vvEPA
United States
Environmental Protection
Agency
Prevention, Pesticides
And Toxic Substances
(7508W)
EPA738-R-95-011
April 1995
Pesticide Reregistration
Rejection Rate Analysis
Environmental Fate
Follow-up Guidance for:
Submission of Raw Data
Recycled/Recyclable • Printed with Vegetable Oil Based Inks on 100% Recycled Paper (JiO% Postconsumer)
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f Guidance on Submission of Raw Data
Raw data, in the sense used here, are not the detailed laboratory
records required for a GLP audit. The "raw data1!1 required for an
EFGWB review is the uninterpreted factual information that formed
the basis for the study report. Enough data should be provided so
that the EFGWB reviewer is able to understand how the experiment
was performed and reconstruct the development of the study results.
As pointed out in the Environmental Fate "Rejection Rate Analysis"
document, the need for additional raw data does not normally result
in the rejection of a study, and is usually corrected by the
submission of the required data. It is generally most efficient to
provide a well-organized presentation of all potentially necessary
data, rather than respond to requests for data during the study
review. The data requirements listed below may not apply to all
reviewers or all studies, but should provide a general outline of
the kind of information necessary in order to make a reliable data
evaluation.
General
Data presenting results from soil and/or water physicochemical
characterization.
Data supporting the nominal test substance application rate,
with calculations, where applicable.
All dates (not just intervals) associated with the study: site
preparation, test substance preparation, dosing or
application, sampling, extraction, analysis, etc. Tabulation
with calculated intervals would be helpful.
The registrant should ensure that description of any
referenced SOP's or standard methods must be| available to the
Agency at the time of the review. If these SOP's have been
previously submitted to the Agency, the registrant may
reference the documents by MRID or Accession number.
Information on reference substance characterization (as
required by GLP's).
Techniques used for preparation of aliquots or subsamples.
If automated data calculation methods are usied, some
discussion/examples of the calculation techniques, such as
spreadsheet formulae, calculation parameters from a commercial
system, etc.
The quantitative data which form the basis for calculating the
reported concentrations of radioactivity in
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radioactivity may be verified. Data should be provided 'for
control and treated samples. Background data for solvents
should be included as well.
Supporting chromatograms, mass spectra, NMR spectra, IR
spectra, UV-Vis spectra, and any other data used to
characterize or identify degradation products. This would
include chromatograms or spectra which demonstrate the
absence of any proposed metabolites.
Quantitative data associated with chromatograms,
autoradiograms, spectra, etc., so quantitative assessment of
metabolite identification can be confirmed. This would
include the amount of radioactivity (in dpm) used in the
analysis and the amount recovered. A complete set of sample
calculations should be included with formulae and variables
defined in generally understood terms, using data from the
submitted report.
Chromatograms of standards and controls.
Information on sample storage including conditions, sample
form (extract or homogenized) and sample container. Often a
range of temperatures is provided, which account for
temperature spikes; information should also be included about
the condition of samples during temperature spikes. Reports
should detail how samples are handled and stored prior to
receipt by the analyzing lab. In particular, the time
between taking the sample and freezing the sample should be
reported.
Analytical methods
Schematic diagram(s) of the analytical approach for the
separation, identification, and quantitation of the test
substance and its degradates.
Supporting validation data associated with all methods
submitted for each matrix (soil, water, air, biological
tissue, etc.). This would include not only final results
but also sample weights, extraction volumes, final volume
of extracts, peak heights/areas, injection volumes, and any
other data which would allow the reviewer to reproduce the
results. These data can be summarized in a table, and may
be reported along with analytical data for treated samples.
Chromatograms for each matrix of interest at all spiking
levels, including the claimed limit of quantitation. A
minimum of ten chromatograms is suggested for each matrix
including both spiked and control samples, particularly in
those instances where tolerances are proposed at or near
the limit of quantitation. There is a need for control and
method blank chromatograms so reviewers can assess the
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reported limits of detection and quant itat ion.
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provided. If there are more than 10 samples, at least 10
chromatograms should be provided. «PAe*, at least 10
A minimum of three chromatograms each of control and fortiori
samples in order to assess the limit of wntita?fon? d
A sample calculation should be presented wh<-re a treats
sample and fortified control are taken through ?he Int ire
a°n £r°Cedure- A reviewer should be Ible to ?ie ?his
t0 ' Chr°mato^am «* quantitative data° included
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corrected values are reported for trea?ed sampfls* thfn
apparent values should be reported as well? P'
Notes on any technical communications between the studv
'JUSH^ ?°teS °n the difficulties of the method and
modifications to facilitate method implementation?
All appropriate manufacturer and lot numbers if or
chromatography columns, chemicals, and equipment.
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Field data
Field notes and/or reports on application, harvest, plot
preparation and maintenance.
Procedure and results for calibration of application
equipment.
A specific description as to how and where (within the field
plot) samples were taken. What was done to insure that the
sample was representative?
Daily wind, rain, and temperature data is required to
determine the relationship between environmental conditions
and pesticide dissipation.
Irrigation data, including date, quantity, and application
method is required.
Soil series of test plots, with SCS description of a typical
profile for that soil type.
Description of terrain, including percentage and direction of
slope, and depth to the water table.
Additional considerations
No data should be included from analyses aborted due to
equipment failure or other circumstances. The registrant is
required to keep such data in accordance with GLP standards,
but such data should not be submitted with the final study
report.
Information should be provided in a manner which is complete
and legible. It should be organized so that the reviewer can
easily find the desired information, and not have to look in
many different places in a report to find the dates or
analytical results.
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