oEPA
United States
Environmental Protection
Agency
Office of
Solid Waste and
Emergency Response
DIRECTIVE NUMBER: 9445.02(84)
TITLE: Topics Relating to-RCRA Methodology and Quality
Assurance (QA) Activities
APPROVAL DATE: 4-23-84
EFFECTIVE DATE: *-23-84
ORIGINATING OFFICE: offlce of Solid Waate
E FINAL
D DRAFT
STATUS:
t 1
A- Pending OMB approval
t ] B- Pending AA-OSWER approval
[ 3 C- For revlev 4/or comment
[ ] D- In development or circulating
REFERENCE (other documents):
headquarters
OSWER OSWER OSWER
VE DIRECTIVE DIRECTIVE Dl
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PART 261 - APPENDICES DOC: 9445.02(84)
Key Words: EP Toxicity Test, QA/QC, Analytic Methods
Regulations:
Subject: Topics Relating to RCRA Methodology and Quality Assurance (QA)
Activities
Addressee: N/C
Originator: David Friedman, Manager, Methods Program
Source Doc: #9445.02(84) '
Date: 4-23-84
Summary:
EP Toxicity Test
The EP toxicity test requires that pH measurements be made only with a pH
meter. Frequent calibration of the pH meter is important; pH strips are not
accurate enough and must not be used.
All extracts must be digested before analyses, unless it was demonstrated,
on similar samples, that digestion is not necessary. All metal test methods in
SW-846 require this.
According to the EP toxicity test procedures, a representative sample of
the material tested must be prepared for extraction by crushing, cutting, or
grinding it into pieces which can pass through a 9.5 mm sieve.
In rare cases, manufactured articles with material inside which presents
an environmental problem, but which is encased in a leak-resistant, non-
destructible container that is an appropriate size, may be tested without
being cut-up pursuant to the Structural Integrity Procedure.
The Agency has not yet developed standardized EP toxicity test procedures
for structurally strong articles such as batteries which do not disintegrate
after disposal.
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9445.02~( 8"4T
RE: WCBFR0136
MEMORANDUM
SUBJECTi Notes on RCRA "Methodology and QA Activities
PROMj David Friedman
Manager
Methods Program (WH-S65B)
TOt Addressees
This menorandum is an attempt to assist regional, state
and other interested persons in keeping abreast of Agency
RCHA methodology and-Quality Assurance activities. I plan to
send out these brief memo ran'I
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,P Toxiclty Test
/
Adjustment o f pH
Recently, differences in the results of lead analyses
between two laboratories resulted in the discovery of a
problem in execution of the EP Toxicity Test. Upon examination,
by the Quality Assurance Officer for Region VI, it was determined
that pH adjustment was bein-j performed using pH paper and
not with a PH aoter. Tne E? tost is especially sensitive to
pH adjustment and for that reason the method requires that pH
measurements be made only with a pH meter. The pH strips
are not accurate enough *nd must not be used. In addition,
frequent calibration of tho pH meter is important. (See
SW-846 "Tost Methods for Evaluation Solid Waste," Method
1310, Step 7.13.1.)
»
Extract Digestion
Please remenbec that all extracts must be digested
prior to analysis unless it has been demonstrated, on similar
samples, that d-iges'tion is not necessary. All metal test
methods in SW-346 explicitly require this (see, for example,
Method 7040, Step 1.0).
Testing Manufactured Articles
T
The EP toxicity test procedure requires that a representative
sample of the material be prepared for extraction by crushing,
cutting or grinding into pioces which can pass through a 9.5
mm sieve.
The difficulty arises with manufactured articles when
the natorial Inside is an onvironraental problem but is encased
in a leak resistant container designed to be structurally
resistant to crushing, cutting or grinding. In rare cases where
such products are an appropriate size, they may be tested
without being cut-up pursuant to the Structural Integrity
Procedure.
Although sone batteries tend to degrade rapidly when
placed in a landfill, certain batteries are manufactured in
such a manner as to prevent disintegration after disposal.
However, at this time the Ayency has not developed standardized,
EP toxicity test procedures for structurally strong articles
such as batteries. EPA is considering proposing amendments
to the E? Toxicity test which would allow a package designed
to be structurally resistant to crushing, cutting, or'grinding
to be evaluated in the EP Toxicity test without being cut-up.
One possibility would be to test the corrosion resistance of
structurally resistant articles by submerging tha article in
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a 1M salt (HaCl) water solution at an elevated temperature
(60*-30*) for a period of one month. If no leaks occur the
product can be considered corrosion resistant. - ^.
I would appreciate hearing about any other suggestions you
may have with respect to this issue. We hope to be able to develop
a proposed amendment package in the near future.
Methods Evaluation
The Agency has Initiated an extensive research program
to determine the accuracy and precision of methods currently
in SW-846. At the present tine, the following methods are
being evaluated.
1110 Corrosivity Toward Steol
1120 Polarization Resistance Method
3030 Acid Digestion of Oils, Greases, or Waxes
3040 Dissolution Procedure for Oils, Greases, or Waxes
3050 Acid Digestion of Sludges
3010' Acid Digestion Procedure for Flame Atomic
Absorption Spectroscopy
3020 Acid Digestion for Furnace Atoaic Absorption
Spec tro 9 copy
7190 Chroraiun: Acoraic Absorption, Direct Aspiration
7191 Chromium: Atomic Absorption, Furnace Method
7195 Hexavalent Chromium: Coprecipitation
7196 Hexavalent Chroniuw: Cblorisietric
7197 Hexavalant Chromium: Chelation - Extraction
7198 Hexavalent Chromium: Differential Pulse
Polarography Method
t XXXX Hexavalent Chromium: Ion Chroroatography
Method Development
Our efforts continue with rsapect to the devolopsent of
additional methods for identifying hazardous wastas. Protocols
are being developed or existing methodology is being modified
to address the following areast
Ignitable Solids
*
The objective is to develop methods for
use in the da f In it ion. of ignitable solids.
Protocols have been developed and subjected
to single Ivr^ratory evaluation using actual
waste samples. Test have b
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-4-
Hazards Posod by Liquids with Flash Points belov 60*C
The objective is to- develop a ainple test
for identifying those liquids that should
not be considered as hazardous even though
they will flash at a temperature balow 60*C.
Many such materials will not sustain combustion
nor release sufficient ataounts of energy to
surrounding materials to spread the fire.
The evaluation report of this method is also
scheduled to be prepared and available for
regional review and comment by the end of
1934.
Reactive Gases - Cyanide and Sulfide
The objective is to develop a method for
determining when a waste is a reactive waste
(40 CPR 261.33) by reason of potential H2S or
HCN release. A method has been evaluated
using standards and actual waste samples.
Tie test method is expected to be available for
Regional review and cotncaent by June of 1984.
Work is also progressing on establishing
reactive waste definition thresholds using
the oethod. while it looks like it works
acceptably woll for sulfide-boaring wastes,
further method refining will be necessary
before it can bo adopted for cyanides.
Haste Analysis Plans Guidance Manual
Under Section 3004 of RCRA, EPA promulgated standards
applicable to owners and operators of hazardous waste management
facilities. These standards govern the issuance of permits
for facilities that treat, store, or dispose of hazardous
waste. OSW is currently developing permit Guidance Manuals
to describe the permit application process and to provide
guidance to applicants and permit writers in addressing the
information requirements.
As part of the permit application, owners/operators aro
required to submit a Waste Analysis Plan. The requirement
for a Waste Analysis Plan is to insure that owners or operators
possess sufficient information on the properties of wastes
so that they will be able to treat, store, or dispose of the
waste in a manner which will not pose a threat to human
health or the environment.
To assist permit applicants and State and EPA staff ~~^
members who review applications and draw up periaits, the
Office of Solid Waste is in the process of preparing a Waste
Analysis Plan Guidance Manual. This Manual will provide
specific guidance on how to comply with the general waste
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analysis requirements of 40 CFR 264.13. The Manual will
include a discussion of the Wasta Analysis Plan requirements,
model waste Analysis Plans for each of the principal waste
disposal management situations, and'a checklist for reviewers
to use in evaluating permit applications. We anticipate .
that a draft of this manual will be available for Regional
review early in Spring 1984. ' .."
* *
Reference Standards • •
Since 1930, EPA1a Office of Research and Development
has maintained and continues to expand an inventory of standard
compounds for use in analytical efforts.
Organic standards consist of either s ingle-component
solutions (for instrunent calibration) or raulti-conponent
solutions, containing several chomicals. Analytical reference
standards can be utilized in several ways to enhance sample
analysis and quality control. Reference standards can bet
' • added tso media before analysis to check recoveries
and thus bo used as .3 matrix spike;
* added to a sample which has been prepared for
instrumental analysis, and thus be used as an internal
standard;
• used as a surrogate for a particular compound allowing
for both sample analysis and recovery verification to
be done in the sama run, e.g., deuterated or fluorinated
standards can thus bo used as surrogates for compounds
found in hazardous waste.
• used for instrunent calibration.
A single source of standard chemicals of known purity
and reference materials is necessary to assure that data of
known quality are produced. The Quality Assurance Materials
Bank provides reference standards to analytical laboratories
to support the Agency's pro j rams for no ni to ring hazardous
waste (RCRA/ CERCLA). Pure ("neat") compounds ara- purchased
and analyzed and low purity compounds are purified. Once
verified, high purity organic and inorganic standards are
prepared (standard solutions) and distributed for use by
laboratories in calibration of instruments and for quality
control in sample analysis. The purity, concentration,
stability and applicability of each standard is evaluated by
the QA Materials Bank. For information regarding the availability
of specific standards contact Ed Kantor at BMSL-LV (702-798-2690j
PTS545-2690), Ed Berg at EMSL-Cinn (513-684-7325; FTS-684-7325),
or Florence Richardson at the office of Solid Waste (202-382-4301;
FTS-382-4801). ~' '
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