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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