oEPA
United St
Environmental Protection
Agency
Office of
Solid Warn and
Emergency Response
DIRECTIVE NUMBER: 9445.01(84)
TITLE: Notes on RCRA Methdds and Quality Assurance
Activities
APPROVAL DATE: 4-23-84
EFFECTIVE DATE: 4-23-84
ORIGINATING OFFICE: office of Solld Wa8te
Q FINAL
D DRAFT
STATUS:
1
REFERENCE (other documents):
A- Pending OMB approval
[ ] B- Pending AA-OSWER approval
[ ] C- For review 4/or coonent
[ ] D- In development or circulating
headquarters
OSWER OSWER OSWER
VE DIRECTIVE DIRECTIVE Dl
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PART 261 - APPENDICES DOC: 9445.01(84)
Key Words: Test Methods, QA/QC
Regulations:
Subject: Notes on RCRA Methods and Quality Assurance Activities
Addressee: N/A
Originator: David Friedman, Manager, Methods Program
Source Doc: #9445.01(84)
Date: 4-23-84
Summary:
The following topics were discussed:
Method 3030 - Acid Digestion of Oils, Greases, and Waxes
Region V's recovery data for oils spiked with organometallic standards (as
part of the Region's waste oil analysis) showed the spike recoveries were
unacceptable for barium, lead, mercury, and selenium. As a result of these and
other comments, the Methods Branch is considering modifications or adjustments
to the current methods and is considering methods from other sources in the
evaluation program.
Method 1310 EP Toxicity
If the maximum amount of 0.5N acetic acid is added to the extractor and
pH 5.0 _+ 0.2 is not reached, the 4 meg/gm maximum amount of acid specified is
controlling and no additional acid should be added to the system. Under such
conditions, the extraction is conducted at the pH reached after the maximum
amount of acid is added.
When the EP toxicity test is performed on oily or greasy samples that
cannot be filtered, it is permissible to heat these at a low temperature to
remove organics and then determine the metals present.
Materials that do not pass through the 0.45 um filter are considered solids,
irrespective of their liquid properties and must be extracted with the acetic
solution. Unlike an oil that passes through the filter, they are not considered
to be an extract.
pH of Oil and Grease
It is .impossible to determine the pH of non-aqueous materials. When the
material is multiphasic, containing both an oil and a water layer, the water
layer can be measured.
Method 3550
Results of method 3550 are to be reported, unless specifically stated in a
method, "as received" and the sample is not dried before analysis.
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9445.01 (84)
MEMORANDUM
SUBJECT: Notes en RCRA Methods and QA Activities
TO: Addressees
The response to my previous RCRA Methods and QA Activities
memo was very gratifying. We vary much appreciate the content.i
and suggestions that you sent us. In this memo I will address
some of the topics you suggested in your comments. The topics
to be discussed are:
• Delisting Spot-Check Program
* Performance Audit Program for Volatile POHC
• Method 3030 - Acid Digestion of Oils, Greasos and Waxes
• EP Toxicity - pH Adjustment
• Method 3550 - Sonication extraction
0 pH of Oil/Grease
Delisttng Spot-Check Program
OSW has a program, which is approximately a year.old
now, in which unannounced visits are made to facilities that
have submitted delisting petitions. Included in these visits
are both on-site waste management facilities and commercial,
off-site, multiple wasto treatment facllitlos.
"" * * « - _ • ~"
The purpose of the spot-check program is to collect
representative samples of the material being nan^gnd in
order to verify data submittad in the facility's dolisting
petition/ and, if appropriate, to Inspect the treatment
process and ensure that exclusion contingencies are being
observed.
A total of elavon visits have been made (one to Region
I, two to Region II and four each to Regions III and V). As
a result of the inspections, recommendations wore made to deny
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—petit-ions subtnrtted^by three "of the" facilities. In some
cases, recommendations to the Regions for enforcement action
resulted from those checks.
*f
The spot-check program will continue with trips planned
to Regions IV,V, and VII by late spring. Both tha Regional
^ffice and the appropriate Stata office are notified and
nvited to accompany the OSW team on these visits.
<•
Performance Audit Program for Volatile POHC
EMSL-RT? has prepared standard cylinders of organic
substances in nitrogen in support ot" the OAQPS and RCRA -nonitorimj
programs. Each cylinder contains tha following five organic
compounds: carbon tefcrachloride, chloroform, porchloroethylene,
vinyl chloride and benzene. Some cylinders have compound
concentrations in the range of 7 to 90 ppb suitable for
auditing the VOST and others are in the range of 90 to 430
ppb and suitable for auditing a bag sampler.
While it is presently not required, OSW is considering the
implementation of a performance audit program that would require
source test measurements during all hazardous waste trial
burns. Since EMSL-RTP is already in a position to conduct
audits of VOST and bag sampling operations, we recommend
that Regional permit and BSD personnel immediately begin to
require use of the RTP audit cylinders during all sourco
measurement programs.
4
Please direct all requests for audits to Florence Richardson
f my staff. She will record tha requests and forward the™
^ EMSL-RT? for scheduling.. This will permit us to determine
the future resource implications of such a requirement. We
would also appreciato any suggestions that you nay have for
implementing the program.
Method 3030 - Acid Digestion of Oils, Greases and Waxes
Region V has initiated analyses of waste oils to determine
their hazardous characteristics, and the determination of
metals is one of the principal waste oil analyses of interest.
The lead and barium contents of waste oil are important
because of their use as gasoline additives.
Prior to the metals' analyses, recovery data for oils
s'piked with organometallic standards w*sre collected. The
spik« recoveries were definitely unacceptable for barium,
lead, mercury and selenium.
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We appreciate Region V bringing this problem to our
attention, EMSL-Cinn is currently evaluating all of the SW-84S
digestion methods. In response to comments such as these,
we are considering modifications or adjustments to the current
methods and also methods from other sources in the evaluation
program. The report on the evaluation of this method is
scheduled to be prepared and available for review by July, 1934.
Method 1310 EP Toxicity
One question frequently asked is "What is the procedure to
use if the maximum amount of 0.5N acetic acid has been
added to the extractor and pH 5,0 £ 0.2 has not been reached?"
* In such a case the 4 raeq/gm maximum amount of acid specified
is controlling and no additional acid should be added to the
system. Under such conditions the extraction is conducted
at the pH reached after the maximum amount of acid is
"Also, when the EP toxicity test Is performed on oily or
greasy samples that cannot be filtered; ia it permissible
to heat these at low temperature to remove organics and then
determine the metals present."
• Materials that do not pass the 0.45 urn filter are considered
as solids, irrespective of their' liquid properties, and
thus must be extracted with the acetic acid solution. They
are not considered to be an extract as would an oil that
passes through the filter.
pH of Oil and Grease
*• ~ . * . .
., Another question that is often raised deals with how to
measure the pB of oily materials.
w '• ' '
It ia impossible to determine the pH of non-aqueous
materials. In cases where the material is multiphasic,
containing both an oil and a water layer, the water
layer can measured.
Clarification of Method 3550
"A laboratory inquired about method 3550 and wanted to
-know if the results were to ba reported in dry weight.
"This methods states 'a weighed sample of solid waste is
ground, etc., etc.' The sample referred to is the 'as
received material1 not a dried portion."
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Unless specifically stated in a method, results are to
be reported "as received" and th* sample is not dried
before analysis.
NOTE
ORD provides vital OA support to th« P.OA program through
a nunber oc laboratories. From ti^e to ti^ I thought it night
he worthwhile to highlight these laboratories and describe some
of the support they provide. In tM - -rjr.o /o will ai^aii^ht
Quality Asauranco ac £M3L-Cinn, BMSL-LV and EMSL-RTP.
The BMSL-Cinn QAB staff is headed up by John A. Winter with
Harold Clements and Ed Berg as section chiefs. They are
responsible for preparing and distributing certain types of
laboratory performance evaluation samples, quality control
samples and reference materials. They also maintain and operate
the BPA repository of toxic and hazardous materials and thus
are responsible for distributing analytical standards to
laboratories performing RCRA testing. The repository of
calibration standards have been verified by multiple laboratory
analyses as to percent purity of the neat compounds ami-
concentration oc solutions in the sealed ampules.
Responsibility for developing and distributing non-aqueous
Ktandard reference materials, maintaining the Quality Assurance
iterials Bank, evaluation of biological testing methods an«1
development of leaching procedures is with EHSL-LV. Compounds
in tho bank are not calibration standards but are of various
levels of purity and nay or may not have been fully verified
Gareth Pearson ia the Branch Chief. Llew Williams is the
Project Leader for the Ames autagenlcity and daphnia raagna
bioassay projects and for development of the second
generation Extraction Procedure. These activities will be
discussed in a future memo.
BMSL-RTP provides QA roaterials and conducts audits of
laboratories dealing with airborne or gaseous sampling and
analysis. As previously stated in this merao EMSL-RTP provides
cylinders of standard gases for ensuring the measurement of
organic compounds in trial burns and/or landfills. Darryl von
Lehroden heads up this OA effort.
Onco again let me thank you for your interest and
please keep sending us your comments and ideas for future
roonos. •'..--'-' - - . - •. .-...••-
David Fricdraan
Manager
May 1984 . . . Methods Program
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