-
ator shall proceed to Step 4. If the surface
area Is smaller or the particle size larger
than specified above, the solid material
shall be prepared for extraction by crush-
Ing, cutting or grinding the material so that
k These methods are also described In
"Samplers and Sampling Procedures for
Hazardous Waste Streams," EPA 600/2-80-
018. January 1980.
•The percent solids Is determined by
drying the filter pad at 80*C until It reaches
constant weight and then calculating the
percent solids using the following equation:
Percent solids -
- Q»» •*•(*) o«p»d)
375
376
-------
Environmental Pratstctlon Afancy
It psssm through a 9.6 mm (0.975 Inch) sieve
or. If the material Is In a single piece, by
subjecting the material to the "Structural
Integrity Procedure" described below.
4. The tolld material obuined in Step I
•hall be welched and placed In an extractor
with 16 time* Its weight of delonised water.
Do not allow the material to dry prior to
weighing. For purposes of this test, an ac-
ceptable extractor li one which will Impart
sufficient agitation to the mixture to not
only prevent itratlfication of the (ample
and extraction fluid but also insure that all
•ample surfaces are continuously brought
Into contact with well mixed extraction
fluM.
6. After the Mild material and delontaed
water are placed In the extractor, the opera-
tor shall begin agitation and measure the
pH of the solution in the extractor. If the
pH Is greater than 6.0. the pH of the solu-
tion shall be decreased to 5.0 ± 0.2 by
adding 0.5 N acetic add. If the pH U equal
to or less than 6.0, no acetic add should be
added. The pH of the solution shall be mon-
itored, as described below, during the course
of the extraction and if the pH rises above
6.2. 0.5N acetic add shall be added to bring
the pH down to 6.0 ± 0.2. However, In no
event shall the aggngrate amount of add
added to the solution exceed 4 ml of add
per gram of solid. The mixture shall be agi-
tated for 24 hours and maintained at 20'-
40'C (68--104T) during this time. It ls rec-
ommended that the operator monitor and
adjust the pH during the course of the ex-
traction with a device such as the Type 46-A
pH Controller manufactured by Chemtrix.
Inc.. Hlllsboro. Oregon 97123 or its equiva-
lent, in conjunction with a metering pump
and reservoir of 0.6N acetic add. If such a
system Is not available, the following
manual procedure shall be employed:
(a) A pH meter shall be calibrated In ac-
cordance with the manufacturer's specifica-
tions.
(b) The pH of the solution shall be
checked and. If necessary, 0.6N acetic add
shall be manually added to the extractor
until the pH reaches 5.0 ± 0.2. The pH of
the solution shall be adjusted at 16. 30 and
80' minute intervals, moving to the next
longer Interval If the pB does not have to be
adjusted more than 0.6N pH units.
(c) The adjustment procedure shall be
continued for at least 6 noun.
(d) If at the end of the 24-hour extraction
period, the pH of the solution Is not below
5.2 and the maximum amount of acid (4 ml
per gram of solids) has not been added, the
pH shall be adjusted to 5.0 ± 0.2 and the ex-
traction continued for an additional four
hours, during which the pH shall be adjust-
ed at one hour Intervals.
8. At the end of the 24 hour extraction
period, delonlzed water shall be added to
Part 261, App. II
the extractor In an amount determined by
the following equation:
V-(20XW)-16-A
V-ml detonised water to be added
W-weight in grams of Mild charged to ex-
tractor
A-ml of 0.6N acetic add added during ex-
traction
7. The material in the extractor shall be
separated into its component liquid and
Mild phases as described under "Separation
Procedure."
8. The liquids resulting from Steps 2 and 7
shall be combined. This combined liquid (or
the waste Itself If it has leas than M percent
solid*, as noted In step 2) Is the extract and
shall be analyzed for the presence of any of
the contaminants specified in Table I of
1281.24 using the Analytical Procedures
designated below.
Separation Procedure
Equipment: A filter holder, designed for
filtration media having a nominal pore sice
of 0.45 micrometers and capable of applying
a 6.3 kg/cm* (75 pel) hydrostatic pressure to
the solution being filtered, shall be used.
For mixtures containing nonabsorptlve
solid*, where separation can be effected
without <"T*"-<"g a 5.3 kg/cm' pressure dif-
ferential, vacuum filters employing a 0.46
micrometers filter media can be used. (For
further guidance on filtration equipment or
procedures see "Test Methods for Evaluat-
ing Solid Waste. Physical/Chemical Meth-
ods" incorporated by reference, see
I 260.11). Procedure:*
(I) Following manufacturer's directions,
the filter unit shall be assembled with a
filter bed consisting of a 0.45 micrometer
filter membrane. For difficult or slow to
filter mixtures a prefilter bed consisting of
the following prefllters in increasing pore
size (0.65 micrometer membrane, fine glass
'This procedure Is Intended to result In
separation of the "free" liquid portion of
the waste from any solid matter having a
particle size >0.45 pm. If the sample will
not filter, various other separation tech-
niques can be used to aid In the filtration.
As described above, pressure filtration Is
employed to speed up the filtration process.
This does not alter the nature of the separa-
tion. If liquid does not separate during fil-
tration, the waste can be centrlfuged. If sep-
aration occurs during centiifugatlon, the
liquid portion (centrlfugate) Is filtered
through the 0.45 pm filter prior to becoming
mixed with the liquid portion of the waste
obtained from the Initial filtration. Any ma-
terial that will not pass through the filter
after centrifugatlon Is considered a solid
and Is extracted.
Part 261, App. II
fiber prefilter. and coarse glass fiber pre-
filter) can be used.
(U) The waste shall be poured Into the ni-
tration unit.
(ill) The reservoir shall be slowly pressur-
ized until liquid begins to flow from the fil-
trate outlet at which point the pressure In
the filter shall be Immediately lowered to
10-16 pslg. Filtration shall be continued
until liquid now ceases.
(Iv) The pressure shall be Increased step-
wise In 10 psl Increments to 76 pslg and fil-
tration continued until now ceases or the
pressurizing gas begins to exit from the fil-
trate outlet.
(v) The filter unit shall be depressurtced.
the Mild material removed and weighed and
then transferred to the extraction appara-
tus, or. in the case of final filtration prior to
analysis, discarded. Do not allow the materi-
al retained on the filter pad to dry prior to
weighing.
(vl) The liquid phase shall be stored at 4'C
for subsequent use In Step 8.
B. Structural Integrity Procedure
Equipment: A Structural Integrity Tester
having a 3.18 cm (1.26 In.) diameter hammer
weighing 0.33 kg (0.73 IDS.) and having a
free fall of 16.24 cm (6 In.) shall be used.
This device is available from Associated
Design and Manufacturing Company, Alex-
andria, VA 22314, as Part No. 125. or It may
be fabricated to meet the specifications
shown In Figure L
40 C« Ch. I (T-1-S3
Procedure
1. The sample holder shall be filled with
the material to be tested. If the sample of
waste Is a large monolithic block, a portion
shall be cut from the block having the di-
mensions of a 34 cm (1.3 In.) diameter x 7.1
cm (2.8 In.) cylinder. For a fixated waste.
samples may be cast In the form of a 3.3 cm
(14 In.) diameter x 7.1 cm (2.8 In.) cylinder
for purposes of conducting this test. In such
casts, the waste may be allowed to cure for
30 days prior to further testing.
2. The sample holder shall be placed into
the Structural Integrity Tester, then the
hammer shall be raised to Its maximum
height and dropped. This shall be repeated
fifteen tunes.
3. The material shall be removed from the
•ample holder, weighed, and transferred to
the extraction apparatus for extraction.
Analytical Procedure* for Analysing Extract
Contaminant!
The test methods for analyzing the ex-
tract are as follows:
I. For arsenic, barium, cadmium, chromi-
um, lead, mercury, selenium, silver, endrin.
llndane. methoxychlor, toxaphene, 2,4-
D(2,4-dlchlorophenoxyacetic addl or 2.4.5-
TP [2.4.5-trtehlorophenoxyproplonlc add):
"Test Methods for the Evaluation of Solid
Waste, Physical/Chemical Methods" (Incor-
porated by reference, see 1260.11).
2. [Reserved]
For all analyses, the methods of standard
addition *h«n bg used for qinntlflratlftn of
spedes concentration.
377
378
-------
Environmental Protection Agency
Part 261, App. II
O-i
1525cm
COMBINED
• WEIGHT
33Kg
I 73101
(3 IScml
11.25"!
J
•SAMPLE
ELASTOMERIC*
SAMPLE HOLDER
*ELASTOMERIC SAMPLE HOLDER FABRICATED OF
MATERIAL FIRM ENOUGH TO SUPPORT THE SAMPLE
Figure 1
COMPACTION TESTER
[45 PR 33119. May 19. 1980. « amended at 46 FR 35247. July 7. 19B11
379
Port 261, App. Ill
APPENDIX III—CHEMICAL ANALYSIS
TEST METHODS
Tables 1. 2. and 3 apeclfy the appropriate
analytical procedure*, described In "Teat
Methods (or Evaluating Solid Waite. Phyal-
cal/Chemlca) Method*." (Incorporated by
reference, aee I 260.11) which shall be lued
to determine whether a sample contains a
given Appendix VII or VIII toxic constitu-
ent.
Table 1 Identifies each Appendix VII or
VIII organic constituent along with the ap-
proved measurement method. Table 2 Iden-
tities the corresponding methods (or inor-
ganic apeclea. Table 3 summarizes the con-
tents of 8W-S4B and supplies specific sec-
tion and method numbers for sampling and
analysis methods.
Prior to final sampling and analysis
method selection the analyst should consult
the specific aectlon or method described In
SW-846 for additional guidance on which of
the approved methods should be employed
for a specific sample analysis altuatlon.
TABLE 1—ANALYSIS METHODS FOR ORGANIC
CHEMICALS CONTAINED IN SW-846
Compound
Ac'fl'i'"
BaVtMM
IUft»<^x-*O«yirj+
Cutann ib.Mrt.
CNordane _ _.
CNonattd Uphwiyta
Chtorimtid d*>*ruo-
look)
TricNoiani
VkMM»
X»tw,_
•.01. (412.
a 12. us
•4)1. 174
•.01. U4
(.40. ITS
•.12, *TS
•4M. 875
8.09. 875
8.04, 875
8 09. 875
(.OS. US
•4)1. 802.
874
•4)1. (74
a.oa. ITS
8.06. STS
8 12. 876
• 12, 875
•.12. ITS
8.12. US
•.0*. US
•.08. ITS
•4)1. 874
•32
•4)1. 84)2.
874
•4)1. 802.
874
HO. 87S
8 06, 8.M.
875
8.08. 875
•.04, ITS
8.01. 874
8.04, 875
84M. STS
•4W, 8.08.
•.OS. 8.08.
875
8 08, 8.09.
•.OS, 8.08.
875
8.12. 8TS
8.01. 874
8.01, 874
8.04. U4
8.02. 874
8.08. 875
8.08. 87S
8.01, 874
8.01. 874
8.01, 174
8.04. 875
•.40, STS
•.01. I
•.01, 874
•.01. 874
•.02. 874
M10. 8120.
8290
M10. 8240
M10. 8240
8150. 8290
8120. 8250
8040. 8250
•090. 8250
8040. 8290
MM, B2SO
aoao! 82M
MIS. 8240
MIS. 8240
8290
SOM. 8290
8120. 82M
8120, 8290
M10. 8240
8120.8250
MM. 8260
•290
M10. 8240
8250
MIS, 1240
MIS, (240
•100. 8260
MM. 8260
MM. 82SO
•040, 1240
M1S. 8240
8040. 8290
•040. 8290
•140
•140
MM. KM
MM, 8250
8090, 8290
8120. 8250
MtO. 8240
M10. 8240
8040. 8260
•020. M24
8250
8290
80M. 8250
M10. 8240
M10, 8240
M10. 8240
•040. 8290
•190. 8250
M10. 8240
M10. 8240
MtO. 8240
8020. 8240
380
-------
Environmental Protection Agency
>Anafcna tor |Hiaiia»e»ana and oarbanto: I «waa •
praurK k> a raao banman 1.4:1 and 5:1 enoaota ahouU I
Port 261, App. Ill
TABLE 2—ANALYSIS METHODS FOR INORGANIC
CHEMICALS CONTAINED IN SW-646—Conttn-
•ort Ml, App. Ill 40 C« Ch. I (7-1-.S ioltion)
TABLE 3—SAM-UNO AND ANALYSIS METHODS CONTAINED m SW-*46—Continued
TABLE 2—ANALYSIS METHODS FOR INORGANIC
CHEMICALS CONTAINED m SW-M6
CompoiKd
Compound
Anarac.
CrnmUKl
matrnoXa)
9.M
9.51
1.52
9.93
9*1
9A45. 9.54C.
Saeond
7040,7041
TOM. 7061
TOM, 7091
TOM. 7091
71M. 7191
7196, 7196.
Uarouy-
Total Organic Hatogan
mavwdO)
1.647
9.56
9.57
»M
9.M
9.M
9.55
9.M
9.97
7197
7420, 7421
T4TO. 7471
7620. 7521
7740. 7741
77M. 7791
M10
•020
9030
TABLE 3—SAMPLING AND ANALYSIS METHODS CONTAINED IN SW-846
TW.
tencting of Sold WM*M
j>M»tapm«iH of App«opf»te famptng Ram ,.,,
FuTVaWittntAl BtttMtiCtV Conotpti
Diwr ptitrtral Rmv^M
S«TVrn« RiWwtom S*vnptk>o
Smitftod Rwmm Swrc>1'V)
&y*namtr nwrt?fn fivv^^X)
Conipo«to 6tMt^nO
fit*Mmp*«ig , ,
Cott md Lou Fww*^^
WMQM^ Bo***.
Pn^
ThM
Trt»
AJ^M
ffatortk^i «J Sangria rVwtfMnov*.
DocuiTBBtititaon o( CVMin ol CuMody ™ _-_ .
Sanytoj LAtMto. — ~ - —
Sarrtpto G*Mli
Fialfj tog Boo*
ChtMrxHOmodv ^tf^ftl
Svnpta AnvJyw FtequMt ShMt
R«c**pi and LoognQ of C >mpi< ~
SeUfltih CtOiWtf-Ciap Method
FMa
Saekon
No.
1.0
1.0
1J>-2
1 0-7
1.0-7
10-7
3.2 1
377
37J
37.4
375
37.6
37,7
3.3
33
2.0
2.0-1
20-3
2.0-5
2.0-e
2.0-A
20-10
20-10
20-12
2.0-13
30
38-2
3.2-2
3.2-2
37-2
4.0
4 1
4.1
SO
5.3
9.0
7.0
dMon
Maowd
No.
"
Saoond
Saekon
No.
1.0
1.1
111
1.1.47
1 1 4 .3
17
1717
17 U
171 4
171 6
17.1.6
1717
177
17.3
1.3
1.3.1
1.3.2
1.3.3
1.3.4
13.S
1.3.6
1.3.7
1.3.6
1.3.9
1 4
1.4.1
1.47
1.4.3
14.4
2.0
2.1
2.1.1
2.1.1
21.1
2.17
2.12
2.1.3
2.1.4
adMon
Uamod
No.
—
1010
1020
1110
Ta*
E»ae*n Proo-ur. Teft* T«t
lriotv.wteT.Khn.quat..-.. .--- — •
"***• i,™ _ ..-
Ouok/ton Prooadura tor OH. Qraaaa or Wan
Saparaury Fumal UqwMJquU Extraction
Conttnuoua Uquld-UquhJ Extraction ,, _ - ...,.,.-
Haaflanana
Antimony. Ftama AAS
Araanic, Flama AAS -,..,.„,,,,-., ,,,„.„,-- , -
ytraanlf Fumac* AAS ... . • .•<
Barium Ramt AAS r ,
Cadrrium. Fumaet AA*
Chromum Furnana AAS . .
Laad Flamt AAS
LaarJ Furtrr AAS ,.., ,
Marcury CoM Vapor liquid
Mwruy CoM V«m S&M , ,, ,
taokal Ftamp A, A$
NMial Fumaot AA8
Saiw, Fum»e» AAS
Organte Analytical Mtthnoa ,,
Kmm CrMonatuuiaplaL MaBmH
Hatonanatad Votatta Organlra
AcroWn AcrytonlMa Aoatonittaa
Pim-ut. ft-*
Oroanochlonna Paattddaa and PCS.
Organaphoaphonja raatictdai
OC/MS Volattlaa
QC/MS Saml-Volat»aa, Packad Column
QC/MS Saml-VolatlMa. CapWary
Analym of CrUomatad Duma and Obantolurana .
Potrnudaar Aromatic Hydnxartxma
MlacalUnanm An^ytcml Mattioda
Cyanida: Total and AmanaMa to CNortnaaori..,
Total Omanic Hatooan fTOX).
SuHUM ' "
pM Maamamanl
•acwn
No.
7.1. 7 A 74
74
•.49
.1
1
•.49-9
9.49-«
•.0
9.0
»JO
»JO
9.0
•.0
' 9.0
1.0
(.0
IJ)
•.0
•.0
•.0
•.0
IJ)
9.0
90
9J)
9.0
ta
CO
9.0
IX)
1.0
• 0
• 0
9.0
1.0
9.0
•J)
90
• 0
•A
9.0
1.0
9.0
1.0
90
9.0
• 0
1.0
90
10
idWon
UatHod
No.
~tM»
9.1
9.01
• 94.
•JM
9.96
•.92
•.M
(.60
(.51
. 62
9.52
1.53
1-54
1.54
1,540
• 547
1.46
1.56
U7
157
-__
159
9.M
9.M
1.04
1.06
1.01
•.09
9.40
974
• 10
K>
•acend
SacHm
No.
21.4
4.0
4.1
4.1
4.1
4.1
4.1
47
47
4_2
47
47
5.0
5.0
5.0
7.0
7.0
74
7.0
7.0
70
7.0
7.0
7.0
7.0
7.0
7.0
70
7.0
70
7.0
7.0
70
70
70
7.0
7.0
90
|1
0 i
1.1
1.1
1.1
10
on
No
1310
3010
3020
3030
30M
3510
3520
3530
3540
3550
5020
5030
7470
7471
TOM
T061
TOM
7091
7130
7131
TOM
7191
7195
7196
7197
7420
7421
7470
7471
7520
7521
7740
7741
77M
mi
9040
90M
MM
MM
91M
6240
•250
62M
381
382
-------
Prot*cH*n Agency Fart 261. App. VII
TABLE 3—SAMPLING, AND ANALYSIS METHODS CONTAINED m SW-846—Continued
Part 261, App. VII
40 CF« Ch. I (7-l-*5 EaHton)
Mmdu
No.
10.0
104)
10.0
104
10.0
10.0
No.
EPA
heunl-
No.
10.1
10.1
10.1
10J
lOJ
No.
•024.
•See apedflc met*L
148 PR 18281. Apr. 8.1983, M amended at M PR 2000. Jan. 14.1986)
DAW NOTE At 50 PR 3000, JUL
14. 1986, Put Ml. App. TJI wu amended M
followi: In Table 1. the entry (or "Chlorin-
ated dlbensodloxlni" wai removed, and the
entrie* for "Chlorinated dlbenzo-p-dloxlna.
and "Chlorinated dlbenzof urani" were added.
In Table 3. the entry for "AnalyBii of Chlor-
inated Diozini and Dlbensofurani" wai
added under "Organic Analytical Method*—
Oat ChromatoKTaphic/Maai Spectroicopy
Method! (DC/MS)" after the entry "OCX
MS Seml-VolatUet, Capillary". Thete
amendments are effective July 16.19S6. For
the convenience of the uaer, the luperaeded
entry from Table 1 U *et out below:
TABLE 1—ANALYTICAL METHODS FOR ORGANIC
CHEMICALS CONTAINED m SYV-846
Arrofonc VII—BASIS FOB LISTING
HAZARDOUS WASTE
Compound
Fnt
edNon
mettodla) methodta)
CNooneleddtieiiiDdiuiana..
. M*. US MM. 1250
APPENDIX IV—[RESERVED FOR
RADIOACTIVE WASTE TEST METHODS]
APPENDIX V— [RESERVED FOR INFEC-
TIOUS WASTE TREATMENT SPECIFICA-
TIONS]
APPENDIX VI—[RESERVED FOR
ETIOLOOIC AGENTS]
POOL
FOW-
FOM_
F004_
F006-
FOO»_
F007_
F008-
F00»..
F010-
F011_
F012..
F019..
F020..
FOZ1..
F022
F023..
Hazardoua eoneMuenia tor oNoh
V1.1->tchlc»o«l)iena,
itonnBvBd ftuofOCMtooflB.
fi)Mnt, nMttiytanc ct«onbs.
FOM.
FOZ7.
FOM —
K001-
NA
kMora. carton
toobuttnol, pynArw.
duonturu floni,
Cywiidi (Mtt«).
Cymnid* (ula).
CyinfcM (»tt»).
Cymnb. (MM).
Cyvnkto (camptoitd)
Heuvctani chromun, cyi
Xurane; M- and
leiiachloiutihenoia and ttwr chtorophenoiy de-
pt»nol wd to dwiviM*.
p«iUcNo>o-
Ten-, and penuohlonxtt»nio-^d0m. tm-
•nd pexleciilonxtti*n>oturan»; >v and Mra-
ttitm uphenoli and mav cnlofophenoxy danva-
feva aoda, avtan. ethera, amna and olhat aalti.
K010-
K011.
K01S.
K014.
K01t_
K016.
K01T.
KOH_
K01t-
coneMuanla for when haled
Chtoromethane. OcMoromeihana,
ana. cartoon MacNortda. dHoroethytena. 1.1-
oKMoroefhana, U-djentoroethane. nna-l-t-
UVIiluiuelhylene, 1,1-dKhtoroetnytaoa, 1,1,1-
MoNoroelhana, t.U-Mchloroamna, Mentor-
otnAiM, l.1,U-ana. oeniena. cNatieraena. drcn-
nna. Wuena. iietinaialana.
Ten-, penu-, and nenacntororjbenio p dk)«jni. le-
n-. penta-, and haiaehlonxtbeniohvana.
Ten-, penta-. and henchkxodioenio^diorina: la-
n- Dent*-, end heuehloroditaeniorinna: kV.
len-. and penlacMorophenoU end their cMoro-
phenoiy derivakve acxta. edert, ethera, emne
and other aalla.
Ten-, pema-, and heKechlcndrbenio^-dioilna: le-
ka-, penta-, end heiachlorodlbenio
-------
Environmental Protection Agency
1.1 J vqtamttmm, t.1.1 J tt»mMut^»m\»,
MM - 1 1,l-aaNaiw*im. 1.1.1
(46 FR 4419. Jan. 16.1981. u amended at 46
TO 17477. May 30. 1981; 49 FR 5313. Feb.
10.1984; 60 FR 3000. Jan. 14, 1985]
Emcrrvc DATS NOTE At 50 FR 3000, Jan.
14. 1985. Put 361, App. Vn was amended by
adding the entrle* tor F030 through P023.
and F036 through F038. effective July 16.
1985.
Aimnnx VIH— HAZARDOUS
Acetonltrfle (Ethanerutrfle)
Acetopnenone (Ethanone. 1-phenyl)
3Xalpha-Acetonylbenzyl>-4-
hydroxycoumaiin and salts (Warfarin)
3-Aeetylaminofluorene (Acetamlde. N-(BH-
fluoren-3-yl)-)
Acetyl chloride (Ethanoyl chloride)
l-Acetyl-3-thiourea (Aoetamlde. N-
6-Amino-l.la.2.8,8a,8b-hexahydro-8-
( hydro Jtymethyl >-8»-methoxy-5-methyl-
carbamate azlrinot2'.3':3.4]pyrrolo(1.2-
allndole-4.7-dlone, (ester) (Mltomycln C)
(AElrlno[2'3<:3,4)pyrrolo(l,2-a)lndole-4.7-
dlone. 6-amino-B-[((amtno-
carbonyl)oxy>methylM.la,2.8.8a,8b-
hexahydro-8amethoxy-S-methy-)
6-(Amlnoinethyl>-3-lBOxazolol (3(3H)-Isoxa-
rolone, Mamlnomethyl)-) 4-Aminopyrt-
dlne (4-Pyrldinamine)
Amltrole (lH-1.2.4-Trlazol-3-amlne)
Port 261, App. VIM
Aniline (Benaenamine)
Antimony and compoundi. V.OJB.'
Aramlte (Bulfuroui acid. 3-chloroethyl-. 1-
C4-( l.l-dlmethylethyl)phenoxy)-l-
methylethyl ecter)
Anenlc and compoundi, V.OM.'
Arsenic acid (Orthoarsenic add)
Arsenic pentoxlde (Arsenic (V) oxide)
Anenlc trioxlde (Arsenic (III) oxide)
Auramine (Benzenanune. 4.4'-
carbonlmldoylbls[N,N-Dlmethyl-. mono-
hydrochloride)
Azaserine (L-6erlne, dlaaoacetate (ester))
Barium and compounds. N.OJB.*
Barium cyanide
Benzlclacrldlne (3.4-Benzacrldlne)
Benclalanthracene (1.3-Benuinthracene)
Benzene (Cyclohexatrlene)
Benzenearsonlc add (Arsonlc acid, phenyl-)
Benzene, dlchloromethyl- (Benzal chloride)
Bencenethiol (Thlophenol)
Benzidlne (tl,r-Biphenyn-4.4'dUmlne)
Bencolblfluoranthene (3,3-Benzof)uoranth-
ene)
BensotJIOuoranthene (7,8-Benzonuoranth-
ene)
Beazotalpyrene (3,4-Benzopyrene)
p-Benzoqulnone (1.4-Cydohexadlenedtone)
Benzotrichloride (Benzene, trichloromethyl-
)
Benzyl chloride (Benzene, (chloromethyl)-)
Beryllium and compounds, Jt.OS.*
Bl*(3-chloroetboxy>methane (Ethane. 1.1'-
[methylenebis(oxy»bls[2-chloro-])
Bls(3-chloroethyl) ether (Ethane. 1.1'-
oxyblsI3-chloro-))
NJf-Bls(3-ch]oroethyl>-2-naphthylamlne
(Chlomaphazlne)
Bls(3-chlorolsopropyl) ether (Propane. 2.3'-
oxy bist S-chloro- ])
Bls(chloromethyl) ether (Methane.
oxyblitchloro-})
Bls(2-ethylhexyl) phthalaU (1.2-Benzenedl-
carboxyllc acid. blB(3-ethylhexyl> ester)
Bromoacetone (2-Propuione, 1-bromo-)
Bromomethane (Methyl bromide)
4-Bromophenyl phenyl ether (Benzene, 1-
bromo-4-phenoxy-)
Bruclne (8trychnldln-10-one. 2.3-dlmethoxy-
)
3-Butanone peroxide (Methyl ethyl ketone.
peroxide)
Butyl benzyl phthalate (1,2-Benzenedlcar-
boxyllc acid, butyl phenylmethyl ester)
2-sec-Butyl-4.6-dinltrophenol (DNBP)
(Phenol, 2.4-dlnltro-6-(l-methylpropyl)-)
Cadmium and compounds, N.O.S.*
Calcium chromate (Chromic acid, calcium
salt)
Calcium cyanide
'The abbreviation N.O.S. (not otherwise
specified) signifies those members of the
general class not specifically listed by name
In this appendix.
Port 261, App. VIII
Carbon dlsulflde (Carbon bisulfide)
Carbon oxyfluorlde (Carbonyl fluoride)
Chloral (Acetaldehyde. trichloro-)
ChlorambucU (Butanolc acid, 4-Cbls<2-
chloroethyDamlnolbenzene-)
Chlordane (alpha and gamma Isomers) (4,7-
Methanolndan. 1.3.4,5.6.7,8.8-ocUchloro-
3.4.7.7a-tetrahydro-> (alpha and gamma
Isomers)
Chlorinated benzenes. N.OJB.*
Chlorinated ethane. N.O A'
Chlorinated nuorocarbons. N.OJB.'
Chlorinated naphthalene, N.O.8.*
Chlorinated phenol, N.O J.'
Chloroacetaldehyde (Acetaldehyde. chloro-)
Chloroalkyl ethers. N.OJB.*
p-ChloroanlUne (Benzenamlne. 4-chloro-)
Chlorobeniene (Benzene, chloro-)
CnlorobenzUate (Benzeneacetlc add, 4-
chloro-alpha-(4-chlorophenyl>-alpha-
hydroxy-, ethyl ester)
3-Chloro-l, 3-butadlene (chloroprene)
p-Chloro-m-cresol (Phenol, 4-chloro-3-
methyl)
l-Chloro-3.3-epoxypropane (Oxlrane. 3-
(chloromethyl)-)
3-Chloroethyl vinyl ether (Ethane, (2-chlor-
oethoxy)-)
Chloroform (Methane, trichloro-)
Chloromethane (Methyl chloride)
Chloromethyl methyl ether (Methane.
chloromethoxy-)
3-Chloronaphthalene (Naphthalene, beta-
chloro-)
3-Chlorophenol (Phenol, o-chloro-)
l-(o-Chlorophenyl)thiourea (Thlourea, (3-
chlorophenyl)-)
3-Chloropropene (allyl chloride)
3-Chloroproplonltrne (PropanenltrUe, »-
chloro-)
Chromium and compounds. N.O^.*
Chrysene (1,3-Bensphenanthrene)
Citrus red No. 3 (3-Naphthol, l-t(X»-
dlmethoxyphenyl)azo)-)
Coal tars
Copper cyanide
Creosote (Creosote, wood)
Cresols (Cresyllc add) (Phenol, methyl-)
Crotonaldehyde (3-Butenal)
Cyanides (soluble salts and complexes).
N.0.8.'
Cyanogen (EthanedlnltrQe)
Cyanogen bromide (Bromine cyanide)
Cyanogen chloride (Chlorine cyanide)
Cycasin (beta-D-Olucopyranoalde. (methyl-
ONN-azoxyhnethyl-)
3-Cydohexyl-4.6-dlnltrophenol (Phenol, 3-
cyclohexyl-4,6-dlnltro-)
Cyclophosphamide (2H-l,3.3,-Oxazaphos-
phorine, [bli(2-chloroeUiyl)amlno)-tetra-
hydro-. 2-oxide)
Daunomydn (5.13-Naphthacenedlone. (88-
cts)-8-acetyMO-[(3-amlno-3.3.6-trideoxy)-
alpha-L-lyxo-hexopyranosyl)oxy)-7,8.B.10-
tetrahydro-6,8,ll-trihydroxy-l-methoxy-)
40 Cnt Ch. I (7.145 MHton)
DDO (Dtehlorodiphenyldlchloroethane)
(Ethane. l,l-dlchk>ro-2.2-bl»
Dlbens[a.hlanthracene (U.t.6-DIbenzanth-
racene)
7H-Dibenao[fM)carbaiole (3.44.6-Dlbenscar.
bazole)
Dlbenao(a,«)pyrene (1.3.4>Dlbenapyrene)
Dlbenio(a.hlpyrene (l.U.t-Dlbenzpyrene)
Dlbenzo[aJ)pyrene (1,3.7.8-Dtbenzpyrene)
1.3-Dibromo-3-chloropropane (Propane. 1.3-
dlbromo-*-chloro-)
1,3-Dtbromoethane (Ethylene dlbromlde)
Dibromomethane (Methylene bromide)
Dl-n-butyl phthalate (U-Benzenedlcarbox-
yllc add, dlbutyl ester)
o-Dlchlorobencene (Benzene. 1.2-dlchloro-)
m-Dlchlorobenzene (Benzene. l.J-dlchloro-)
p-Dichlorobenzene (Benzene. 1,4-dlchloro-)
Didilorobenzene. N.OJS.* (Benzene.
dlchloro-. N.OA*)
l,3'-Dlchlorobenzldlne ((l.r-Blphenyll-4.4'-
dlamlne. 34'-dlchloro->
1.4-Dlchloro-3-butene (3-Butene, 1.4-dlch-
loro->
Dlchlorodinuoromethane (Methane, dlch-
lorodlfluoro-)
1.1-Dlchloroethane (Ethylldene dlchloride)
1,2-Dichloroethane (Ethylene dlchloride)
trans-l^-Dichloroethene (U-Dichloroethy-
lene)
Dlchloroethylene. N.OB.* (Ethene, dich-
loro-. N.O.8.*)
1.1-Dichloroethylene (Ethene, 1.1-dichloro-)
Dichloromethane (Methylene chloride)
3.4-Dlchlorophenol (Phenol. 3,4-dlchloro-)
3.6-Dlchlorophenol (Phenol. 3.6-dlchtoro-)
2,4-Dlchlorophenoxyaoetlc add (3,4-D), salts
and eaten (Acetic add, 2.4-dlchlorophen-
oxy-, salts and eaters)
Dlchlorophe&yUntne (Phenyl dlchloroar-
slne)
Dichloropropane, N.OB.* (Propane, dlch-
loro-. N.OB.*)
1.2-Dlchloropropane (Propylene dlchloride)
Dlchloropropanol, N.OB* (Propanol, dlch-
loro-. N.OB.*)
Dlchloropropene. N.OB.* (Propene. dlch-
loro-. N.OB.*)
1.3-Dlchloropropene (1-Propene. 1.3-dlch-
loro-)
Dleldrin (1.3.3.4,10.10.hexachloro4.7-epoxy-
1.4.4a.6,6,7.8.8a-octa-hydro-endo,exo-
1,4:6.8-Dimethanonaphthalene)
l.*c3.4'Dlepoxybutane (2.2'-Bioxirane)
Dlethylanlne (Andne, dlethyl-)
385
386
-------
Environmental Protection Agency
NJI-Dtethylhydradne (Hydnudne, 1.2-
dlethyl)
O.O-Diethyl 8-methyl ester of phosphoro-
dlthlole Mid (Phosphorodlthiolc acid.
O.O-dlethyl 8-methyl eater
O.O-Dlethylphosphoric add. O-p-nltro-
pbenyl ectcr (Phosphoric add. diethyl p-
nltropbenyl ester)
Diethyl phthalate (1.3-Benzenedlcarboxyllc
add. diethyl eiter)
O.O-Dlethyl O-2-pyradnyl phoaphoroth-
loate (Phosphorothlolc add, O.O-dlethyl
O-pyrazlnyl eater
Diethylstllbesterol u^'-Stilbenedlol.
alphajOpha-dlethyl. bla(dlhydrogen phos-
phate. ->
Dthydroaairole (Bencene. 1,2-methylene-
dlozy-4-propyl-)
J.4-Dihydroxy-alpha--2-oxoethyn
erter
LS'-Dlmethoxybenzidlne (Cl.l'-BlphenyU-
4.4'dlamlne. 3-3'-dlmethoxy-)
p-Dimethylamlnoazobenzene (Benzenamlne,
N.N-dlmethyl-4-(phenylazo>-)
7.12-Dlmethylbenz[a)anthracene (1.2-Ben-
zanthracene. 7.12-dlmethyl-)
3.3'-Dimethylbenzldine ([1.1-Blphenyl]-4.4-
dlamlne. 3.3'-dimethyl-)
Dlmethylcarbamoyl chloride (Carbamoyl
chloride, dimethyl-)
1.1-Dimethylhydnztne (Hydracine. Li-di-
methyl-)
1.2-Dlmethylhydratlne (Hydracine. 1.2-dl-
metbyl-)
S.3-Dlmethyl-l-(methylthlo)-2-butanone. O-
[(methylamlno) carbonyDoxlme (Thlo-
fanox)
alpha^lpha-Dlmethylphenethylamlne (Eth-
anamlne. l.l-dlmethyl-2-phenyl-)
2.4-Dimethylphenol (Phenol. 2.4-dimethyl-)
Dimethyl phthalate (1.2-Benzenedicarboxy-
llc add. dimethyl eater)
Dimethyl aulfate (SuUuric acid, dimethyl
eiter)
Dlnitrobenzene. N.O.S.* (Benzene, dlnltro-.
N.O.8.')
4,6-Dlnltro-o-cresol and talU (Phenol. 2,4-
dlnltro-6-methyl-, and aalta)
2.4-Dlnltrophenol (Phenol. 2,4-dlnltro-)
2.4-Dlnltrotoluene (Benzene, l-methyl-2,4-
dlnltro-)
2.6-Dlnltrotoluene (Benzene, l-methyl-2.6-
dlnltro-)
Dl-n-octyl phthalate (1.2-Benzenedlcarboxy-
Uc acid. dJoctyl eater)
1.4-Dloxane (1.4-Diethylene oxide)
Diphenylamlne (Benzenamlne. N-pheny)-)
1.2-Diphenylhydracine (Hydracine. 1,2-dl-
phenyl-)
Port 261, App. VIII
DI-n-propylnitroMmlne (N-Nltro*o-dl-n-pro-
pylamlne)
Dliulfoton (O.O-dlethyl 8-t>-
(ethylthlo)ethyn pho«phorodlthioat«)
2,4-Dlthlobluret (Thlolmldodlcarbonlc dla- •
mlde)
Kndoiulfan (6-Norbomene. 2.1-dlmethanol.
1.4.B.6.7.7-hexachloro-. cyclic lulflte)
Bndrin and metabolite* (1.2,1,4.10.10-hex-
achloro-6,7-epoxy-l,4,4a.6.a.7,8.8a-
octahydro^ndo.endo-1.4:6.8-
dimethanonaphthalene, and metabolite*)
Ethyl carbamate (Drethan) (Carbamlc add.
ethyl eater)
Ethyl cyanide (propanenitrlle)
EthylenebUdlthlocarbamic add. aalta and
eaten (1.2-EthanedlylblacarDamodlthlolc
add. aalta and eaten
Ethylenelmlne (Azlridlne)
Ethylene oxide (Oxlrane)
Ethylenethlourea (2-ImidazoUdinethlone)
Ethyl methacrylate (2-Propenolc acid. 2-
methyl-. ethyl eater)
Ethyl methaneaulfonate (Uethaneaulfonlc
acid, ethyl eater)
Fluoranthene (BcnzoCJjLlfluorene)
Fluorine
2-Fluoroacetamlde (Acetamlde, 2-fluoro-)
Fluoroacetic add. aodlum aalt (Acetic add,
fluoro-, aodlum aalt)
Formaldehyde (Methylene oxide)
Formic acid (Methanoic acid)
Olycldylaldehyde (l-Propanol-2,3-epoxy)
Halomethane. N.O^.'
Heptachlor (4.7-Methano-lH-indene,
1.4.6,6.7.B,8-heptacnloro-3a,4.7,7a-
tetrahydro-)
Heptachlor epoxlde (alpha, beta, and
camma laomen) (4.7-Methano-lH-lndene.
1.4.E.8.7.S.e-heptachloro-2.3-epoxy-3a,4,7.7-
tetrahydro-. alpha, beta, and camma Uo-
men)
Hexachlorobenzene (Benzene, hexachloro-)
Hexachlorobutadlene (1.3-Butadlene,
1.1,2.3.4,4-hexachloro-)
Hexachlorocyclohexane (all Isomen) (Un-
done and Uomen)
Hexachlorocyclopentadlene (1.3-Cydopen-
tadlene, 1.2,3.4.S,6-hexachloro->
Hexachlorodlbenzo-p-dloxlna
Hexachlorodlbenzofurani
Hexachloroethane (Ethane. 1.1.1,2.2,2-hex-
achloro-)
1.2.3.4.10.10-Hexachloro-1.4.4a.S.8.B«-
hexahydro-1.4:&.B-endo.endo-
dlmethanonaphthalene (Hexachlorohexa-
hydro-endo.endo-dimethanonaphthalene)
Hexachlorophene (2.2'-Methylenebls(3.4.6-
trichlorophenol))
Hexachloropropene (1-Propene. 1.1.2.3.3.}-
hexachloro-)
Hexaethyl tetraphoaphate (Tttrapboa-
phorlc acid, hexaethyl eater)
Hydrazlne (Dlamlne)
Hydrocyanic add (Hydrofm cyanide)
Hydrofluoric add (Hydroten nuorldt)
Part 261, App. VIII
Hydrogen auldde (Sulfur hydride)
Hydroxydlmethylanlne oxide (Caeodylle
acid)
Indeno(l,2.3-cd)pyrene
phenylene)pyrene)
lodomethane (Methyl Iodide)
Iron dextran (Ferric dextran)
kocytnlc acid, methyl eater (Methyl lao-
cyanate)
Uobutyl alcohol (1-Propanol. 2-methyl-)
Uoaalrole (Benzene. 1.2-methylenedloxy-4-
allyl-)
Kepone (Decachlorooctahydro-1.3.4-Meth-
ano-2H-cyclobuta[cd]pentalen-2-one)
Lulocarplne (2-BuUnolc acid. 2-methyl-. 7-
[(2,3-dUiydroxy-2-(l-methoxyethyl>->-
methyl-l-oxobutoxy)methyl)-2.3.8.7a-
tetrahydro-lH-pyrrollzln-1-yl eater)
Lead and compounds. N.O.8.*
Lead acetate (Acetic acid, lead aalt)
Lead phoaphate (Phosphoric acid, lead aalt)
Lead subacetate (Lead, bla(acetato-
O)tetrahydroxytri->
Malelc anhydride (2.5-Furandlone)
Malelc hydrazide (1.2-Dlhydro-3.e-pyridaxtn-
edlone)
Malononitrile (Propanedlnltrile)
Melphalan (Alanlne. 3-[p-bla(2-
chloroethyl)aminolphenyl-, L-)
Mercury fulminate (Fulmlnlc add. mercury
aalt)
Mercury and compound!. N.O.8.*
Methacrylonltrlle (2-Propenenltrlle, 2-
methyl-)
Methanethlol (Thiomethanol)
Methapyrilene (Pyrldlne, 2-1(2-
dlmethy lamlno )ethyll-2-thenylamlno-)
Metholmyl (Acetlmidlc add. N-
C(methylcarbamoyl)oxy3thio-, methyl
eater
Methoxychlor (Ethane, l.l.l-trtchloro-2.2'-
bla(p-methoxyphenyl)-)
2-Methylaziridlne (1,2-Propylenlmlne)
3-Methylcholanthrene
(Benz[J]aceanthrylene, 1.2-dlhydro-l-
methyl-)
Methyl chlorocarbonate (Carbonochloridic
acid, methyl ester)
4,4'-MethyleneMs(3-chloroanUine) (Benzen-
amlne. 4.4'-methyleneb!s-(2-ch)oro-)
Methyl ethyl ketone (MEK) (2-Butanone)
Methyl hydrazlne (Hydrazlne, methyl-)
2-Methyllactonltrile (Propanenltrile, a-hy-
droxy-2-methyl-)
Methyl methacrylate (3-Propenolc add, 2-
methyl-. methyl ester)
Methyl methanesulfonate (Methanesulfonlc
add. methyl ester)
2-Methyl-2-(methylthlo)proplonaldehyde-o-
(methylcarbonyl) oxime (PropanaL 2-
methyl-2-(methylthlo>-, Q-
I( methy lamlno Xajbonylloxlme)
N-Methyl-N'-nltro-N-nltroaoKuanldlne (Qua-
nldlne. N-nltroso-N-methyl-N'-nltro-)
Methyl parathlon (O.O-dlmethyl O-(4-nitro-
phenyl) phoaphorothloate)
40 CFR Ch. I (7-1-«5 Edition)
Methylthlouraell (4-lH-Pyrtmldinone. 2.3-
dlhyoro-tt-methyl-3-thloxo-)
Mustard gas (Sulflde. bia(2-chloroethyl)-)
Naphthalene
1.4-Naphthoqulnone (1.4-Naphthalene-
dlone)
1-Naphthylamlne (alpha-Naphthylamlne)
2-Naphthyiamlne (beta-Naphthylamine)
l-Naphthyl-2-thlourea (Thiourea, 1-naphth-
alenyl-)
Nickel and compounds. N.O.8.*
Nickel carbonyl (Nickel tetracarbonyl)
Nickel cyanide (Nickel (U) cyanide)
Nicotine and aalU (Pyrldlne, (8>-3-U-
methyl-a-pyrrolidlnylK and aalts)
Nitric oxide (Nitrogen (D) oxide)
p-Nltroanlllne (Benzenamlne, 4-nltro-)
Nltrobencine (Benzene, nltro-)
Nitrogen dioxide (Nitrogen (TV) oxide)
Nitrogen mustard and hydrochloride aalt
(Ethanamlne. 3-ehloro-, N-(2-chloroethyl)-
N-methyl-. and hydrochloride aalt)
Nitrogen mustard N-Oxlde and hydrochlo-
ride aalt (Ethanamlne. 2-chloro-. N-(2-
chloroethyl>-N-methyl-, and hydrochlo-
ride aalt)
Nitroglycerine (1.2.1-Propanetriol. trinl-
trate)
4-Nltrophenol (Phenol, 4-nltro-)
4-NltroqulnoUne-l-oxide (Qulnollne. 4-nltro-
1-oxide-)
Nltroaamine. N.O.S.*
N-Nltroaodi-n-butylamlne (1-Butanamine,
N-butyl-N-nltroao-)
N-Nttrosodlethanolamme (Ethanol, 2.21-
(nltroaolmlno)bls-)
N-Nltroaodlethylamlne (Ethanamlne. N-
ethyl-N-nltroao-)
N-Nltrosodlmethylamlne (Dlmethylnltroaa-
mlne)
N-Nltroao-N-ethylurea (Carbamide, N-ethyl-
N-nitroao-)
N-Nltroaomethylethylamine (Ethanamlne.
N-methyl-N-nltroso-)
N-Nltroso-N-methylurea (Carbamide. N-
methyl-N-nltroao-)
N-Nltroao-N-methylurethane (Carbamlc
add. methylnltroso-. ethyl ester)
N-Nltroaomethylvlnylamine (Ethenamlne,
N-methyl-N-nltroao-)
N-Nltroaomorphollne (Morphollne, N-nltro-
ao->
N-Nltrosonomicotine (Nomteotlne. N-
nitroao-)
N-Nltroaoplperidlne (Pyrldlne, hexahydrc-.
N-nitroao-)
Nltroaopyrrolldlne (Pyrrole, tetrahydro-, N-
nltroao-)
N-Nltroaoaarcoalne (Sarcoaine. N-nltroao-)
5-Nltro-o-toluldlne (Benzenamlne. 2-methyl-
5-nltro-)
Octamethylpyrophosphoramlde (Dlphos-
phoramide, octamethyl-)
Osmium tetroxlde (Oamlum (Vm> oxide)
7-OxablcycloC2J.l]heptane-2.3-dlcarboxyllc
add (Endothal)
387
388
-------
Environmental Protection Agoncy
Paraldehyde (1,3,5-Trioxane, 2,4.6-trl-
methyl-)
Parathlon (Phosphorothlolc Mid. O,O-
diethyl CMp-nitrophenyl) eater
Pentachlorobenzene (Bensene. penUchloro-
)
Pentachlorodlbenzo-p-dloxlna
Pentachlorodlbenzofuran*
PenUchloroethuie (Ethane, penUchloro-)
Pentmchloronltrobenzene (PCNB) (Benzene.
pentachloronltro-)
PenUchloraphenol (Phenol, penUchloro-)
Pheiucetin (AceUmlde. N-(4-ethoxy-
phenyl)-)
Phenol (Benzene, hydroxy-)
Phenylenediamine (Benzenediamine)
Phenylmercury acetate (Mercury. aceUto-
phenyl-)
N-Phenylthloure* (Thiourea, phenyl-)
Phosgene (Carbonyl chloride)
PhMphlne (Hydrogen phoiphlde)
Phoephorodlthioic acid. O.O-diethyl 8-
[(ethylthiotanethyl) eater (Phorate)
Phoephorothlolc acid. O.O-dimethyl O-lp-
((dlmethylaminotoulfonyDphenyl] ester
(Famphur)
Phthalic acid eaten. N.O.S.* (Benzene, 1.2-
dlcarboxylic acid, eaten. N.O.S.*)
Phthalic anhydride (1.2-Benzenedlcarboxy-
llc acid anhydride)
2-Plcoline (Pyridine, a-methyl-)
Polychlorlnated blphenyl. N.O.S.*
Potassium cyanide
Potassium silver cyanide (ArgentateUO. dl-
cyano-. potassium)
Pronamide (3.5-Dichlorc-N-U.l-dlmethyl-2-
propynyDbenzamlde)
1.3-Propane sultone (1.2-Oxathiolane, 2,2-dl-
oxide)
n-Propylamlne (1-Propanamlne)
Propylthlouracil (Dndecamethylenedla-
mine. N.N'-bia(3-chlorobenzyl>-. dlhy-
drochlorlde)
2-Propyn-l-ol (Propargyl alcohol)
Pyridine
Reserpine (Tohlmban-16-carboxyllc acid.
1 1.17-dlmethoxy-18-[(3.4.5-
trimethoxybenzoyl)oxy)-. methyl eater)
Resorctnol (1,3-Benzenedlol)
Saccharin and salts (l,2-Benzoiaothlazolin-3-
one. 1,1-dioxlde, and salts)
Saf role (Benzene, 1.2-methylenedloxy-4-
allyl-)
Selenlous acid (Selenium dioxide)
Selenium and compounds. N.O.8.*
Selenium sulflde (Sulfur selenide)
Selenourea (Carbamlmldoselenolc acid)
Silver and compounds, N.O.S.*
Silver cyanide
Sodium cyanide
Streptozotocln (D-Glucopynnose. 2-deoxy-
2-( 3-methyl-3-nltroaoureldo >-)
Strontium aulflde
Strychnine and salts (Strychnldln-10-one.
and salts)
1,2,4,6-Tetrachiorobenzene (Benzene.
1.2.4.5-tetrachloro-)
fort 961, App. VIII
XS.7.B-Tetnchlorodlbenso-p-dloxln (TCDD)
(Dlbenco-p-dloxln, 2.3.7.B-tetrachloro-)
Tetrachlorodibenzo-p-dloxins
Tetrachlorodlbenzofurans
Tetrachloroethane, N.O.S.0 (Ethane, tetra-
chloro-. N.O.8.*>
l.l.l.a-Tetrachlorethane (Ethane. 1.1.1.2-
tetrachloro-)
1.1.2.2-Tetrachlorethane (Ethane, 1.1,2.2-
tetrachloro-)
Tetrachloroethane (Ethene. 1.1.2.2-tetra-
chloro-)
Tetrachloromethane (Carbon tetrachlorlde)
2.3.4.6,-Tetrachlorophenol (Phenol, 2,3,4.6-
tetrachloro-)
Tetraethyldlthlopyrophosphate (Dlthlopyr-
ophosphorlc acid, tetraethyl-eater)
Tetraethyl lead (Plumbane, tetraethyl-)
Tetraethylpyrophospbate (Pyrophoaphorlc
acide. tetraethyl ester)
Tetranltromethane (Methane, tctrmnitro-)
Thallium and compounds. N.O.8.*
Thalllc oxide (Thallium (HI) oxide)
Thallium (I) acetate (Acetic acid, thallium
(I)salt)
Thallium (I) carbonate (Carbonic add, dlth-
alllum(I)salt)
Thallium (I) chloride
Thallium (I) nitrate (Nitric add, thallium
(I) salt)
Thallium selenite
Thallium (I) sullate (Sulfurlc add. thallium
(I) salt)
Thloacetamlde (Ethanethioamide)
Thiosemlcarbszide (Hydrazlnecarbothioa-
mlde)
Thiourea (Carbamide thlo-)
Thiuram (Bls(dimethylthlocarbamoyl) dl-
aulflde)
Toluene (Benzene, methyl-)
Toluenedlamlne (Dlaminotoluene)
o-Toluldlne hydrochloride (Benzenamine. 2-
methyl-. hydrochloride)
Tolylene dllsocyanate (Benzene. 1.3-dllso-
cyanatomethyl-)
Toxaphene (Camphene, octachloro-)
Trlbromomethane (Bromofonn)
1.2.4-Trichlorobenzene (Benzene. 1.2.4-trlch-
loro-)
1.1.1-Trlchloroethane (Methyl chloroform)
1.1,2-Trichloroethane (Ethane. 1,1,2-trich-
loro-)
Trlchloroethene (Trlchloroethylene)
Trlchloromethanethlol (Methanethlol.
trlchloro-)
Trichloromonofluoromethane (Methane.
trlchlorofluoro-)
2,4.5-Trlchlorophenol (Phenol, 2.4.6-trich-
loro-)
2.4.6-Trich)orophenol (Phenol. 2,4.8-trich-
loro-)
2.4.5-Trlchlorophenoxyacetlc acid (2.4.5-T)
(Acetic acid, 2.4,5-trichlorophenoxy-)
2,4,B-Trlchlorophenoxyproplonic acid (2,4.5-
TP) (Sllvex) (Propionolc acid. 2-(2,4,S-
trlchl orophenoxy >-)
Part 261, App. IX
Trlchloropropane. N.OJ.' (Propane, trich-
loro-. N.OA*)
1.2.3-Trlchloropropane (Propane, l,J,3-trich-
loro-)
O.O.O-Trlethyl phoaphorothloate (Phoa-
phorothlolc acid. O.O.O-triethyl eater)
sym-Trlnltrobenzene (Benzene, 1,3.6-trlnl-
tro-)
Trls(l-azridlnyl) phosphlne sulflde (Phoa-
phlne aulflde. triad •azlridinylO
Trls(2.3-dlbromopropyl) phosphate (1-Pro-
psnol, 2.3-dlbromo-, phosphate)
Ttypsn blue (2,7-Naphthalenedlsulfonlc
acid. 3,3'-[(3.3>-dlmethyl(l.r-blphenyl>-
4.4'-dlyl)bls(azo)lbls(5-amino-4-hydroxy-.
tetrasodlum salt)
Uracll mustard (Dracll B-[bl»(2-
chloroethyDamlno)-)
Vanadlc acid, ammonium salt (ammonium
vansdate)
Vanadium pentoxide (Vanadium (V) oxide)
Vinyl chloride (Ethene. chloro-)
Zinc cyanide
Zinc phosphide
[46 PR 27477. May 20, 1081: 46 FR 29708,
June 3.1881. as amended at 49 FR 5312. Feb.
10. 1984; 60 FR 2000. Jan. 14. 1885]
EmcTTVi DATE NOTE At 60 FR 2000. Jan.
14. 1985, Part 261, App. VIII was amended
by adding the entries for Hexachlorodl-
tMttH>-p-dioxlna, Hexachlorodlbenzofurans.
Pentachlorodlbenzo-p-dloxins, Pentachloro-
dlbenzofurana, Tetrachlorodlbenzo-p-dlox-
1ns. and Tetrachlorodlbenzofurans. effective
July 15.1986.
APPENDIX IX—WASTES EXCLUDED
UNDER i{ 260-20 AND 260.22
TABLE 1—WASTES EXCLUDED FROM NON-
SPECIFIC SOURCES
Mmopotttvi
DiMnttol
Grtctw
Crannall
StofwyPaM.
NY.
Qnckmtl. OH..
fl»n«rat«d in*
Scpuntxr 21, 18*4.
wtiic^i oootain EPA Hex*
•ntow Wut* Not. FOO3
and F005 M wall u «•!
Icgoan u ol
21. 19S4.
SUiwd bottom nh
(«Pt»o«Jr»«>«ty 29.000
attc ywdt). oanWnid
In th» North LtQOon, on
S«p»mb»r 21, 19M.
EPA
Not
FOOL F002. F003. FOO4,
•ndFOOS.
40 CM Ch. I (7-105 Edition)
TABLE 2—WASTES EXCLUDED FROM SPECIFIC
SOURCES
FcoWy
(Rwciv**)
AddraH
WMttt OMOnptOO
TABLE 3—WASTES EXCLUDED FROM COMMER-
CIAL. CHEMICAL PRODUCTS, OFF-SPECIFICA-
TION SPECIES, CONTAINER RESIDUES. AND
SOIL RESIDUES THEREOF
FHMy
Union Cotkte
Coip.
T«n.LA..
ConUnwMMd tai (weraa-
miMy 11.000 eubk
torn ol tow Km 9 ppm.
[49 FR 17070. Sept 21. 10S4)
APPENDIX X—METHOD or ANALYSIS FOR
CHLORINATED DiBEnio-r-DioxncB AND
-DIBENZOimtANS L l * 4
ttethod 1210
1. Scope and Application
i This method Is appropriate for the anal-
ysis of tetra-, penta-, and hexachlorinated
dlbenio-p-dioxlna and -dibensof urana.
•Analytical protocol for determination of
TCDDs In phenolic chemical wastes and soil
samples obtained from the proximity of
«-h»mii*«i dumps. T.O. Tlernan and M.
Taylor. Brehm laboratory. Wright State
University, Dayton. OH 46436.
•Analytical protocol for determination of
chlorinated dlbenco-p-dloxlns and chlorinat-
ed dlbenzofurans In river water. T.O. Tier-
nan and M. Taylor. Brehm Laboratory.
Wright State University, Dayton. OH 46436.
4 In general, the technique* that should be
used to handle these materials are those
which are followed for radioactive or infec-
tious laboratory materials. Assistance In
evaluating laboratory practices may be ob-
tained from Industrial hyglenlsts and per-
sons specialising In safe laboratory prac-
tices. Typical infectious waste Incinerators
are probably not satisfactory devices for dis-
posal of materials highly contaminated with
CDDs or CDFs. Safety instructions are out-
lined In EPA Teat Method 613(4.0)
See also: 1) "Program for monitoring po-
tential contamination In the laboratory fol-
lowing the handling and analyses of chlorin-
ated dlbenzo-p-dloxlns and dlbenzofurans"
by F. D. Hlleman et aL. In: Human and En-
ConUnued
389
300
-------
Environmental Protection Agoncy
1.1 This method measure* the coneentra-
.Ion of chlorinated dlbenao-p-dioxlns and
chlorinated dlbeniofunni In chemical
vastes including still bottom*, (liter aids.
Judges, ipent carbon, and reactor residues.
Ad In soils.
1.2 The sensitivity of thli method 1* de-
jendent upon the level of Interference*.
1.3 This method to recommended for use
inly by analysts experienced with residue
inalyili and skilled In mat* spectral analytl-
:al techniques.
1.4 Because of the extreme toxlclty of
.hese compounds, the analyst must take
lecessary precautions to prevent exposure
•o himself, or to others, of materials known
>r believed to contain CDDs or CDPs.
2. Summary of Ote Method
2.1 This method is an analytical extrac-
ion cleanup procedure, and capillary
xilumn IBS chromatograph-low resolution
nass spectrometry method, using capillary
x>lumn QC/MS conditions and Internal
itandard techniques, which allow for the
aeasurement of PCDDs and PCDPs In the
ixtract.
2.2 If Interferences are encountered, the
nethod provides selected general purpose
•Jeanup procedures to aid the analyst In
,helr elimination.
3. Interference*
3.1 Solvents, reagents, glassware, and
ither sample processing hardware may yield
Uscrete artifacts and/or elevated baselines
Busing misinterpretation of gas chromato-
{rams. All of these materials must be dem-
onstrated to be free from Interference*
jnder the conditions of the analysis by run-
ling method blanks. Specific selection of
reagents and purification of solvents by dls-
miatlon In all-glass systems may be re-
quired.
3.2 Interferences co-extracted from the
lamples will vary considerably from source
jo source, depending upon the diversity of
,he industry being sampled. PCDD is often
usociated with other Interfering chlorinat-
ed compounds such as PCB's which may be
it concentrations several orders of magnl-
:ude higher than that of PCDD. While gen-
eral cleanup techniques are provided as part
Df this method, unique samples may require
additional cleanup approaches to achieve
.he sensitivity stated In Table 1.
3.3 The other Isomen of tetrachlorodi-
aenzo-p-dloxln may interfere with the meas-
urement of 2.3.7,8-TCDD. Capillary column
tas chromatography IB required to resolve
/ironmental Risks of Chlorinated Dtoxlns
uid Related Compounds. RJC. Tucker, et al,
ads.. Plenum Publishing Corp.. 1083. 2)
Safety procedures outlined In EPA. Method
313. Federal Register volume 44. No. 233,
December 3.1979.
Part 261, App. X
those Isomen that yield virtually Identical
mass fragmentation patterns.
4. Apparatus and Uaterialt
4.1. Sampling equipment for discrete or
composite sampling.
4.1.1 Orab sample bottle—amber glass, 1-
liter or 1-quart volume. French or Boston
Round design Is recommended. The contain-
er must be washed and solvent rinsed before
use to minimize Interferences.
4.1.2. Bottle caps—threaded to screw on
to the sample bottles. Caps must be lined
with Teflon. Solvent washed foil, used with
the shiny side towards the sample, may be
substituted for the Teflon if sample is not
corrosive.
4.1.3. Compositing equipment—automatic
or m""i»i composing system. No tygon or
rubber tubing may be used, and the system
must Incorporate glass sample containers
for the collection of a minimum of 250 ml.
Sample containers must be kept refrigerat-
ed after sampling.
4.2 Water bath—heated, with concentric
ring cover, capable of temperature control
(±2 'C>. The bath should be used In a hood.
4.3 Oas chromatograph/mass spectrome-
ter data system.
4.3.1 Oas chromatograph: An analytical
system with a temperature-programmable
gas chromatograph and all required accesso-
ries including syringes, analytical columns,
and gases.
4.3.2 Column: SP-2250 coated on a 30 m
long x 0.25 mrn ij). glass column (Supelco
No. 2-3714 or equivalent). Olass capillary
column conditions: Helium carrier gas at 30
cm/sec linear velocity run splitless. Column
temperature Is 210 'C.
4.3.3 Mass spectrometer: Capable of scan-
ning from 35 to 450 amu every 1 sec or leu,
utilizing 70 volts (nominal) electron energy
In the electron Impact ionlzstlon mode and
producing a mass spectrum which meets all
the criteria in Table 2 when 50 ng of deca-
fluorotriphenyl-phosphlne (DFTPP) Is In-
jected through the OC Inlet. The system
must also be capable of selected Ion moni-
toring (SIM) for at least 4 Ions simulta-
neously, with a cycle time of 1 sec or less.
Minimum integration time for SIM Is 100
ms. Selected ion monitoring Is verified by in-
jecting .015 ng of TCDD Cl" to give a mini-
mum signal to noise ratio of 5 to 1 at mass
328.
4.3.4 OC/MS Interface: Any OC-to-MS
Interface that gives acceptable calibration
points at 60 ng per Injection for each com-
pound of Interest and achieves acceptable
tuning performance criteria (see Sections
8.1-8.3) may be used. OC-to-MS Interfaces
constructed of all glass or glass-lined materi-
als are recommended. Olass can be deacti-
vated by sllanlzlng with dlchlorodlmethylsl-
lane. The Interface must be capable of
Part 261, App. X
transporting at least 10 ng of the compo-
nents of Interest from the OC to the MS.
4.3.5 Data system: A computer system
must be interfaced to the mass spectrome-
ter. The system must allow the continuous
acquisition and storage on machine-readable
media of all mass spectra obtained through-
out the duration of the chromatographlc
program. The computer must have software
that can search any OC/MS data file for
Ions of a specific mass and that can plot
such Ion abundances versus time or scan
number. This type of plot Is defined as an
Extracted Ion Current Profile (EICP). Soft-
ware must also be able to Integrate the
abundance. In any EICP. between specified
time or scan number limits.
4.4 Pipettes-Disposable. Pasteur, 150 mm
long x 5 mm ID (Fisher Scientific Co.. No.
13-678-6A or equivalent).
4.6 Flint glass bottle (Tenon-lined screw
cap).
4.8 Reactl-vlal (sUanlzed) (Pierce Chemi-
cal Co.).
6. Reapenti
6.1 Potassium hydroxlde-
-------
Environmental Protection Agency
traction. Chemical preservative* should not
be used In the field unless more than 24
houn will elapse before delivery to the labo-
ratory. If an aqueous lunple Is Uken and
the aample will not be extracted within 48
houn of collection, the sample ahould be
adjuited to a pH ranee of 9.0-8.0 with
aodlum hydroxide or iulf uric acid.
8.3 All aamplei must be extracted within
7 dayi and completely analyzed within 30
days of collection.
.9. Extraction and Cleanup Procedure*
9.1 tlae an aUquot of 1-10 I aample of the
chemical waste or aoU to be analysed. Soil*
ihould be dried using a ctream of prepurl-
fled nitrogen and pulverized in a ball-mill or
•Imllar device. Perform this operation In a
clear area with proper hood apace. Transfer
the aample to a tared 136 ml flint clan
bottle (Teflon-lined acrew cap) and deter-
mine the weight of the aample. Add an ap-
propriate quantity of "Cl-labelled 3.3,7.8-
TCDD (adjuit the quantity according to the
required minimum detectable concentra-
tion), which U employed at an internal
standard.
B.I Extraction
9.2.1 Extract chemical wa*te aample* by
adding 10 ml methanol, 40 ml petroleum
ether. 60 ml doubly distilled water, and then
shaking the mixture for 2 minute*. Tan
should be completely dlaaolved in any of the
recommended neat aolvenU. Activated
carbon aamplef muct be extracted with ben-
zene using method 3640 In 8W-846 (Test
Method* for Evaluating Solid Waite—Phyai-
cal/Chemlcal Method*, available from
Qf.O. Stock #056-022-81001-2). Quantita-
tively transfer the organic extract or dis-
solved aample to a clean 260 mi nint glass
bottle (Teflon lined screw cap), add 60 ml
doubly distilled water and shake for 2 min-
ute*. Discard the aqueous layer and proceed
with Step 9.3.
9.2.2 Extract soil sample* by adding 40
ml of petroleum ether to the aample, and
then shaking for 20 minute*. Quantitatively
transfer the organic extract to a clean 260
ml flint glass bottle (Teflon-lined screw
cap), add 60 ml doubly distilled water and
shake for 2 minutes. Discard the aqueous
layer and proceed with Step 9.3.
9.3 Wash the organic layer with 60 ml of
20% aqueous potassium hydroxide by shak-
ing for 10 minutes and then remove and dis-
card the aqueous layer.
9.4 Wash the organic layer with 50 ml of
doubly distilled water by shaking for 2 min-
utes, and discard the aqueous layer.
9.6 Cautiously add 60 ml concentrated
•ulfurtc add and shake for 10 minute*.
Allow the mixture to stand until layers sep-
arate (approximately 10 minutes), and
remove and discard the add layer. Repeat
acid washing until no color Is visible in the
acid layer.
Part 261, App. X
9.6 Add 60 ml of doubly distilled water to
the organic extract and shake for 2 minute*.
Remove and discard the aqueous layer and
dry the organic layer by adding lOg of anhy-
drous sodium sulf ate.
9.7 Concentrate the extract to Incipient
dryneas by heating in a 66' C water bath
and simultaneously flowing a stream of pre-
purlfled nitrogen over the extract. Quanti-
tatively transfer the residue to an alumina
mlcrocolumn fabricated as follows:
9.7.1 Cut off the top section of a 10 ml
disposable Pyrex pipette at the 4.0 ml mark
and Insert a plug of sllanlzed glass wool Into
the Up of the lower portion of the pipette.
9.7.2 Add 2.8g of Woelm basic alumina
(previously activated at 000° C overnight
and then cooled to room temperature In a
desiccator lust prior to use).
9.7.3 Transfer sample extract with a
small volume of methylene chloride.
9.8 Elule the mlcrocolumn with 10 ml of
1% methylene cholrlde-in-hexane followed
by 16 ml of 20% methylene chlorlde-ln-
hexane and discard these effluent*. Elute
the column with 16 ml of 60% methylene
chlorlde-in-hexane and concentrate this ef-
fluent (66' C water bath, stream of prepurl-
fled nitrogen) to about 0.3-0.5 ml.
9.9 Quantitatively transfer the residue
(using methylene chloride to rinse the con-
tainer) to a sllanized Reactl-Vial (Pierce
Chemical Co.). Evaporate, using a stream of
prepurtfted nitrogen, almost to dryness.
rinse the walls of the vessel with approxi-
mately 0.6 ml methylene chloride, evaporate
just to dryness, and tightly cap the vial.
Store the vial at 6* C until analyst*, at
which time the aample Is reconstituted by
the addition of trldecane.
9.10 Approximately 1 hour before GC-
MS (HRQC-LRMS) analysis, dilute the resi-
due in the micro-reaction vessel with an ap-
propriate quantity of trldecane. Gently
swirl the trldecane on the lower portion of
the vessel to ensure dissolution of the CDDs
and CDF's. Analyze a sample by OC/EC to
provide Insight into the complexity of the
problem, and to determine the manner In
which the mass spectrometer should be
used. Inject an appropriate aliquot of the
sample Into the OC-MS instrument, using a
syringe.
9.11 If, upon preliminary OC-MS analy-
sis, the sample appears to contain Interfer-
ing substances which obscure the analyses
for CDDs and CDFs, high performance
liquid chromalographtc (HPLC) cleanup of
the extract Is accomplished, prior to further
OC-MB analysis.
10. HPLC Cleanup Procedure'
' For cleanup see also method #8320 or
#8330, SW-846. Test Methods for Evaluat-
ing Solid Waste, Physical/Chemical Meth-
ods (1982).
Part 261, App. X
10.1 Place approximately 2 ml of hexane
in a-60 ml flint glass sample bottle fitted
with a Tenon-lined cap.
10.2 At the appropriate retention time,
position sample bottle to collect the re-
quired fraction.
10.3 Add 2 ml of 6% (w/v) sodium car-
bonate to the sample fraction collected and
shake for one minute.
10.4 Quantitatively remove the hexane
layer (top layer) and transfer to a micro-re-
action vessel.
10.6 Concentrate the fraction to dryness
and retain for further analysis.
11. OC/ltS Analyti*
11.1 The following column condition* are
recommended: Olas* capillary column condi-
tion*: BP-2260 coated on a SO m long x 0.26
mm LD. glass column (Bupelco No. 2-3714.
or equivalent) with helium carrier gas at 30
cm/sec linear velocity, run splltless. Column
temperature I* 210'C. Dnder these condi-
tions the retention time for TCDDs I* about
9.5 minutes. Calibrate the system daily
with, a minimum, three Injection* of stand-
ard mixture*.
11.2 Calculate response factors for stand-
ards relative to •Kn-TCDD/P (see Section
12).
114 Analyse sample* with selected Ion
monitoring of at least two Ion* from Table
1 Proof of the presence of COD or CDF
exists If the following conditions are met:
11.3.1 The retention time of the peak In
the sample must match that In the stand-
ard, within the performance specification*
of the analytical system.
11.3.2 The ratio of ions must agree
within 10% with that of the standard.
40 CPU Oi. I (7-103 fdttlan)
11.3.3 The retention time of the peak
maximum for the tons of interest must ex-
actly match that of the peak.
11.4 Quantltate the CDD and CDF peaks
from the response relative to the "Cl-
TCDD/F internal standards. Recovery of
the Internal standard should be greater
than (0 percent.
11.5 If a response I* obtained for the ap-
propriate set of ion*, but I* outside the ex-
pected ratio, a oc-eluting impurity may be
suspected. In this case, another set of ion*
characteristic of the CDD/CDF molecules
should be analysed. For TCDD a good
choice of Ions I* m/e 367 and m/e 269. For
TCDF a good choice of Ion* Is m/e 241 and
343. These Ion* axe useful In characterizing
the molecular structure to TCDD or TCDF.
For analysis of TCDD good analytical tech-
nique would require using all four Ion*, m/e
287. 330. 133. and 138. to verify detection
and signal to noise ratio of 5 to 1. Suspected
impurities such as DDE*. DDD. or PCB resi-
due* can be confirmed by checking for their
major fragments. These materials can be re-
moved by the cleanup columns. Failure to
meet criteria should be explained In the
report, or the sample reanalyzed.
11.6 If broad background Interference re-
.strict* the sensitivity of the OC/MS analy-
sis, the analyst should employ cleanup pro-
cedures and reanalyze by OC/MS. See sec-
tion 10.0.
11.7 In those circumstance* where these
procedures do not yield a definitive conclu-
sion, the use of high resolution mas* spec-
trometry I* suggested.
12. Calculation*
12.1 Determine the concentration of Indi-
vidual compound* according to the formula:
Concentration, fig/am-
AxA.
where:
A-(ig of Internal standard added to the
sample'
O-gm of sample extracted
A,-area of characteristic Ion of the com-
pound being quantified.
A*-area of characteristic Ion of the Inter-
nal standard
R,-response factor •
Response factors are calculated using data
obtained from the analyst* of standards ac-
cording to the formula:
'The proper amount of standard to be
used is determined from the calibration
curve (See Section 6.0).
,,'JL rt*"1**"1* 'or PCDDs/Fs and
HxCDDs/Fs are not available, response fac-
ton for Ions derived from these congeners
are calculated relative to 'Xn-TCDD/F The
analyst may use response factors for 1.2.3.4-
or 2.1.7.8-TCDD, 1,2.1,4,7-PeCDD. or
1.2,3,4.7.8-HxCDD for quantltatlon of
TCDDs/F*. PeCDDs/Ps and HxCDDs/Fs.
respectively. ImpUdt In this requirement Is
the assumption that the same response Is
obtained from PCDDs/Fs ccontalnlng the
same numbers of chlorine atoms.
393
394
-------
Environmental Protection Aaoncy
A.XC.
Rf
A..XC.
Port 261, App. X
•aual lo (~» MKM *<• QC background DOM attumng « 1
ml xwcto* Iml «ouiw o< »• 1 m> MTVM « 442.
1 J W EeMtMrp*. LE. Hvra. and W.L BmkM. 1876
n«l»r»no« compound to cahbrvw ion abundino* m«uur»-
fmnl In ou ehronuiography^niu •pcdromny. Anilvtccl
TABLE 3—LIST OF ACCURATE MASSES MONITORED USING GC SELECTED-ION MONITORING, Low
RESOLUTION, MASS SPECTROMETRY FOR SIMULTANEOUS DETERMINATION OF TETRA-, PENTA-,
AND HEXACHLORINATED DIBENZO-P-DIOXINS AND DIBENZOFURANS
T-»
Itmrfm
NumtMT
•utaM-
uwniO)
4
5
0
Monkoradm/z
tor
C,JB.-,OJ,
1 3K.M7
321. BM
•327M5
•266J33
'2M.B30
356.S55
3»i.ai3
Montaradm/i
tor
dibvcixofurw
C..H.-.OC1.
'303.902
306.903
•311M4
339MO
376.B1S
Approio-
miu
totorvfeoil
rMo
^(paCHfj
onbua of
IWKHC
•bundmoi
074
1.00
.
Oil
0.20
1.00
0.67
i Molcculsr no pvfttL
• c^—labelled standard
• torn when can M monHor»d n TCOO analyMi tor conflrmabon purpom
[SO PR 2001. Jan. 14.1B851
Emcnvr DATT NOTE At 60 FR 2001. Jan.
14. 1886, Part 261. App. X was added, effec-
tive July IS. 1085.
395
-------
APPENDIX C
QUALITY ASSURANCE PROJECT PLAN
(Must Be Completed For All Field Operations)
Project Name:
Project Manager:
Field Operations:
QA Office Concurrence:
ESD Peer Review:
Project No.:
Date:
Date:
Account No.:
Laboratory Designated:
EPA
CLP
Private
Sample Numbers assigned: from _
Sample Schedule and Milestones:
Activity/Date; / I
to
Reports Required;
Regional Sample Control Center Review
Date:
Project Description and Site Location:
Project Measurement Objectives (Intended use of data):
Sample rationale and network derivation:
- 1 -
-------
Analyses Rationale:
# of Parameter QA Matrix Container Holding Preservation
Samples Time
Data Quality Objectives:
Parameter Method Detection Precision Accuracy Completeness
lit
Sample procedures to he used:
Sample Custody and Documentation:
Calibration Procedures and Frequency:
Prevent ative Maintenance:
If, for any reason, the schedules or procedures above cannot be followed, the appropriate
person must complete a "Sample Alteration Checklist" for each element changed and have
it (them) verified and reviewed by the Project Manager and the QA Officer/Peer Review.
(See page 5)
- 2 -
-------
Laboratory Data Reduction / QA Review:
Field Data Reduction/QA Review:
Reports (as deliverable or required):
System and Performance Audits:
Scheduled: Conducted:
Corrective Action: (IF YES, COMPLETE CORRECTIVE ACTION CHECKLIST AND/OR
SAMPLE ALTERATION FORMS, Appendix B.)
QA Report to Management:
- 3 -
-------
Safety:
-4-
-------
SAMPLE ALTERATION CHECKLIST
Project Name and Number:
Material to be sampled:
Measurement Parameter:
Standard Procedure for Field collection & Laboratory Analysis (cite references):
Reason for change in Field Procedure or Analytical Variation:
Variation from Field or Analytical Procedure:
Special Equipment, Materials, or Personnel Required:
Initiators Name: _ _ Date:
Project Approval: _ _ _ Date:
Laboratory Approval: • _ _ _ Date:
Officer/Reviewer: Date:
SainPle Control Center: _ Date:
- 5 -
-------
CORRECTIVE ACTION CHECKLIST
Project Name and Number:
Sample Dates Involved:
Measurement Parameters):
Acceptable Data Range:
Problem Areas Requiring Corrective Action:
Measures Required to Correct Problems:
Means of Detecting Problems and Verifying Correction:
Initiators Name: Date:
Project Approval: _ Date:
Laboratory Approval: Date:
QA Officer/Reviewer: Date:
Sample Control Center: Date:
-6-
------- |