United States Prevention, Pesticides EPA712-C-96-022
Environmental Protection and Toxic Substances August 1996
Agency (7101)
&EPA Product Properties
Test Guidelines
OPPTS 830.6313
Stability to Normal and
Elevated Temperature,
Metals, and Metal Ions
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INTRODUCTION
This guideline is one of a series of test guidelines that have been
developed by the Office of Prevention, Pesticides and Toxic Substances,
United States Environmental Protection Agency for use in the testing of
pesticides and toxic substances, and the development of test data that must
be submitted to the Agency for review under Federal regulations.
The Office of Prevention, Pesticides and Toxic Substances (OPPTS)
has developed this guideline through a process of harmonization that
blended the testing guidance and requirements that existed in the Office
of Pollution Prevention and Toxics (OPPT) and appeared in Title 40,
Chapter I, Subchapter R of the Code of Federal Regulations (CFR), the
Office of Pesticide Programs (OPP) which appeared in publications of the
National Technical Information Service (NTIS) and the guidelines pub-
lished by the Organization for Economic Cooperation and Development
(OECD).
The purpose of harmonizing these guidelines into a single set of
OPPTS guidelines is to minimize variations among the testing procedures
that must be performed to meet the data requirements of the U. S. Environ-
mental Protection Agency under the Toxic Substances Control Act (15
U.S.C. 2601) and the Federal Insecticide, Fungicide and Rodenticide Act
(7U.S.C. I36,etseq.).
Final Guideline Release: This document is available from the U.S.
Government Printing Office, Washington, DC 20402 on The Federal Bul-
letin Board. By modem dial 202-512-1387, telnet and ftp:
fedbbs.access.gpo.gov (IP 162.140.64.19), internet: http://
fedbbs.access.gpo.gov, or call 202-512-0132 for disks or paper copies.
This guideline is available in ASCII and PDF (portable document format)
from the EPA Public Access Gopher (gopher.epa.gov) under the heading
"Environmental Test Methods and Guidelines."
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OPPTS 830.6313 Stability to normal and elevated temperature, met-
als, and metal ions.
(a) Scope—(1) Applicability. This guideline is intended to meet test-
ing requirements of the Federal Insecticide, Fungicide, and Rodenticide
Act (FIFRA) (7 U.S.C. 136, et seq.).
(2) Background. The source material used in developing this har-
monized OPPTS test guideline is OPP guideline 63-13 Stability (Pesticide
Assessment Guidelines, Subdivision D: Product Chemistry, EPA Report
540/9-82-018, October 1982) and 40 CFR 158.190 Physical and chemical
characteristics.
(b) Test method—(1) Objective, (i) Data on the physical and chemi-
cal characteristics of pesticide active ingredients and products are used
to confirm or provide supportive information on their identity. Such data
are also used in reviewing the production or formulating process used to
produce the pesticide or product.
(ii) The objective of this guideline is to determine how stable the
active ingredient is in the presence of normal and elevated temperatures,
metals, and metal ions. Data regarding stability to metal and metal ions
is required only if there is a likelihood that the technical grade of the
active ingredient (TGAI) will come into contact with metals during its
storage and use.
(2) Test details, (i) In order to fully characterize the stability of the
pesticide chemical, standard methods may be used. Subjective judgements
by a chemist familiar with the chemical and its intended use are needed
in selecting appropriate tests.
(ii) The agency recommends the CIPAC method "MT 46 Accelerated
Storage Tests by Heating" to determine stability of a pesticide when sub-
jected to elevated temperature (see paragraph (d)(l) of this guideline).
(A) Test procedure. Dispersible powders: A 20 g sample of the pes-
ticide is placed in a beaker and spread in a smooth even layer of constant
thickness. A plastic coated metal disk of the approximate diameter of the
beaker is placed on top of the sample and the beaker is placed in an oven.
The sample is maintained in the oven at 54 °C for 14 days. Upon removal
from the oven, the specimen is allowed to cool in a dessicator without
dessicant and samples of the hard cake are submitted for appropriate test-
ing and analysis.
(B) [Reserved]
(iii) To determine stability in the presence of metals and metal ions,
the following test method is recommended.
(A) Test method. A fine metal is typically uniformly dispersed in
a solid mixture or sunk in liquid formulations and analyzed for active in-
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gredient at time 0 and after 14 days of exposure; or by differential scan-
ning calorimetry/differential thermal analysis (DSC/DTA) by comparison
to a non-exposed test sample. Two metals in their natural state and in
their ionic form are typically tested. Oven testing is usually periodic, typi-
cally analyzing after 1, 2, 7 and 14 days of exposure to collect more than
single point data for exposure to each material. Typically the metal and
salt of a weak acid, such as an acetate or carbonate (e.g., iron filings and
ferric acetate, aluminum rods and aluminum acetate, lead shot and lead
acetate) are used. Since exposure to metals is usually of short duration,
especially if reactive, testing at ambient temperature can be used as a con-
trol, as measured against elevated temperature.
(B) [Reserved]
(iv) Consultation with the Agency is recommended if there are ques-
tions about appropriate methods for the other determinations.
(v) If an alternative method is used, it is recommended that the reg-
istrant consult with the Agency prior to adopting the test method.
(c) Reporting. (1) Descriptions and results of all tests should be re-
ported. The information on stability shall include consideration and discus-
sion of the sensitivity of the active ingredient to metals and metal ions
it may come in contact with, at normal and elevated temperatures.
(2) Any methods used to characterize the physical properties of a
pesticide shall be referenced or described in the application for registration.
If the methods used are listed in this guideline, reference to the method
will suffice. If other methods are used, copies of such methods must be
submitted with the application.
(3) References denoting "CIPAC" refer to standardized methods of
the Collaborative International Pesticide Analytical Council, Ltd., Hatching
Green, Harpenden, Hertfordshire, England.
(4) The applicant shall submit his own statistical evaluation of the
precision and accuracy of these measurements (e.g., standard deviations
or confidence intervals) when appropriate.
(d) References. The following references should be consulted for ad-
ditional background material on this test guideline.
(1) Collaborative International Pesticide Analytical Council Ltd.
(CIPAC) Handbook, "MT 46 Accelerated Storage Tests by Heating,"
CIPAC, Hatching Green, Harpenden, Hertfordshire, England (1970).
(2) [Reserved]
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