UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
REGION III
841 Chestnut Bundling
Philadelphia, Pennsylvania 19107
SUBJECT: Region 3 Superfund Data Validation DATE: MUU • 6 ^95
Policy1 -
FROM: Abe Ferdas, Associate Director /^b<£~'\^'
Office of Superfund Programs (3HW02)
TO: Superfund Program Staff
Purpose:
The Environmental Protection Agency makes consequential
decisions regarding public health and environmental conditions.
Analytical data are the cornerstone of this Agency's decision
making processes. Thus, it is imperative that the data used in
these processes be of known and documented quality. The quality
of analytical data is determined through the data validation
process. Specifically, data validation is a systematic procedure
for reviewing analytical data against a set of established
criteria to determine its validity relative to the data's
intended use. The purpose of this memo is to clearly define this
Region's data validation policy for the Superfund program.
Background:
Each environmental data collection activity is different due
to elements of variability which include site history, project
objectives, and the amount of historical data available. The.
Site-specific procedures for data validation are specified in the
individual Sampling and Analysis Plans developed for each site.
Organizations performing environmental data collection activities
should specify data validation requirements. These requirements
should adequately support the intended use of the data.
1 This policy and the procedures set out in this document
are intended for the use of U.S. EPA response personnel. EPA
reserves the right to change this Policy at any time, without
prior notice, or to act at variance with this policy. This
policy does not create any rights, duties or obligations, implied
or otherwise, in any third parties.
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Implementation:
Data review/validation procedures for this Region are
delineate'd in:
• Region III Modifications to the National Functional Guidelines
for Organic Data Review
• Region III Modifications to the Laboratory Data Validation
Functional Guidelines for Evaluating Inorganic Analyses.
These procedures provide the reader with instructions on how to
perform a full data validation.
EPA Region III advocates full data review/data validation to
support quantitative Superfund Baseline Risk Assessments. This
data validation is performed by an independent party other than
the laboratory that generates the analytical data. The
validation is performed on all (100%) of the data. The
appropriate qualifiers should be applied to 100% of the data.
There are various EPA national guidance documents that
address the objectives for data review/validation. Risk
Assessment Guidance for Superfund. Volume 1 and the Guidance for
Data Useability in Risk Assessment include discussions of data
quality as a function of data use. For quantitative risk
assessment, EPA National Guidelines indicate a preference for
full data review.
For uses of data other than quantitative baseline risk
assessment, the degree or intensity of data validation may vary
based upon the intended use of the data. Region Ill's
"Innovative Approaches to Data Validation" supports this concept.
The Region's primary goal is to verify that the data quality
produced is adequate for the intended data use. The "Innovative
Approaches to Data Validation" defines levels of data review
which are based on how data are to be used. Each review level
contains data validation evaluation criteria which support the
data use category. However, it is important to note that under
all circumstances the following conditions should be met:
• The analytical deliverable requirement must contain all of
the documentation listed in Appendix A of this memorandum.
• Data qualifiers are applied to 100% of the data in all
cases.
• All data used to support quantitative baseline risk
assessment should be reviewed using full Region III
data validation procedures.
The Region encourages dialogue between EPA and PRPs during
the scoping phase of a project to establish site-specific data
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quality objectives that will meet the needs of each data
collection activity. It should be emphasized that the scoping
phase of the remedial process is the best time to present and
discuss the data validation objectives of the project. An early
and comprehensive discussion of the data validation procedures of
the project will reduce the uncertainty during risk assessment.
The final decision regarding the appropriate level of review must
be approved by the EPA project manager.
Summary:
• Site specific data validation objectives are specified in the
sampling and analysis plan for each site.
• Region III advocates 100% data validation to support
any quantitative baseline risk assessment developed for the
Superfund program.
• For data uses other than quantitative baseline risk assessment,
Region III Innovative Approaches may be used with EPA project
manager approval.
• Data validation procedures are provided in the Regional
Guidelines as noted above.
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Appendix A
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The contents of a data validation package are as follows:
Narrative
The narrative describes and summarizes the results of the
analytical process. It is composed of:
Overview - Describes the sample set (e.g. number of samples,
matrices) and informs the user of the method of analysis.
summary - Provide* a synopsis of the sample analysis and
advises the user of any unsuccessful analyses.
Xajor issues - Presents issues which directly affect data
quality in an adverse manner. Kay include statements
regarding suspect and unusable data, or problems concerning
sample integrity.
Minor issues - Summarizes data qualifiers that have been
applied to positive values or quantitation limits and
informs tae user of the limitations of data use.
Attachments
Each report must have the following attachments:
Appendix A - Glossary of data qualifiers
Appendix B - Data Summary Forms (Regional data summary forms
are available from the Quality Assurance Branch.)
Appendix C - Results as reported by the laboratory (Form 1
or equivalent)
Appendix D - Results of all Tentatively Identified Compounds
which have been corrected to exclude blank contamination
(Organics only)
Appendix E - Support documentation which substantiates
qualifiers placed on data during review (i.e. method blanX
forms/ calibration forms, quantisation reports).
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Deliverables Listing
Metals Analyses
I. Chain of Custody
II. Narrative - Describe analyses performed and discuss any problems
associated with the data reported.
III. Sample Results (for each sample)
sample number
date received
matrix
% solids (for non-aqueous samples only)
concentration units
metal and determined concentration
IV. QC Data (for those QC samples required by the method used to
determine the metals analyzed for)
.'
0 Initial and Continuing Calibration Results
source of calibration standard(s)
concentration units
true value (for each analyte)
measured value (for each analyte)
percent recovery (for each analyte)
0 CRDL Standard Recoveries for AA and ICP. (These analyses are
required under the CLP protocols, other methods may or may
not require that a standard at or near the detection limit of the
instrument be analyzed to verify acceptable performance at that
concentration level. If the method does not require such an
analysis than this form is omitted.)
same as listed for initial and continuing calibration
0 Blanks
preparation blank matrix
instrument and preparation blank units
initial calibration blank results
continuing calibration blank results
preparation blank results
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ICP Interference Check Sample (only needed if any analytes are
determined by ICP methods)
ICP instrument ID (only if more than one ICP)
concentration units
true values (for each analyte and solution)
found values (for each analyte and solution)
percent recovery (for each analyte)
Matrix Spike Sample Recovery
matrix
concentration units
control limit
^ spike sample result
'unspiked sample result
amount of spike added
percent recovery
Post Digest Spike Sample Recovery. (These analyses are
required under the CLP protocols, other methods may or may
not require that a post digest spike sample analysis be
performed when the pre-digestion spike recovery is outside
acceptable limits. If the method does not require such an
analysis than this form is omitted)
same as for matrix spike recovery
Duplicates (note: for laboratory duplicate analysis results only)
matrix
percent solids for sample and duplicate (if non-aqueous
matrix)
concentration units
control limit
sample results
duplicate results
relative percent difference (% RPD)
Laboratory Control Sample
matrix
concentration units
true value
found value
percent recovery
control limits (if applicable)
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0 Method of Standard Addition Results (for each analyte result
determined by MSA)
sample no.
analyte
0 ADD ABS
1 ADD and ABS
2 ADD and ABS
3 ADD and ABS
final cone.
correlation coefficient
0 ICP Serial Dilutions (only if ICP methods were used)
matrix
concentration units
initial sample result
serial dilution result (corrected for dilution)
percent difference
0 Instrument Detection Limits
instrument ID's
wavelength
type of background correction
instrument detection limit
0 ICP Interelement Correction Factors (only if ICP methods were
used)
wavelength
correction factor by analyte/interfering analyte
0 ICP Linear Ranges (only if ICP methods were used)
V. Raw Data
For each reported value, the laboratory should include in the data
package all raw data from the instrument used to obtain the sample
values and the QA/QC values reported (except for raw data for
quarterly verifications of instrument parameters such as IDLs and
interelement correction factors). Raw data must contain all
instrument readouts used for the sample results, including those
readouts that may fall below the IDL. All AA and ICP instruments
should provide a legible hard copy of the direct real-time instrument
readout (i.e., stripcharts, printer tapes, etc.). A photocopy of the
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direct sequential instrument readout must be included. A hardcopy of
the direct instrument readout for cyanide should be included if the
instrumentation has the capability.
All raw data should include intensities (ICP) and absorbances (AA)
with concentration units (unless instrument direct readout is in
concentration units). All flame and furnace AA data should be
grouped by element.
To facilitate data validation, it is recommended that the raw data be
identified to identify the following:
0 Calibration standards, including source and prep date.
0 Initial and continuing calibration blanks and preparation blanks.
0 Initial and continuing calibration verification standards,
interference check samples, and ICP serial dilution samples.
0 Diluted and undiluted samples (by sample number) and all
weights, dilutions and volumes used to obtain the reported
values. (If the volumes, weights and dilutions are consistent
for all samples in a given data package, a general statement
outlining these parameters is sufficient).
0 Duplicates.
0 Spikes (indicating standard solutions used, final spike
concentrations, volumes involved). If spike information (source,
concentration, volume) is consistent for a given data package, a
general statement outlining these parameters is sufficient).
0 Instrument used, any instrument adjustments, data corrections
or other apparent anomalies on the measurement record,
including all data voided or data not used to obtain reported
values and a brief written explanation.
0 All information including date for furnace analysis clearly and
sequentially identified on the raw data, including sample
number, sample and analytical spike data, percent recovery,
coefficient of variation, full MSA data, MSA correlation
coefficient, slope and y intercept of linear fit, final sample
concentration (standard addition concentration), and type of
background correction used.
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0 Time and date of each analysis. Instrument run logs can be
submitted if they contain this information. If the instrument
does not automatically provide times of analysis, these should
be manually entered on all raw data for initial and continuing
calibration verification and blanks, as well as interference check
samples and linear range analysis.
0 Integration times for AA analyses.
VI. Digestion and Distillation Logs
Digestion and distillation logs for all samples analyzed should be
submitted. These logs should include: (1) date, (2) sample weights
and volumes, (3) sufficient information to unequivocally identify which
QC samples^i.e., laboratory control sample, preparation blank)
correspond to each batch digested, (4) comments describing any
significant sample changes or reactions which occur during
preparation, and (5) indication of pH <2 or >12, as applicable.
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Deliverables Listing
Organic Analyses
.1. Chain of Custody
II. Narrative - Describe analyses performed and discuss any problems
associated with the data reported.
III. Volatiles/Semi-Volatiles Data
QC Summary
- Surrogate Recovery Summary
- Matrix Spike/Matrix Spike Duplicate Recovery Summary
- Method Blank Summary (list associated samples for
each method blank)
- Tuning Summary for BFB and DFTPP .
in chronological order by instrument
Sample Data (for each sample)
- Form I (from Org. SOW) or Lab Generated Reports
header must include the following:
sample no.
date received
matrix
units.reported
amount of sample
date extracted (Semi-VOA only)
% Moisture (soils only)
pH (waters only)
. - Reconstructed Ion Chromatogram (RIC)
label internal and surrogate standards
normalize to highest non-solvent peak
header must include to following:
sample no.
date and time of injection
instrument ID
lab file ID
- Quantitation Reports
header must include:
same as for RIC
dilution factors
amount injected
- Compound Identification (for all compds. detected
except surrogates and internal standards)
- Raw mass spectra •
- background subtracted mass spectra1
- standard spectra , •
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Standards
- Initial Calibration Form
include:
date calibrated
time calibrated
applicable file IDs
response factors for each compound at each level
mean response factor
Percent Relative Standard Deviation (%RSD)
- RIC/Chromatogram and Quantitation report for each
standard in initial calibration
in chronological order by instrument
- Continuing Calibration Form
include:
date and time calibrated
mean response factor from initial calib.
response factor from continuing calib.
percent difference (%D)
*- Internal Standard Area Summary
in order by instrument
include:
continuing calib. internal standard areas
cont. calib. internal std. retention times
internal standard areas and retention times for
all samples quantitated against continuing calib,
Raw QC
- Tuning BFB/DFTPP ...
bar graph spectrum
mass listing
- Blank Data
- Form I or lab generated report forms
for each method blank
- RIC/Chromatogram
- Quantitation report
- Mass Spectrum of each positive result
(above same header as samples)
- Matrix Spike/Matrix Spike Duplicate Data
- Form I or lab generated report forms
- RIC/Chromatogram
- Quantitation report
- spectra not required
Copies of Sample Preparation/Extraction Logbooks
Run log/Injection logbook
11
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IV. Pesticide/PCB Data
QC Summary
- Surrogate Recovery Summary
- Method Blank Summary
- Matrix Spike/Matrix Spike Duplicate Recovery Summary
Sample Data
- Form I or lab generated report forms
- Chromatogram
header must include:
sample no.
volume injected
date and time of analysis
column
instrument identification
all positives labelled
- Confirmation Chromatogram (if applicable)
header same as above
- GC integration report
- GPC Chromatogram (if performed)
- GC/MS Spectra (if confirmation on GC/MS performed)
Standards Data
- Pesticide Evaluation Standards Summary
- Pesticide/PCB Standard Summary
include:
calibration factors
percent difference (%D) for continuing and initial
calib. ,
- Pest/PCB standards data
- Chromatogram and integration reports
in chronological order by instrument
label all peaks for individual compounds
list total ng injected
retention time and peak areas
date and time injected
GC column ID
GC instrument ID
ii-i
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Raw Data
Blank Data
- Form I or lab generated result form
- chromatogram
- integration reports
in chronological order
Matrix Spike/Matrix Spike Duplicate
- Form I or lab generated result form
- chromatogram
- integration reports
IV
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