PB83-153981
PESTICIDE ASSESSMENT GUIDELINES, SUBDIVISION O:
RESIDUE CHEMISTRY "" " -
Office of Pesticides Programs
Washington, D. C.
OCT 82
U.S. .DEPARTMENT OF COMMERCE
National Technical Information Service
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PB83t-153981
EPA San/Q-B?-n?3
October, 1982
PESTICIDE ASSESSMENT GUIDELINES
SUBDIVISION O
RESIDUE CHEMISTRY
by
Richard D. Schmitt, Ph.D.
Hazard Evaluation Division
Office of Pesticide Programs
Guidelines Coordinator
Robert K. Hitch
Hazard Evaluation Division
Office of Pesticide Programs
U.S. Environmental Protection Agency
Office of Pesticide and Toxic Substances
Washington, D.C. 20460
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REPORT DOCUMENTATION 1
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SUBDIVISION O: RESIDUE CHEMISTRY
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October, 1982
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Richard Schrmtt, et. al
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Office of Pesticides Programs
U.S. Environmental Protection Agency
Washington, D.C. 20460
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, 11 C o t ' r a c • (C1 or C.r^^
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12 Sponsoring Organization Nim« and Address
Office of Pesticide Programs
U.S. Environmental Protection Agency
Washington, D.C. 20460
(C)
13 Typ*- of Report <\ Pcf.oiJ Cov(f Identifiers/Open Ended Terms
c COSATl Field/Group
IB. Availability Statement
19 Security Class (This Report)
j 21 No of Pages
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20 Security Class (This Page)
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(See ANSi-239 '8)
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OPTIONAL fOflu 272 (<-;?)
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Foreword
Subdivision 0 describes protocols which may be used to perform food,
feed, or tobacco residue testing to support the registration of pesticides
under the Federal Food, Drug, and Cosmetic Act (FFDCA) and Federal
Insecticide, Fungicide and Rodenticide Act (FIFRA). These data are used
to estimate the exposure of the general population to residues in food
and to establish and enforce tolerances for pesticide residues in food
and feed.
Subdivision 0 is a non-regulatory companion to 40 CFR Part 158, Data
Requirements for Registration. References to requirements established in
40 CFR Part 158 are presented in Subdivision O so that this document can
be read as a complete package and so that the protocols may be explained
in their proper context.
II
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SUBDIVISION O
RESIDUE CHEMISTRY GUIDELINES
Table of Contents
Page
§170-1 Scope of Data Requirements 1
(a) General 1
(b) Petitions for tolerance 1
(c) Minor changes in use pattern 1
(d) Food use/Non-food use determinations 1
(e) Tobacco uses 2
(f) Aquatic uses 2
§171-1 List of requirements 2
§171-2 Chemical Identity 3
(a) Active Ingredient 3
(b) Inert Ingredient 4
§171-3 Directions for Use 4
(a) Application directions 4
(1) Field and orchard crops.... 4
(2) Animal treatments 5
(3) Fumigants '. 5
(4) Aquatic uses 6
(5) Foreign uses 6
(6) Food handling establishments 7
(7) Agricultural premises 7
(8) Miscellaneous applications 8
(b) Restrictions 8
§171-4 Results of tests on the amount of residue remaining.. 9
(a) Nature of the residue 9
(1) Characterization of the total terminal
residue 10
(2) Nature of the residue in plants 11
(3) Nature of the residue in livestock 12
(b) Analytical methods 13
(1) General requirements 13
(2) Validation of method by petitioner 14
(3) Extraction efficiency 14
(4) Determination of the total toxic residue 15
(5) Requirements for regulatory methods 16
(c) Magnitude of the residue 17
(1) General Considerations 17
(i) Residues determined 18
(ii) Sampling 18
(2) Design of residue experiments 19
(i) Field studies 19
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(ii) Fumigation uses 20
(iii) Slow release encapsulated formulation
uses 20
(iv) Processed food/feed studies 21
(3) Meat, milk poultry and egg feeding studies 22
(i) Residues in feed items 22
(ii) Direct animal treatment 24
(iii) Agricultural premise use studies 24
(4) Potable water, fish and irrigated crop
studies 25
(5) Food handling establishment uses................ 27
§171-5 Practical methods for removing residues that exceed
the tolerance 30
§171-6 Proposed tolerances 30
§171-7 Reasonable grounds in support of the petition... 31
§171-8 Exemptions from the requirement of a tolerance 31
(a) Active ingredients 31
(b) Inert ingredients 31
§171-9 Tolerances for foreign uses 32
§171-10 Rotational crop tolerances 32
§171-11 Tobacco uses 33
§171-12 Food use/non-food use determination data requirements... 34
(a) Seed treatments 34
(b) Crops grown for seed only 35
(c) Fallow land............ 35
(d) Non-bearing crop uses 35
§171-13 Submittal of Analytical Reference Standards 36
§171-14 Special considerations for temporary tolerance
petitions 36
§171-15 Presentation of residue data 37
§171-16 Translation of data 37
Table I. Categories and representative types of food
establishments.
Table II. RAC's, processed commodities, feeds and per-
cents of livestock diets for all crops.
/V
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SUBDIVISION O - § 170 RESIDUE CHEMISTRY GUIDELINES
§ 170- 1 Scope of Data Requirements
(a) General. Sections of this subdivision describe the
residue chemistry data requirements specified by 40 era Part 158
and the Federal Food, Drug and Cosmetic Act (FFDCA) and some other
information needed for pesticide uses that may result in residues
in food, feed or tobacco. Residue chemistry data are used by the
Agency to estimate the exposure of the general population to pesti-
cide residues in food, and for setting and enforcing tolerances
for pesticide residues in food or feed.
(b) Petitions for Tolerance. Residue chemistry data for a new
use of a pesticide are generally submitted to the Agency in a peti-
tion for tolerance as required under Sections 408 or 409 of the
Federal Food, Drug and Cosmetic Act (FFDCA). The format, procedures
and fees associated with petitions for tolerance are included in
Sections 408 and 409 of the FFDCA, and in sections 180. 1 to 180.35
of the Code of Federal Regulations (CFR) , Title 40.
(c) Minor Changes in Use Pattern. If a minor change in the
use pattern or formulation of a currently registered pesticide is
requested, the registrant may have to submit additional residue
data to demonstrate that the change will not result in residues
exceeding the established tolerance. Examples of changes in pesti-
cide use patterns that are likely to require residue studies, and
possibly another petition for a new tolerance, include: ( 1) signifi-
cant changes in preharvest interval and in postharvest treatment;
(2) extension of use patterns to include low volume or ultra low
volume (ULV) aerial as well as ground application; (3) alteration
of use patterns to include new types of usage; (4) addition of a
sticker or extender to the formulation; (5) conversion to a slow-
release formulation; (6) use in additional climatic regions; (7)
an increase in the application rate; and (8) an increase in the
number of applications allowed.
Examples of minor changes that may not require residue studies
include: ( 1) a change in surfactant concentration; (2) substitution
of a new but similar surfactant; (3) substitution of one clay
diluent for another. Exceptions must be made individually based on
a thorough knowledge of the chemistry of the ingredients involved.
Residue data in support of a changed use pattern are normally
submitted to the Agency under the Federal Insecticide, Fungicide
and Rodenticide Act (FIFRA) in a form described in CFR 40, Section
162.
(d) Food Use/Non-Food Use Determinations. The term "food"
is defined in Section 20 1(f) of the FFDCA as ( 1) articles used for
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food or drink for man or other animals, (2) chewing gum, and (3)
articles used for components of any such articles. If a pesticide
use is likely to result in residues on food, then the use is a food
use, a petition for tolerance or exemption is required, and appro-
priate residue chemistry considerations apply. Non-food uses are
those uses that are not likely to yield residues in food. Uses
that could result in residues in meat, milk, poultry or eggs are
also considered to be food uses.
(e) Tobacco Uses. Use of a pesticide on tobacco does not
require a tolerance or an exemption from the requirement to obtain
a tolerance. Nonetheless, data are needed to assess the exposure
of man to residues on tobacco. The residue chemistry data require-
ments for tobacco uses are described in this subdivision and such
data should be submitted to the Agency using the procedures for
submitting data under FIFRA referred to above.
(f) Aquatic Uses. When a pesticide is applied directly to
water, data on potential residues in potable water, fish and '
irrigated crops will be required. Tolerances are not established
for potable water, thus data on residues in water are submitted
under FIFRA.* Residue limits for potable water will be established
under the auspices of the Safe Drinking Water Act (SDWA) when
appropriate. Tolerances for fish and/or irrigated crops will be
established if appropriate. Thus, if a pesticide is to be applied
directly to water, data on residues in fish and/or irrigated crops
should be submitted in the form of a petition for tolerance or
exemption from tolerance under the FFDCA.
§171-1 List of Requirements« The sections of this subdivision
specifying the residue chemistry information and data requirements
are as follows:
§171-2 Chemical Identity. (Section A of a petition)
§171-3 Directions for Use. (Section B of a petition)
§171-4 Results of Tests on the Amount of Residue Remaining,
Including a Description of the Analytical Methods
Used. (Section D of a petition)
(a) Nature of the residue in plants and livestock
(b) Analytical methods
(c) Magnitude of the residue
~Federal Register, Vol. 47, No. 115, Tuesday, June 15, 1982, page
25746, Pesticides Applied to Bodies of Water, Proposed Procedural
Changes.
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(1) General considerations
(2) Design of residue experiments
(3) Meat, milk, poultry and eggs
(4) Potable water, fish and irrigated crops
(5) Food handling establishment uses
§171-5 Practical Methods for Removing the Residue. (Section E
of a petition)
§171-6 Proposed Tolerances* (Section F of a petition)
§171-7 Reasonable Grounds in Support of the Petition. (Section
G of a petition)
§171-8 Exemptions from the requirement of a tolerance.
(a) Active Ingredients
(b) Inert Ingredients
§171-9 Tolerances for Foreign Uses.
§171-10 Rotational Crop Tolerances.
§171-11 Tobacco Uses.
§171-12 Food Use/Non Food Use Determinations.
(a) Seed treatments
(b) Crops grown for seed
(c) Fallow land
(d) Dormant crop uses
§171-13 Submittal of Analytical Reference Standards.
§171-14 Temporary Tolerance Petitions.
§171-15 Presentation of Data.
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addition to these data required in the Product Chemistry Subdivi-
sion, Section A of the petition should include an assessment of
whether any of the impurities will present a residue problem.
an impurity is likely to occur as a significant residue in food/,
feed, then residue data for the impurity as described in Section
171-4, Section D of a petition, will be required. The determin-
ation of whether residue data for an impurity is needed will be
based on the impurity stability, toxicity and detectability.
(b) Information Required for Inert Ingredients. Inert
ingredients of the formulation should be fully described, including
the chemical as well as any trade names. Chemical abstract numbers
(CAS) should be included if available. The chemical names should
be in the same form as those for inert ingredients cleared under 40
CFR 180.1001 (c), (d) and (e). If only the trade name is known,
the petitioner should request that the supplier of the inert
ingredient furnish the descriptive information on the nature of the
inert ingredient directly to th~ Environmental Protection Agency.
Any inert ingredient that has not yet been cleared should be
indicated, and a request for clearance initiated as described in
Section 171 8 (b).
§171-3 Directions for Use. (Section B of a petition)
The directions for use are ordinarily contained in specimen
labeling submitted concurrently for registration under the Federal
Insecticide, Fungicide and Rodenticide Act (FIFRA). Labeling means
the actual label affixed to the container together with circulars
or leaflets that may accompany it.
It is important that the proposed use be described concisely
to facilitate correlation of the proposed use patterns with the
method of application used to obtain residue data. The directions
should be stated so as to be readily understood by the user of the
product. Where several products or multiple uses are involved in
the petition, it is suggested that Section B should contain a
summary table of all the uses relating to the proposed tolerance(s).
This table should show the crop, dosage range, schedule of
applications, formulations to be used, preharvest interval and all
other use relevant use limitations.
The following additional points should be observed in specifying
the directions for use in adequate detail:
(a) Application directions.
(1) Field and orchard crops.
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Application of dusts, sprays, and granular formulations
should be expressed in terms of pounds active ingredient per acre.
For band or row treatments, it should be clearly stated whether the
lbs/A rate refers to the area treated or the entire field. In the
case of full coverage sprays, as for orchards, the dosage should
also be expressed as pounds active ingredient per 100 gallons spray
solution to runoff, because of the large variation in the number of
pounds per acre needed for small trees versus large trees. The
quantity of pesticide applied per acre for concentrate orchard
sprays should also be related to tree size, usually by specifying
the same or less active ingredient as that which would be applied
using a full coverage spray. For special modes of application
(aircraft, ULV, mist sprays), the directions for use should include
both the spray concentration and the spray volume per acre. The
names and quantities of any stickers, spreaders, or other adjuvants
used in the spray solution should be given. The maximum number of
applications allowed, the minimum interval between application and
harvest (PHI), and the minimum interval between treatments should
be indicated.
(2) Animal treatments.
Animal treatments present special dosage control problems.
The concentration of pesticide in the working solution is the
primary consideration in dips and wetting sprays. The directions
for dips should include some instructions for recharging and
maintaining a constant solution strength in the dip tank, and for
the disposal of spent dip solutions. Any factors which may affect
the deposition of residues should be covered in the directions for
use, e.g. , the maximum number of retreatments, time of the animal
in the dip tank, nozzle type, pressure, or delivery rate of sprays,
and the amount of solution to be applied per animal for "pour-on"
or other specialized treatments.
When application of pesticides by automatic devices (i.e.,
photoelectric or treadle actuated sprays) or backrubbers is pro-
posed, the directions for use should take into consideration such
factors as how often they should be recharged and where they are
to be placed so that the degree of exposure of the animals may be
gauged.
(3) Fumigants.
Dosages may be expressed in terms of weight of fumigant
per volume of storage space (lbs act/100 ft3) or, where appropriate,
weight of fumigant per unit weight of commodity treated (lbs
act/1000 lbs grain).
Parameters such as time of exposure, temperature, pressure,
geometry and airtightness of containers, and aeration procedures
(including time of aeration) should be specified.
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(4) Aquatic uses.
The application of a pesticide to flowing water, impounded
water, irrigation ditch banks, dry beds of water conveyance systems,
or other aquatic sites is termed an aquatic use.
The types of application will vary widely, depending on
the mode of action of the pesticide. Herbicides for deep growing
submersed weeds may require deposition of slow release granules on
the bottom near the root zone. For this type of treatment, the
dosage would be expressed in terms of lbs act ingredient per surface
acre, much like an agricultural field use. The use of a water-
soluble herbicide which acts by direct absorption into the target
plant is dependent on maintaining a certain concentration in the
water and the dosage should be expressed in terms of ppm in water.
In the latter case, the directions for use must relate the dosage
per surface acre to average pond depth.
Aquatic herbicide applications may require some very
specialized equipment. A detailed description of the equipment
and principles involved in the treatment should be included; for
example, metered pumping of invert emulsions to the bottom of
lakes through weighted hoses. A proposed use of timed release
capsules will require information on how the encapsulated material.
is placed and the mechanism of the release.
It is frequently necessary to include limitations on the
minimum distance from a potable water or irrigation intake pipe.
This limitation is necessary whenever unacceptable levels occur in
water at the intake pipe.
To avoid loss of desirable species through oxygen deple-
tion, it is sometimes necessary to treat at intervals only portions
of ponds with heavy weed infestations. The label should state
what proportions of a pond should be treated per application and
the required interval between treatments. If treatments are intended
only for pond margins, as opposed to overall broadcast treatment,
it should be so indicated.
Ditch bank treatments are usually made by boom sprayers
from trucks. For adequate coverage, there is an unavoidable over-
lap with some direct addition to the water as well as runoff
contamination. The label should clearly direct how such treatments
are to be made with minimum contribution of herbicide to the water.
A prohibition may be required against cross-ditch spraying.
(5) Foreign uses.
Tolerances may be proposed to cover residues resulting
on food treated in foreign countries so that such foods may be
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imported into this country. The pesticide products used in the
treatment may be of foreign manufacture, or may be manufactured in
the United States and exported'"to the country where the application
is made. Use of a pesticide in„a foreign country is of course not
registered under FIFRA. Therefore, Section 408(d) of the FFDCA
which provides only that registrants under the FIFRA may petition
for tolerances, is not applicable. The proponent of a tolerance
on imported foods should therefore petition under Section 408(e)
of the FFDCA.
For domestic pesticides uses, a determination is made by
the Agency that the tolerance is adequate to cover residues likely
to result from uses as directed on registered labels. In the case
of foreign uses, it is required that the petitioner provide all
necessary information on the amount, frequency, and time of appli-
cation, along with a statement as to what regulatory mechanism is
available to control the use in the country of origin.
(6) Food handling establishments.
A Food Additive Regulation set under Section 409 of the
FFDCA specifying the conditions of use in food handling establish-
ments shall be a requirement for registration of such a use under
FIFRA. The regulation may or may not specify a numerical tolerance
for residues in foods.
Although directions for use will ordinarily be contained
on the product label, the usage directions for those products
intended for use solely by professional pest control operators may
be presented as a technical bulletin. The potential for food
contamination from treatments in areas where food is prepared or
processed rests largely upon the care exercised by the applicator
in following the directions and observing specified restrictions.
For this reason, the instructions should be explicit. The direc-
tions for use should include (for example) the type of establish-
ments that may be treated, the dilution instructions for preparing
the working solution, the spray concentration, the type of equip-
ment by which it is to be applied, the mode of application (di-
rected spray to crevices, baseboards, space spray, etc.), dosage
limitations including cubic and square foot limitations, frequency
of treatment, time of treatment (after-hours in restaurants), and
other pertinent information, as: (1) sanitation procedures; (2)
removal of food; (3) covering of dishes and utensils; (4) cleanup
procedures before food preparation, processing or serving resumes.
(7) Agricultural premises.
Agricultural premise uses will vary widely and might in-
clude distribution of granular insecticides to feed lots; fogging
of dairy barns; installation of impregnated strips or cords in
animal barns; or applications of sugar-base bait sprays to walls,
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stanchions, and other surfaces of barns. The directions for use
should .be sufficiently detailed to permit an evaluation of the
potential for residues-.oft milking-equipment, exposed feeds, drink-
ing and feed troughs, or in meat, milk, poultry and eggs of animals
quartered on treated premises. The directions should state what
areas are to be treated, frequency of treatment, whether animals
must be removed at time of treatment, and any other pertinent
information. Dosage for fogging treatments should be expressed
in terms of lbs per unit volume of the structure treated; im-
pregnated strips and similar devices in terms of number of
installations per unit volume; sprays in terms of concentra-
tion of active ingredient in the solution applied; and feed
lot applications in terms of weight of active ingredient per
unit area.
(8) Miscellaneous applications
The general criteria for use directions do not apply to
certain specialized processes, such as the manufacture of im-
pregnated fruit wraps to control fungus diseases, or processes
in which pesticide are applied post-harvest to fruits, such as
in a wax coating. Under these circumstances, the user of the
pesticide product is a trained operator experienced in the
use of relatively complex mechanical equipment, and directions
for use on the retail packages are usually not necessary. How-
ever, a complete * description of the process including quality
control measures and directions for disposal of spent dip solu-
tions or runoff should be made a part of Section B of a petition.
(b) Restrictions.
Clearly written and practical uses restrictions are
necessary so that the Agency may gauge the residues likely
to result. The following are limitations which should be
specified when pertinent to the use:
(a) State the maximum number of applications permitted
during a growing season together with the timing and the inter-
val between treatments.
(b) Specify the interval between last application
and harvest (or slaughter). This may be expressed in terms
of days before harvest or may be tied to a stage of crop
maturity such as "not after first bolls open." If the
directions for use are related to some identifiable growth
stage, such as "first bolls open" or "pegging time," the
petitioner should indicate the minimum time from this
stage to harvest.
(c) Avoid impractical or unrealistic use restrictions.
Restrictions against the food or feed uses of plant parts other
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than the primary raw agricultural commodity are practical only
when the item remains under the control of the grower and the
item is not of ma]or economic importance. For example, a re-
striction against feeding sugar beet tops is practical because
the tops remain under control of the grower; a restriction
against feeding dried citrus pulp from a treated grove is not
practical or acceptable, since the pulp from a treated fruit
would not retain its identity in processing. As another example,
a restriction against feeding corn forage or fodder is impractical
because of the major economic importance of corn forage and fodder.
Restrictions of more than 2 days in the time interval between
application to animals and slaughter are considered impractical
because animals may be sent to slaughter over an extended period
of time, and once sold are no longer under control of the user of
the pesticide. Table II and the "Guide for Estimating Toxic
Residues in Animal Feeds or Diets"* may be consulted for an indi-
cation of whether a feed item is under control of the grower.
A restriction calling for discarding of milk during a
prolonged interval after the treatment of lactating dairy cattle
would be considered unrealistic, since it would impose an economic
hardship on the user and would tend to be ignored.
(d) Use restrictions should be as specific as possible.
A restriction such as "Do not use after lay-by" is indefinite in
that lay-by time for a given crop may vary considerably due to
differences in cultural practices and geographical areas. Indefi-
nite terms such as "Do not use on animals being finished for
slaughter" should be avoided and a specific withdrawal period
should be stated; similarly, withdrawal times after an animal
treatment must be practical. Restrictions should also be as in-
clusive as possible. For example, the warning "Do not use on
dairy animals," is preferable to "Do not use on dairy cows," since
the latter excludes dairy goats.
In the case of uses in food handling establishments, specific
directions to minimize residue transfer are especially important.
A general caution such as "Avoid contamination of food" is by
itself of limited effectiveness and should be supplemented by
explicit warnings such as "Cover food utensils," "Do not apply
when exposed food is present," "Apply after plant operations are
shut down," or "Wash food contact surfaces before plant resumes
operation."
§171-4 Results of Tests on the Amount of Residue Remaining, Includ-
ing a Description of the Analytical Methods Used.
(a) Nature of the Residue.
* Available from the National Technical Information Service (NTIS)
as document Number PB-243-748-LK.
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( 1) Characterization of the Total Terminal Residue.* Many
pesticides undergo change during or after application to the
soil, water, crop, or livestock. The composition of the termi-
nal residue must therefore be determined before complete residue
detection methodology and residue quantification data can be
developed.
The use of radiolabeled pesticide compounds usually is the
only satisfactory way of providing such metabolism data. In choos-
ing the position to be labeled, assurance is required that a labile
position is not chosen. Usually labeling is preferred, although
32P, 35S or other elements may be more appropriate if no carbons or
only labile carbon side chains exist in the molecule. Tritium use
is strongly discouraged. Ring labeling is preferred for most
aromatic or cyclic compounds. If a potentially labile side chain
or tritium labeling is chosen, a metabolism study will be considered
adequate only if all significant activity in the plant is identified
and found to be associated with the pesticide, and not related to
loss of the label from the basic structure of the pesticide molecule.
While in vitro data are useful to show if the pesticide is
likely to undergo hydrolysis (acid, base, or enzymatic), oxidation
or reduction, photolysis, or other changes, additional data must
usually be submitted to show the fate in the plants and animals.
These metabolism studies are required whenever a pesticide use is
determined to be a food use. Based on the results of the charac-
terization studies, the chemical definition of the "total toxic
residue" should be proposed. The term "total toxic residue" is
used to describe the sum of the parent pesticide and its degra-
dation products, metabolites (free or bound) and impurities which
are of toxicological concern. All components of the "total toxic
residue" will be included in the tolerance expression for the
pesticide and residue analytical methods must be developed for all
components of the "total toxic residue."
The identification of the components of the terminal residues
and the definition of the "total toxic residue" often present
complex problems that must be resolved before finalizing the
analytical methodology and gathering the residue quantification
data. Thus, the petitioner may wish to consult with the Agency's
chemists and toxicologists to determine whether the residue has
been sufficiently characterized, which metabolites should be
covered by the tolerances, and which components of the residue
must be determined by the residue analytical methodology. The
determination of whether the residue has been sufficiently charac-
terized will depend on the level of activity remaining unidentified,
* The term total terminal residue is used to refer to all compo-
nents of the residue whether or not they are toxic enough to be
of concern.
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the importance of the plant or animal tissue containing the uniden-
tified residue as a food or feed, the chemical structure of the
active ingredient and identified metabolites, the toxicity of the
active ingredient, and the toxicity of chemicals similar in struc-
ture to potential metabolites.
The petitioner should delineate, preferably in a flowsheet,
the routes of degradation or metabolism in plants and animals; and
clearly specify the capability of the analytical method(s) to deter-
mine the components of the residue, whether free or bound. Photo-
graphs of thin-layer chromatographic (TLC) plates, paper chromato-
grams, or radio-autographs of plants treated with labeled pesticides
should be furnished. Such evidence will contribute significantly to
the evaluation of the data.
The petitioner should always be alert to the possibility of new
and unexpected metabolites of the pesticide which may affect future
tolerance proposals. Where the structure of a metabolite or altera-
tion product is identical to another registered pesticide chemical,
the petitioner should state this fact.
(2) Nature of the Residue in Plants.
The term "plant metabolism" is used here for convenience to
describe the formation of all alteration products of the pesticide
in or on plants regardless of whether they result from plant meta-
bolic processes. Adequate plant metabolism studies fulfill at
least four purposes: (1) they provide an estimate of total residues
in the treated crops; (2) they identify the major components of the
terminal residue, thus indicating the components to be looked for in
residue quantification studies; (3) they indicate the distribution
of residues, e.g., whether the pesticide is absorbed through roots
or foliage, whether translocation occurs, or whether the residues
are entirely surface residues; and (4) they show the efficiency of
extraction procedures for various components of the residue.
Identification techniques such as co-chromatography with syn-
thesized model compounds, reverse isotope dilution, and mass spec-
troscopy are often employed for identification of the residue com-
ponents. Enzymatic, basic, or acid hydrolysis techniques may need
to be employed to release bound or conj ugated residues. It is im-
portant that the need to use these techniques to release the residue
is determined and that, if necessary, these techniques are included
in the analytical methodology.
The minimum application rate in a plant metabolism study should
approximate the proposed label rates; however, exaggerated rate
studies may be necessary in order to obtain sufficient activity for
identification. The metabolism studies should be carried to plant
maturity whenever possible, so that the composition of the residues
found is indicative of that in the terminal residues at harvest.
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The study should include characterization of the residue in all
plant parts used for food or feed. Table II includes a list of the
RAC's derived from each crop. A metabolism study must be submitted
for each type of plant for which use is proposed. For example,
metabolism studies in bean plants would be representative of all
legumes but would not be translatable to root crops such as potatoes
or carrots. In general, one metabolism study will be required for
each of the crop groups defined in CFR 40 180.34(f), except for
herbs and spices.
If the results of three metabolism studies on dissimilar
crops indicate a similar metabolic route in the three crops, then
additional metabolism studies will not be required.
(3) Nature of the Residue in Livestock. The purpose of
these studies is to identify the nature of the residue in the
edible tissue of livestock, milk and eggs. Animal metabolism
studies are required whenever a pesticide is applied directly to
livestock, animal premises are to be treated, or residues result
in crops or crop parts used for feed. Information on whether crop
byproducts are used for feed can be obtained from Table II and
the "Guide for Estimating Toxic Residues in Animal Feeds or Diets"
cited previously.
Data on the metabolism of a pesticide in laboratory animals
which are required in the toxicology section of these guidelines
will generally not substitute for metabolism data on livestock.
Laboratory animal metabolism studies should, however, be duplicated
or referenced in the residue chemistry section of a petition to
allow for comparison of the metabolism in several species. In
some cases laboratory animal metabolism data may be used to sup-
plement livestock metabolism studies in which couplete charater-
ization of the residue is not attained.
In general, separate metabolism studies are required for
ruminants and poultry. The species of choice are usually goats
and chickens. Non-ruminant (swine) metabolism studies may be
required if the rat metabolism is significantly different than the
goat or chicken metabolism. Additional animal metabolism studies
are required if direct dermal or inhalation application to live-
stock is proposed. These additional studies should reflect the
proposed use so that it can be determined whether dermal or in-
halation exposure results in the same metabolic patterns as oral
dosing.
The minimum dosage used in metabolism studies should approx-
imate the level of exposure expected from the feeding of tolerance
level residues on crops with existing, proposed or anticipated
tolerances, or the proposed use rate for direct animal treatment.
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However, exaggerated dosages are usually required to obtain suffi-
cient residue in the tissues for characterization. Animals dosed
orally should be dosed daily for at least three days. Direct
animal treatment dosing should reflect the proposed use. Animals
should not be preconditioned by dosing with unlabeled material.
The material fed should simulate the terminal residues in feed
items as closely as possible or reflect the material to be used in
a direct animal treatment.
Animals should be sacrified within 24 hours of cessation of
dosing.
Milk and eggs should be collected twice daily. Tissues to
be analyzed should include at least muscle, liver, kidney and fat.
Characterization of the residue in urine and feces frequently
facilitates characterization of the lower levels of residue found
in tissue, but is not required.
The livestock metabolism study should primarily identify the
compounds for which analytical methods and residue data must be
generated. It should also indicate the distribution of residues
in tissues, eggs and milk, and whether residues are stored and
accumulated. The livestock metabolism study should also result in
elucidation of the efficiency of extraction of the various compon-
ents of the residue so that extraction/residue release procedures
can be developed as part of the analytical methods.
(b) Analytical Methods.
(1) General Requirements.
The methods for residue analyses should serve two functions:
(1) they must provide the residue data upon which judgments are
made as to the identity and magnitude of residues from the proposed
use, and (2) they must provide a means for enforcement of the
tolerance. The methods described in the FDA Pesticide Analytical
Manual (PAM) and the Official Methods of Analysis of the Association
of Official Analytical Chemists can be used as examples of suitable
Analytical Methods.
The analytical method(s) must be described in a stepwise
fashion in sufficient detail to enable a competent analyst to apply
the method even though he is unfamiliar with the procedure. Reprints
of published methods may be included in Section D. However, where
modifications have been made to adapt a basic method to other crops
for which a tolerance is proposed, details of the modifications
are needed. This includes application to the byproducts, meat, milk,
poultry, or eggs if these are a consideration.
The method should not be subject to substrate-related interfer-
ences or those arising from reagents. Appropriate clean-up measures
should be incorporated to reduce or eliminate spurious responses
that might jeopardize the results. For example, in gas-liquid
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chromatographic methods, separation should be sufficiently distinct
to yield reasonably discrete peak(s) for the component(s) of interest
rather than a response which appears as a shoulder on an interfering
peak.
Whenever possible, Gas Liquid Chromatography (GLC) retention
times and response values should be reported relative to those of
a stable reference compound, particularly when the residue is con-
verted to a derivative prior to gas chromatography. GLC parameters
should be reported in a form such as the guidelines outlined in
J. Agric. & Food Chem., Vol. 20 No. 6, page 1275; (1972).
(2) Validation of method by petitioner.
Methods must be validated by control sample data and recovery
data for all components of the "total toxic residue" on an adequate
representation of the commodities involved. Blank values should
be reasonably low in relation to the proposed tolerance. Recoveries
should be at fortification levels appropriate to the proposed tol-
erance. Recoveries should be at least 70%, and should not vary
signficantly from sample to sample. If 70% recovery is not attain-
able, the Agency will accept, on a case-by-case basis, methods hav-
ing lower recoveries for active ingredients that are not acutely toxic
or minor metabolites. '
The raw agricultural commodity, or a macerate thereof,
should be fortified, rather than crop extracts. The portion of
the crop to be analyzed is specified in the Pesticide Analytical
Manual (PAM) Volume 1,* in 40 CFR 180.1, and in Table II. The
petitioner should state his estimate of the practical limit of
detection as applied to each of the subject crops or tissues. The
estimate of the practical limit of detection should be based on
the least concentration of pesticide which can be detected with a
reasonable degree of assurance, taking into account the size and
variation of blanks (instrument response due to crop extractives
and reagents).
(3) Extraction efficiency.
Conventional recovery experiments as discussed above do not
necessarily reflect the efficiency with which aged (weathered)
residues are extracted from crops. There should be some assurance
that aged residues are completely extracted by the procedure.
*Available from the National Technical Information Service (NTIS)
as order number NTISVB118.
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Radioisotope labeling provides the best evidence on completeness of
extraction; but other techniques, such as comparison with exhaustive
extraction procedures, may be used. Frequently this information
can be obtained as part of the plant and animal metabolism studies.
Data obtained by surface stripping are not acceptable except
for crops where other data on that crop have established that the
total residues are in fact only surface residues.
As a general rule, chlorinated hydrocarbon insecticides from
watery vegetables should be extracted with a non-polar solvent in
combination with a polar solvent. Very dry samples, such as hay,
often require the addition of water to the sample as well as the
employment of more exhaustive techniques.
Certain components of the residue may occur bound with
naturally occurring plant constituents, and thus may not be
recovered by extraction techniques that are satisfactory for the
free components. Whenever there are indications of the formation
of bound components which may not be recovered by the extracting
solvent, modifications should be made in the procedure that will
free and recover the liberated components. One such modification
would be the initial hydrolysis of the treated crop. These bound
components may also be recovered with polar solvents and hydrolyzed
under acidic, basic, or enzymatic conditions to free the components.
These should not be confused with those fragmentary components
which may be so tightly bound or incorporated into the plant's
metabolic pool that they are not recoverable by any chemical means.
Such components are of interest, but are not usually of toxicological
concern.
(4) Determination of "total toxic residues."
' /
The method or methods employed should measure the "total
toxic residue" found in the metabolism studies outlined in Section
171-4(a), nature of the residue. Often all components of toxico-
logical concern will contain a common chemical moiety so that the
method may be adapted to determine all compounds simultaneously.
However, in some cases, it may be necessary to adapt separate
extraction-cleanup procedures, or even another complete method, to
measure the "total toxic residue" or a significant component of
the residue. In other cases, one or more components of the residue
will be significantly more toxic than other components of the
residue and will have to be determined separately.
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(5) Requirements for regulatory methods.
One or more of the methods proposed in the petition must be
acceptable to enforce the proposed tolerance. Where applicable,
use of the FDA multi-detection methodology outlined in Vol. I of
the Pesticide Analytical Manual is strongly recommended. Also,
the enforcement method should be as simple as possible to decrease
the cost of monitoring for pesticide residues.
A method which may be valid for gathering residue data is not
necessarily suitable for enforcement purposes. In general, an
enforcement method should:
Not require the use of a sample of the untreated commodity
as a blank;
Not require the use of an internal or procedural standard
(such samples are not available to enforcement analysts);
Not require exotic equipment or reagents (or reagents that
are no longer manufactured);
Be reasonably rapid in execution;*
Be sufficiently specific to measure and identify the resi-
due in the presence of residues of other pesticides which
could reasonably be expected to be present on the same
commodity; and
Be sufficiently sensitive in relation to the tolerance
proposed.
Methods based on cholinesterase inhibition are not regarded
as suitable for enforcement purposes. Methods based on paper
or thinlayer chromatography and which visually measure the residue
are not adequately quantitative for enforcement purposes. They
may be useful, however, as confirmatory methods to help identify
the residue.
Although certain gas-liquid chromatographic detection systems
possess inherent specificity, methods based on these systems should
* Regulatory methods should require a maximum of 24 hours for com-
pletion. Methods taking longer than 24 hours will be considered
acceptable on a case-by-case basis for minor metabolites or residues
that are not acutely toxic. Methods taking less than 24 hours will
be required for acutely toxic residues because of the possibility
of the enforcement of accidental or misuse contamination.
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usually be supplemented by a confirmatory method. In general,
confirmation by mass spectrometry is suitable. The specificity may
also be enhanced by the use of special extraction-cleanup pro-
cedures, derivatization, parallel or alternate columns and p-values.
The method(s) proposed for enforcement may be subjected to
trials in EPA laboratories if the pesticide is new, if the analyti-
cal method(s) is new and unfamilar, or if the commodity is known
to be difficult to analyze. The burden of proof is on the peti-
tioner, and should the method fail to perform as expected in these
trials, the petitioner will be asked to resolve the difficulties.
Also, the petitioner will be responsible for improving such a
method and furnishing new residue data by the improved method. If
the method performs satisfactorily and is acceptable as an enforce-
ment method, it will be made available to interested parties by
publication or reference in the FDA Pesticide Analytical Manual.
Thus, a petition must include a copy of the analytical method which
is not claimed to be, or stamped, confidential business information.
The Agency will not release copies of the method to the public
until the permanent tolerance has been established. Methods will
be released to enforcement agencies prior to the establishment of a
permanent tolerance if FIFRA Section 18 emergency exemptions or a
temporary tolerance is in effect.
(c) Magnitude of the Residue.
(1) General Considerations.
The residue field experiments will basically consist of examin-
ation of raw agricultural commodities for residues of the pesticide
chemical after treatment corresponding to the uses proposed in
Section B of a petition. If the pesticide or its formulation(s)
are not from regular production lots, it should be clearly stated
how they differ from regular production lots. If the residue
studies are carried out prior to availability of a commercial for-
mulation, then only analysis of the technical chemical used in the
residue studies and a statement of formula will be required in the
petition. These data are needed for comparison to the commercial
formulations at the time of registration.
Residue investigations should be specifically designed so as
to circumscribe the total residue picture. Data should be available
to show whether residues occur on any plant parts that may be used
in foods or feeds. Use on rice may necessitate residue data for
water, crayfish, catfish, and irrigated crops when water from the
rice field is diverted to such uses.
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Guidelines for specific areas of consideration are as follows:
(i) Residue(s) determined.
The purpose of field experiments is to quantify by chemical
analyses the terminal residues of concern that have been previously
demonstrated in the metabolism studies. The "total toxic residue,"
as defined in Nature of the Residue, should be determined by the
chemical method of choice. In some cases, it may be necessary to
employ more than one analytical method to determine the "total
toxic residue." Terminal residues in some commodities may differ
from those found in other commodities, e.g., residues in meat or
milk may differ from those in plants. In cases where determination
of bound residues or minor metabolites require separate analysis or
unduly increase the cost of processing residue samples, not all
samples must be analyzed for these components. However, enough of
the samples must have been analyzed for these components to allow
estimation of the ratio of these components to the parent compound.
(ii) Sampling.
The samples taken should be of the whole raw agricultural
commodity (RAC) as it moves in interstate commerce. For some crops
there may be more than one RAC derived from the crop. For example
the RAC's for field corn include the seed, fodder and forage.
Table II contains a list of the RAC's derived from each crop. The
sample should not be brushed, stripped, trimmed, or washed except
to the extent that these are commercial practices before shipment,
or to the extent allowable in Section 180.l(j), Code of Federal
Regulations, the PAM or the Codex Document Alinorm 81/24, appendix
III. It should be noted that in the enforcement program, produce
is examined for residues on an "as is" basis, regardless of whether
it meets any Federal or State quality grading standards with respect
to washing, brushing, or number of wrapper leaves retained. Because
certain crops (cabbage, celery, and lettuce) may be shipped without
having been stripped or trimmed, samples of these crop should re-
flect both trimmed and untrimmed samples; only obviously decomposed
outer leaves should be removed. The preparation of each sample
prior to analysis should be indicated.
Samples should be collected to reflect the various parts of
the commodity that might be marketed separately, consumed or fed at
various times. For example, in an early post-planting use on winter
wheat, the green plant should be sampled at the time it might be
foraged, the mature wheat grain should be sampled, the dried straw
should be sampled, and the bran, millings, and flour from the grain
should also be analyzed. Table II includes a list of the various
RAC's and processed commodities that should be analyzed.
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The sample taken from a field should be representative of all
portions of the crop from the field. Thus, there should be a valid
statistical basis for sampling. Standardized procedures, such as
the use of the Latin squares for a forage crop, selection of tree
fruits from the upper, middle, and lower levels of opposing quadrants
of the tree; the use of grain triers for the taking of core samples
of commodities in bulk quantities; and sample reduction by quartering
are desirable to assure a representative sampling. While analysis
of replicate samples from a field is desirable, it is preferable to
have additional field site data rather than replicate data from
within a field if only a limited number of samples are analyzed.
Accepted procedure for maintaining sample integrity should be
followed after taking the sample. Normally samples should be frozen
as soon as possible and kept frozen until analyzed. Information
should be furnished on how samples are shipped and stored until
analyzed. If samples are likely to be held in storage, storage
stability data should be obtained by fortifying control samples,
storing them under the same conditions as the treated samples, and
analyzing at the end of the storage period. It-is always advisable
to have spiked storage stability samples available to allow for
unforeseen delays in analysis, and to verify the results of analysis
of check samples should reanalysis be necessary to verify possibly
aberrant results.
(2) Design of residue experiments.
(i) Field studies.
The field experiments should not be considered merely as an
adjunct to field performance (efficacy) tests but should be designed
specifically to yield residue data. The procedures described in
the Food and Agriculture (FAO) Plant Protection Bulletin, Vol. 24,
1981, pa
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pressure currently exists in some of the major growing areas.
Seasonal variations in the production of crops should also be
represented. These should include an arid region where the crop
is grown by furrow irrigation and residues are likely to be high.
Several varieties should be represented, and cultural practices
for the crop should be followed. For minor crops, the amount of
geographical representation needed may be limited if the registered
label limits the geographical area where the product may be used.
The field experiments must also provide for residue dissipa-
tion or decline studies in which samples are taken at intervals
during the period from the last application of the pesticide to
normal harvest. The data obtained should indicate the pattern of
uptake of the pesticide and its decline. When presented graph-
ically, these data are useful in determining a preharvest interval
if one is needed. Data on the decline of residues after harvest
are also desirable. These data are used by the enforcement agen-
cies following accidental contamination or misuse.
There are no specific requirements as to the number of field
experiments or of individual samples. Because variations in residue
values are always to be expected, the number of samples should be
sufficient to give assurance that the proposed tolerance can be
met. Usually, the more widespread and important the crop, the more
field experiments and samples are required. Similarly, if there is
a great deal of concern over the toxicity of the residue, then more
field experiments and samples will be required to give the needed
assurance. Replicate treatment of individual sites is usually not
necessary since variations in residue levels within a field are
usually small compared to the variation between sites.
'(ii) Fumigation uses.
In addition to treatments at the proposed use conditions,
treatment at exaggerated rates is desirable. The studies should
adequately represent those commodities which might be treated,
including oily foods (peanuts, butter), and high surface area foods
(flour), and types of packaging allowable under the directions for
use. The studies should reflect the effect of parameters such as
time of exposure, dosage, temperature, pressure, geometry and
airtightness of the container upon residue levels. The effect of
aeration time and procedure upon residue reduction should be
demonstrated.
(iii) Slow-release encapsulated formulation uses.
The use of slow-release encapsulated formulations may lead to
higher residues than conventional formulations. Thus, if use of a
slow-release formulation is proposed, residue data reflecting this
formulation will be required. Data showing that the analytical
method detects any active ingredient remaining in the encapsulating
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material at the time of analysis is required. The registrant
should consult the Agency chemists and toxicologists concerning
whether residue data on the encapsulating wall material are needed.
The general criteria used by the Agency is that if the encapsulat-
ing material is an inert polymer and is not absorbed from the gut,
then residue data are not required. For polymers not previously
cleared, this requires a radiolabeled encapsulating material feed-
ing study with rats showing essentially 100% excretion of activity,
with no residual activity in tissues. Data on the residue levels
of the encapsulating material will not be required for uses involv-
ing application before edible parts form.
(iv) Processed Food/Feed Studies.
(a) Concentration of Residues on Processing.
Whenever there is a possibility of residue levels in processed
foods/feeds exceeding the level in a raw agricultural commodity
(RAC), processing data are required. Examples of processed foods/
feeds in which residues may concentrate are apple juice, wet and
dry apple pomace; the hulls, meal, crude and refined oil and
soapstock from cottonseed; or the sugar, dried pulp and molasses
from sugar beet roots.
A list of processed byproducts is contained in Table II.
Processing studies must simulate commercial practices as
closely as possible. RAC samples used in processing studies must
contain field-treated detectable residues, preferably at or near
the proposed tolerance level, so that concentration factors for
the various byproducts can be determined. This may require field
treatment at exaggerated application rates to obtain sufficient
residue levels for processing studies. Processing studies utiliz-
ing spiked samples are not acceptable, unless it can be demonstrated
that the RAC residue consists entirely of a surface residue.
If the processing studies indicate that residues concentrate
on processing, then a Food Additive Petition, including a Food
Additive Regulations proposal, is required. If the processing of
the RAC may result in alteration of the residue, then a radiolabeled
processing study to determine the nature of the residue in food/feed
as consumed may be needed. If significant alteration of the residue
occurs, and the additional residue components are of toxicological
concern, then the Food Additive Regulation must include the additional
residue components.
(b) Reduction of the Residue Level on Processing.
In those cases where the assumption of tolerance level resi-
dues results in unsafe exposure, then the petitioner has the option
of submitting data on food prepared for consumption. If these
data indicate that trimming, cooking, peeling or processing, resi-
dues to the point that the ADI is not exceeded, data indicate that
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washing, trimming, cooking, peeling or processing reduces residues
to the point that the ADI is not exceeded, then the safety evalua-
tion done by the Agency will be based on this lower level of residue.
The tolerance, however, will still be set on the RAC as it travels
in interstate commerce. Of course, if these data indicate that
residues concentrate in some fractions while decreasing in others,
both the higher and lower residue levels will be used in the
safety evaluation. The Agency will also take into account the
wide variation in techniques used to prepare food. For example,
if cooking destroys the residue on a vegetable, the Agency will
use the lower limit of detection in the cooking study as the residue
level for cooked vegetables. The Agency will also use the consump-
tion of uncooked vegetables and the tolerance level to estimate
the exposure from uncooked vegetables. As noted above, if signifi-
cant alteration in the nature of the residue could occur on proces-
sing, then a radiolabeled study will be needed to determine the
nature of the residue following processing.
(3) Meat, Milk, Poultry and Egg Feeding Studies.
Data must be submitted to show the level of residues that
will result in meat (muscle, liver, kidney and fat), poultry, eggs,
or milk. These data are needed whenever a pesticide is to be ap-
plied directly to livestock, residues occur on a feed or forage
crop, or residues occur on any plant parts that could be used in
animal feeds. Based upon the residue level in the feed item and
the residue resulting in meat, milk, poultry, and eggs in these
feeding studies, the use must be classified as specified in 40 CFR
180.6(a). Category 1 of Section 180.6(a) applies to cases where it
is shown that residues will occur in animal products; Category 2
applies if there is a reasonable expectation of residues in animal
products; and Category 3 applies if there is no reasonable expecta-
tion of residues. Since tolerances for residues in animal products
are required when the use is judged to be Category 1 or 2, the
animal feeding studies must not only show whether residues transfer,
but may also need to serve as a a basis for setting appropriate
tolerance levels for the animal products.
(i) Residues in feeds.
The compound(s) or residues fed should correspond, as closely
as possible, to the aged residues found in the items of feed. The
components of the residue to be determined should be those found to
constitute the "total toxic residue" in the animal products as
determined in the livestock metabolism study described in section
171-4b. The feeding study should include the level of intake
expected (1x), plus two exaggerated levels of 3x and 10x. The lx
level should represent the worst case estimate of the potential
livestock exposure based on the assumption of all components of the
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feed having tolerance level residues. The exaggerated levels are
especially important in judging a Category 3 use, as well as to
cover possible future tolerances for the pesticide on additional
feed items and allow estimation of whether residue levels in
tissues vary linearly with the level in the feed. The required
limit of detection of the method applied to the animal products
will be related to the toxicity of the compound but should generally
be on the order of 0.01-0.05 ppm. The dosage levels should be
expressed in terms of concentration (parts per million) in the
total ration (dry weight basis), so that the Agency can relate the
dosage to that expected from the proposed use. It is also desirable
to express the feeding level in terms of mg/kg body weight.
In selecting the dosage levels based on total rations, the
petitioner should take into account the proportion in the diet of
the feed item bearing the residue. Table II should be used as a
guide in determining the proportion of the diet of the various feed
items. For example, dried citrus pulp may in some circumstances
ccmprise up to 20% of the total ration (dry weight basis) of dairy
cows. If. a tolerance of 5 ppm of a given pesticide were proposed
on 'dried citrus pulp, the total diet (dry weight basis) should be
fortified at the 1 ppm level to reflect the expected level of in-
take (1x). If tolerances for other feed items could also be fed
in combination with citrus pulp, the contribution from these feed
items should also be added in. As noted, two dosages at exaggerated
levels are also required, preferably three-fold and ten-fold or
higher where not precluded by toxicity of the pesticide.
Separate feeding studies are required for a ruminant and poul-
try whenever residues occur on the feeds of these classes of live-
stock, or direct animal treatment is proposed. The species of
choice for these feeding studies are the cow and chicken. A swine
feeding study may be required for major swine feeds depending on
the likelihood for residue accumulation in animal tissue. A swine
study is required if direct application to swine is proposed as
indicated in the next part (b) of this section.
In addition to establishing a baseline or blank in a pre-dosing
period, control animals should be carried through the experiment
with treated animals. This is highly desirable, since values for
control animals have been observed to change during feeding studies.
The number of animals carried at each treatment level, and as
controls, will vary with the circumstances; but as a general rule
each group in a cattle feeding study should comprise a minimum of
three animals. For a chicken feeding studies, a minimum of 10
birds per group should be used. It is often advisable to have
additional animals on test that can be used to determine the rate
of decline of residues on the cessation of dosing", so that if
residues above tolerance are found, data on the time necessary for
residues to fall to the tolerance level are available.
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The period of time during which the animals are kept on the
treated feed will also depend on the individual case. Generally,
animals should be kept on test" until residues plateau in milk or
eggs. If no residues are detected in milk or eggs, animals should
be kept on test for four weeks.
(ii) Direct Animal Treatment.
When a pesticide is proposed for direct use on food animals,
data are required to show the extent of residues incurred by the
use. The experimental treatment should reflect as closely as pos-
sible the conditions under which the pesticide will be used com-
mercially. Control animals should be carried along with treated
animals. Factors such as whether sheep passing through a dip tank
were freshly shorn or unshorn should be considered. Generally,
separate studies should be carried out for each species of live-
stock to be treated. The data should also reflect treatment by
several applicators.
When a pesticide may be applied in more than one type of
formulation or by more than one mode of treatment, separate studies
reflecting the usage or combination of usages proposed are required
However, data from dips or high pressure wetting sprays on cattle
may be accepted in lieu of data from dust treatments but not vice
versa. When the use of devices which permit unlimited access (e.g.,
backrubbers) are proposed, the experiment should be designed to
assure the maximum exposure of the animal to the pesticide. Data
reflecting exaggerated treatments are desirable.
(in) Agricultural Premise Use Studies.
When the use of pesticides in agricultural buildings are such
that restrictions cannot preclude the possibility of residues in
meat, milk, poultry eggs or feed, residue studies should be carried
out to determine the maximum conditions of exposure. The studies
should reflect all possible residue transfer routes such as: (1)
direct absorption (dermal or inhalation) from sprays, mists, or
fogs with animals present; (2) direct consumption (e.g., by the
animal licking surfaces treated with sugar base baits, pick up of
bait granules by poultry, or contamination of feed, feed troughs,
(or water troughs) and (3) direct contamination of milk from deposi
tion on milking equipment, treatment of milk rooms, etc.. Separate
studies are required for ruminants (cows), non-ruminants (swine)
and poultry (chickens).
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(iv) Meat, milk, poultry and egg sampling.
The tissues to be analyzed in a feeding study include all
tissues that are used as a human food. If residues concentrate in
a particular tissue such as fat, liver or kidney, then proportion-
ately more of these tissue samples should be analyzed. Also,
since muscle constitutes the majority of the food derived from
livestock, proportionately more of these tissue samples should
be analyzed.
Milk and egg samples should be taken twice daily. Eggs from
birds within a dosage group may be pooled if necessary so that
adequate sample weight is available for analysis and retained sam-
ples. Milk from animals within a dosage group should not be pooled
so that data for individual animals are available. Enough of the
pooled daily milk and egg samples should be analyzed to allow for
a determination of trends in storage of residues with time. Animals
should be slaughtered within 24 hours of the last dosing and tissue
samples taken and frozen as soon as possible. Tissue residue
level results from animals slaughtered long aftea cessation of
dosing are not usable in estimating tolerances, and thus if this
occurs, the feeding study will have to be repeated.
(4) Potable Water, Fish and Irrigated Crop Studies.
Any use of pesticides in or near aquatic sites may lead to
residues in potable water, fish and shellfish, irrigated crops, and
meat, milk, poultry and eggs. For each of these commodities, ade-
quate data are needed to demonstrate both the nature of the residue
and the level of residues resulting from the maximum proposed use.
Because of the nature of aquatic uses, emphasis must be placed on
the use of practical use restrictions which will be followed by
the applicator.
The design of the aquatic pesticide studies to demonstrate the
fate of the pesticide in the aquatic environment must be directly
related to the restrictions imposed on the use. For example, use
in impounded bodies which are completely under the control of the
user may be sub]ect to practical label restrictions that would
preclude livestock watering, fishing, or use for drinking or
irrigation for a specified time period after treatment. On the
other hand, such restrictions would not be practical for use of a
pesticide in a river system.
In the latter type of use, restrictions against treatment
within a given distance of potable water intakes are considered
practical. In general, separate and distinct protocols will be
required for still waters (lakes, ponds), flowing water, irrigation
conveyance systems, and tidal estuaries. The fate of the compound
must be demonstrated with respect to rate of dispersion downstream,
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26
degradation, volatilization, or sorption by plants or hydrosoil.
Degradation products in water should be identified and may need to
be quantified.
Experiments to show possible residues in crops irrigated with
treated water may utilize the crop grouping scheme 40 CFR 180.34(f).
Residue data for representative crops in each crop group are nor-
mally required. If it has been determined that residues are likely
to occur in water when it could be ingested by livestock, animal
feeding studies must be carried out as described previously.
Fish metabolism studies are required when fish may be exposed
to the pesticide or its degradation products. If no is
detected in fish in a static metabolism study then the following
fish residue studies are not required. Shellfish residue studies
will however still be required.
The fish and shellfish residue studies may be of various
types, depending on the aquatic system involved. Controlled
exposure for appropriate time intervals ma^ be carried out under
static or dynamic conditions in aquaria, or the specimens may be
exposed in natural sites if the treated area can be isolated, such
as by cages. Field studies under natural conditions are preferred.
Samples for analyses should reflect the fish commodity definition
in the Pesticide Analytical Manual, Volume I. The proposal for
tolerances in fish should be expressed on the basis of the edible
portion. For fish, residue data are needed for both bottom feeders,
(e.g., catfish) and predators, (e.g., bass); for shellfish, data
are needed for both molluscs (e.g., clams, oysters) and crustaceans
(e.g., shrimp, crabs). If use in estuarme areas is planned, data
on whole fish protein concentrate, and smoked, canned, or other
processed fish products are needed to determine whether a Food
Additive Regulation is necessary.
Potable water is defined as any water at such time as it
enters a public drinking water system whether or not it receives
any treatment or filtering. Data must show the highest level
likely to occur in water at any time it may be used for drinking
purposes. Data showing the extent to which the compound is removed
or reduced in specific water treatment processes are desirable.
However, if safety of the use is predicated on removal or reduction
of the residue in water by a commercial treatment process, there
must be practical restrictions limiting use to bodies of water
that will necessarily receive the processing before consumption of
the water. For example, use to control weeds in reservoirs could
be limited to reservoirs which flow into specific water treatment
facilities.
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(5) Food Handling Establishment Use Studies*
Studies must be conducted to determine residues in food or
feed resulting from treatment of food/feed handling establish-
ments* with residual insecticides** (Asterisked terms are defined
below and m Federal Register Notice Vol. 38, No. 154, Friday,
* A food handling establishment is an area or place other than a pri-
vate residence in which food is held, processed, prepared and/or
served.
a. Nonfood areas of food handling establishments include garbage
rooms, lavatories, floor drains (to sewers), entries and vestibules/
offices, locker rooms, machine rooms, boiler rooms, garages, mop
closets, and storage (after canning or bottling).
b. Food areas of food handling establishments include areas for
receiving, serving, storage (dry, cold, frozen, raw), packaging
(canning, bottling, wrapping, boxing), preparing (cleaning, slicing,
cooking, grinding), edible waste storage, enclosed processing systems
(mills, dairies, edible oils, syrups).
** Nonresidual insecticides are those products applied to obtain insec-
ticidal effects only during the time of treatment and are applied either
as space treatments or contact treatments.
a. Space treatment is the dispersal of insecticides into the air by
foggers, misters, aerosol devices or vapor dispensers for control of
flying insects and exposed crawling insects.
b. Contact treatment is the application of a wet spray for imme-
diate insectlcidal effect.
Residual insecticides are those products applied to obtain insec-
ticidal effects lasting several hours or longer and are applied as
a general, spot, or crack and crevice treatments.
a. General treatment is application to broad expanses of surfaces
such as walls, floors, and ceilings or as an outside treatment.
b. Spot treatment is application to limited areas on which insects
are likely to occur, but which will not be in contact with food or
utensils and will not ordinarily be contacted by workers. These
areas may occur on floors, walls, and bases or undersides of equip-
ment. For this purpose, a "spot" will not exceed 2 square feet.
c. Crack and crevice treatment is application of small amounts of
insecticides into cracks and crevices in which insects hide or through
which they may enter the building. Such openings commonly occur at
expansion joints, between different elements of construction, and be-
tween equipment and floors. These openings may lead to voids such
as hollow walls, equipment legs and bases, conduits, motor housings,
junction or switch boxes.
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28
August 10, 19 73). Establishments to be treated will be typical
commercial operations.selected from among the various types listed
under each of the categories shown in Table I. Data obtained from
tests conducted in two different types of establishments in each
category will normally be adequate for clearance of the insecticide
for use in all types of establishments defined by the category of
which the test establishment is a part. Careful 3 udgment will
have to be applied in selecting the types of establishments to be
tested as well as the number of tests necessary in order to ensure
adequate representation of that category. More than two types of
establishments may require testing as the individual case indicates.
Existing sanitation programs and practices, as well as the type
of building construction (wood, cement block, etc.) at a plant
site, are important factors that should be considered. Usage will
normally involve application of the insecticide as a general,
spot, or crack and crevice treatment; and will include both nonfood
and food areas of the establishment used as the test site. Accept-
able results from a test of the most rigorous type of treatment
(general > spot > crack and crevice) will preclude need for residue
tests involving less rigorous treatments; and will allow clearance
of the insecticide for use by the less rigorous method(s). Label-
ing must specify that treatment of establishments will be performed
in accordance with proposed labeling by a certified (or otherwise
qualified) pest control operator whose work for the past year has
included treatment of establishments in the same category.
The experiment should be designed to reflect all possible
avenues of contamination, taking into account the physical and
chemical properties of the pesticide; proximity of foods and pro-
tective barriers as may be specified in the regulation; mode of
application; and use restrictions.
Considerations should be given to at least the following
residue transfer routes where applicable:
(1) Direct deposition of spray droplets on foods, direct
absorption of fumigant, airborne dust particles;
(2) Volatilization of residual deposits and subsequent
absorption into foods;
(3) Direct transfer of residues from treated surfaces
(countertops, cupboards, utensils, packaging materials, etc.);
(4) Volatilization with condensation on surfaces where food
is subsequently placed;
(5) Leakage or weeping of chemical from devices or impreg-
nated materials, hung in food establishments for insect control;
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29
(6) Transfer of pesticide through permeable barriers (e.g.,
from impregnated shelf papers to packaged food);
(7) Tracking of residues from bait stations or sprayed areas
to foods or food contact surfaces by rodents or insects, or contamina-
tion from fallen insects;
(8) Deposition of solid or crystalline chemicals from repeated
sprays on ceilings over food handling areas;
(9) Distribution of vapors, droplets, or particulate matter
through forced ventilation systems (central air conditioning, duct
heating systems);
(10) Distribution of residues in continuous process food
operations from treatment of ends and tailings, conveyor lines,
boots, etc., when operation is shut down (e.g., flour mills).
Many sources of contamination may be eliminated (or greatly
diminished) as practical sources of contamination through use
restrictions, variations in the mode of application, type of
establishment treated or nature of the product or formulation.
Data should be submitted to establish the relative importance of
these factors on the levels of residue which may be expected to
result from the pesticidal application. Experiments should be
conducted by analyses of representative foods subj ected to expo-
sure by any of the above routes which are potential avenues of
contamination.
The selection of samples for analyses in the more specialized
uses, e.g., flour mills, would be apparent. In the more generalized
exposure situations, e.g., grocery stores, it is suggested that the
selection of samples for analyses represent a range of foods such
as an oily food (butter), baked cereal products, beverages, raw and
processed meats, and fresh fruits and vegetables (lettuce).
In order to demonstrate the residues resulting from the wide
variation of conditions anticipated in actual situations, and to
gauge the potential for misuse, the experiment should include some
exaggerated exposure. This might include spraying at a 2x rate,
exposure of foods for longer periods than might normally be expected,
or even exposure of some foods when there is a restriction to cover
foods when treating.
For certain uses (notably the devices of the automatic dispenser
and impregnated resin strip type), the total exposure would include
inhalation as well as oral ingestion of residues on foods. In
these cases, the experiment should include some determination of
concentration in air under representative conditions.
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30
§171-5 Practical Methods for Removing Residues That Exceed Any
Proposed Tolerance. (Section E of a petition)
Except in certain specialized pesticide applications, the
tolerances are set at levels that are adequate to cover residues
that are likely to result from a proposed use without any special
processing of the commodities to reduce residues to the tolerance
level. In a few pesticide uses, however, the judgment of safety is
predicated on the reduction of residues by aeration of fumigated
commodities or other processes intended to reduce residues. In
these cases, section E should include a discussion of how the
tolerance level residues, which are higher than a safe level, are
reduced to a safe level. The data on which these determinations
must be based is discussed in Section 171-4(c)(2)(iv).
§171-6 Proposed Tolerances. (Section F of a petition)
Tolerances should be proposed in terms that best represent
the total toxic residues on the raw agricultural commodity, whether
it be the parent pesticide or altered forms of it, or both. The
proposed tolerance should not be based on an "average residue"
value but should be large enough to include any residue values
which could be reasonably expected based on the available data.
It should not be larger than is needed for the proposed use
although some limited accommodation to this rule may be necessary
in the interest of avoiding an inordinate multiplicity of tolerance
levels for a single pesticide on a number of different crops.
Analytical methods will commonly determine one or more conversion
products along with the parent compound when the method is based
on measurement of a chemical moiety common to all. In such cases,
it may be appropriate to propose combined tolerance for all of the
compounds calculated as the parent compound, toxicological consi-
derations permitting.
The petitioner should consider whether the proposed tolerance
can be made compatible with Maximum Residue Limits (MRL's) estab-
lished by the Codex Alimentarius Commission (an organization set
up under the auspices of the United Nations to facilitate inter-
national trade) or the tolerances established by Mexico or Canada.
The tolerance comparison should include compatibility of both the
numerical level proposed and the residue definition (i.e., the
metabolites included in the tolerance).
An exemption from the requirement of a tolerance may also be
proposed when appropriate (See Section 171-8). When an exemption
is proposed, data must be presented to show the level of residues
to be expected. Other chemistry data requirements, in general,
parallel those for numerical tolerances.
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31
In the case of Food Additive Regulations covering the use of
pesticides in food handling establishments, it is contemplated that
the regulation may or may not include a numerical tolerance on
foods. In either case, the proposed regulation should specify the
conditions of use of the pesticide. The determination of whether a
numerical tolerance is needed will be based on the toxicity of the
residue and the level of possible contamination.
§171-7 Reasonable Grounds in Support of the Petition. (Section G of
a petition)
The petitioner should present the rationale of how the residue
data support the proposed tolerance. The presentation should
include brief discussions on the adequacy of the analytical method
with respect to sensitivity and determination of the total toxic
residue; an explanation of any aberrant residue values reported; an
explanation for the omission or substitution of requirements set
forth in these Guidelines; and any other residue considerations
pertinent to the proposed use. Where appropriate, a discussion
should be furnished on the status of other components of the
formulations.
§171-8 Exemptions from the Requirement of a Tolerance.
(a) Active Ingredients. Exemptions from the requirement
of a tolerance are appropriate for pesticides for which no enforce-
ment action can be anticipated. Since an exemption from the
requirement of a tolerance means that there is no limit on the
level of residue that could occur, exemptions are limited to
relatively non-toxic pesticides. Examples of active ingredients
for which an exemption is appropriate are acetic acid and sulfur.
Exemptions from the requirement of a tolerance for an active
ingredient should be requested by submission of a petition.
Normally, the only information/data needed in such a petition
are the data from Sections A, B, E, F, and G. The normal
residue chemistry data requirements in Section D will be waived
for toxicologically-innocuous active ingredients, except
possibly for the requirement of an analytical method if needed
for enforcement purposes.
(b) Inert Ingredients. Inert ingredients of pesticide
formulations have been determined to be pesticide chemicals
within the meaning of the Act and are subj ect to the Pesticide
Amendment (Section 408) of the FFDC Act. A large number of
these inert ingredients have been exempted from the requirements
of a tolerance (40 CFR Section 180.1001). Requests to add
other adj uvants should be submitted as petitions for exemption
or as a letter to the Director of the Registration Division,
Office of Pesticides Programs. Data requirements for inerts
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32
will not ordinarily be as extensive as for active ingredients.
However, an analytical method may be required and a basis for
estimation of the level of residues likely to result must be
provided. Limitations on the use may be imposed in the exemption
regulation. Any clearances of the inert ingredient by the
Food and Drug Administration as a food or feed additive should
be referenced. The amount of residue chemistry data needed
for the exemption of an inert ingredient will vary with the
nature of the chemical. The minimum information required are
a description of the identity of the chemical and the possible
uses involved. If the inert ingredient cannot be deemed
toxicologically-inoccuous, then additional data will be
required. In some case the full data requirements described
for active ingredient tolerances will be required, while in
other cases only an analytical method and residue data for
representative crops will be required. The amount of data
required will depend on the toxicity of the chemical and the
use restrictions imposed.
§171-9 Tolerances for Foreign Uses.
Foreign uses are not subject to registration requirements.
However, proposals for tolerances for residues in any imported
foods or feeds should be submitted under Section 408(e) of the
Federal Food, Drug, and Cosmetic Act. Tolerances proposed in
conj unction with requests for domestic registration are submitted
under 408(d) of the Act. Petitions submitted under 408(e) should
contain the same types of information, including sample labelling,
and data as those submitted under 408(d). In addition, the petition
should briefly discuss any controls regulating the use of pesticides
in the country in which the pesticide will be used and some evidence
that the requirements for use in the foreign country have been
met.
§171-10 Rotational Crops Tolerances.
The requirements for rotational crop tolerances are included
in "Tolerance for Pesticide Residues in Rotational and Follow-up
Crops, Meat, Milk, Poultry and Eggs, and for other Indirect
Inadvertent Residues," FR Vol 40, Vol 8, Tuesday, January 13, 1981.
Section 165 of these guidelines (Environmental Fate, Rotational
Crop Data Requirements) should also be consulted concerning when
petitions, and tolerances, for rotational crops are required.
As noted in the FR notice cited above, the residue chemistry
data requirements for a petition for a tolerance in rotational crops
are the same as those required for a conventional tolerance. How-
ever, it should be noted that for rotational crop tolerance peti-
tions, Section B must contain directions for use on the target
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33
crop and limitations as to which, and when, crops may be planted
following harvesting or destruction of the target crop. The
limitations in the number of crops and timing of planting will
determine the amount of data needed for rotational crop tolerances.
If no limitations on rotational crops are added to the label, then
residue data for representative crops in the crop grouping scheme
40 CFR 180.34(f) will be required before rotational crop tolerances
can be established.
The design of the residue field trials must of course also
match the restrictions included in the Section B. For example, the
restrictions could indicate that soybeans may be planted 14 days
after corn has been planted, if the corn germination is poor. The
residue field trial should then consist of application to the soil
planted to corn, followed by planting of soybeans 14 days later and
analysis of soybeans as normally required.
Eighteen months is the longest planting interval which is
considered practical. If residues persist in the soil past 18
months, then rotational crop tolerances for representative crops in
the crop grouping scheme will be required. The field trial data in
this case should include data on the uptake of residues 18 months
after application to the parent crop by all representative crops in
the crop grouping scheme.
Rotational crop tolerances will be distinguished in the CFR
from parent crop tolerances. The publication of a rotational crop
tolerance will not allow for registration of use under FIFRA on the
rotational crop. The purpose of the rotational crop tolerances is
only to allow for the presence of residues of persistent pesticides
that occur in crops other than the target crop.
§171-11 Tobacco Uses.
Use of a pesticide on tobacco does not require a tolerance
or an exemption from the requirement to obtain a tolerance.
Nonetheless, data are needed to assess the exposure of man to
the residue remaining at the time of use of the tobacco. The
data required include a residue profile for the tobacco and its
smoke.
This residue profile must include the active ingredient and
all significant plant metabolites of the active ingredient,
translocated degradation products from soil, and photo degradation
products. Radioisotopic techniques will normally be required to
identify the significant components of the residue. If residues
at 0.1 ppm or more are detected, analytical methods must be
developed.
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34
Data from the following studies must be submitted to show
conclusively the level of residue likely to result from the use
of the pesticide:
(1) Total residues on green freshly-harvested tobacco. If
residues at 0.1 ppm or more are detected, the determinations of
the next paragraph of this section are required.
(2) Pyrolysis products derived from the active ingredient
must be characterized.
§171-12 Food Use/Non-Food .Use Determination Data Requirements.
In some cases residue chemistry data are needed to determine
whether a proposed use is a food use or a non-food use. The gen-
eral criteria for food use/non-food use determinations is that if
residues could occur in foods or feed, then the use is a food use
and a petition for tolerance/exemption from tolerance is required.
In some cases this determination can be made based on the nature
of the site to which the pesticide is to be applied. Thus appli-
cation to non-cropland is considered a non-food use. In other
cases the distinction is not as clear. For example, baiting with
a rodenticide around the borders of cropland or in a tamper-resis-
tant bait box within cropland would be considered a non-food use,
but applying the bait directly to the crop would be considered a
food use.
For the following types of uses, the food use/non-food use
determination will be based on the results of the data described in
each section. Registration for these types of uses will not be
granted until the necessary data have been submitted to the Agency
and found acceptable.
(a) Seed Treatments.
This includes cases where seed is treated either by the
seed company (and dyed according to the Seed Act) or by the farmer
(planting box or hopper treatments).
In order for a seed treatment to be considered a non-food
use, data from a radiotracer study must be available showing
no uptake of residues (activity) from treated seed into the
aerial portion of the growing crop.
If residues occur in the aerial portion of the plant, or if
there is no data available to make this determination, seed treat-
ments are considered to be food uses requiring tolerances.
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35
(b) Crops Grown for Seed Only.
These crops would qualify as non-food uses provided there is
no likelihood of residues in crops grown from the harvested seeds.
Factors affecting this include the level of residues on the har-
vested seed, the half-life of seed residues, the weight of the
seed in relation to that of the subsequent crop and the amount of
residue uptake from the seed into the aerial portion of the crop.
On the other hand, uses on crops where the seed itself is a
major raw agricultural commodity, (such as corn, sorghum,
soybeans, small grains and sunflowers), are considered to
be food uses. In these cases, seeds from treated crops
could not be distinguished from untreated crops and could
be diverted to human and animal comsumption.
Alfalfa and clover grown for seed cannot be considered a
non-food use because of the economic importance of alfalfa
and clover hay. Subsequent cuttings for hay would be taken
regardless of label restrictions. Also, because of the
increasing importance of alfalfa sprouts as a human food
item, use on alfalfa grown for seed only cannot be considered
a non-food use.
Dessication uses for clover grown for seed will be considered
non-food uses because the dessication renders the hay unfit for
consumption by livestock.
(c) Fallow Land. Use of a pesticide on fallow land requires
data indicating whether residues persist in soil long enough for
uptake by crops. See the Environmental Fate Section for the design
of soil persistence studies. Fallow land uses must include a time
limitation on planting to food/feed crops or tobacco. Eighteen
months is the longest time interval deemed practical for a fallow
land use restriction. If residues persist in soil for the length
of the time of planting limitation, or 18 months (whichever is
shorter), then a petition for tolerance for all crops which could
be planted on the fallow land will be required.
(d) Non-bearing Crop Uses. Application of a pesticide to a
non-bearing food or feed crop will be considered a nonfood use only
if data are available to demonstrate that no detectable residues
occur in the crop at the first harvest. Non-bearing crops are
perennial crops that will not produce a harvestable RAC during the
season of application. Thus the label must contain a restriction
against harvesting during the season of application. If residues
are detected, then a petition for tolerance with the full range of
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36
residue chemistry data requirements will be needed before a toler-
ance and registration will be granted.
§171-13 Submittal of Analytical Reference Standards.
To avoid delay in processing petitions for new pesticides,
2 gram samples of purified analytical standards for the pesticide
and/or its principal degradation products or metabolites should be
submitted to the Pesticide and Industrial Chemicals Repository
(MD8), U.S. Environmental Protection Agency, Research Triangle Park
North Carolina 27711, USA.
The letter of transmittal should include the assay of the stan
dards, the analytical methods used, a statement of principal
impurities, purification procedures, storage requirements and
special precautions for safe handling. A copy of the transmittal
letter should be inserted in Section A of the petition. Larger
quantities of standards are usually required once the tolerance is
established. Replacement of standards may be required periodically
should decomposition occur in storage. For non-acutely toxic
metabolites which are difficult to synthesize, quantities less
than 2 grams will be acceptable.
§171-14 Special Considerations for Temporary Tolerance Petitions.
A temporary tolerance may be established in conjunction with
an Experimental Use Permit (pee Section III of these Guidelines).
A petition for a temporary tolerance should specify the amount
of pesticide which will be used under the conditions of the
experimental permit, the crop acreage which will be treated, and
the geographical areas where the treatments will be made.
The chemistry data requirements for permanent tolerances will
in general apply to petitions for temporary tolerances except that
method trials will not be conducted and the metabolism and residue
data need not be as extensive. Whether the latter exception is to
be made will depend on the toxicity of the pesticide or possible
degradation products and/or metabolites, the amount of acreage to
be treated, the importance of the food or feed commodity, and
similar considerations. It is assumed that data will be obtained
while the experimental permit is in effect and will be made avail-
able to the Registration Division.
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37
§171-15 Presentation of Residue Data.
Individual analyses, not average results, should be reported.
The data should include blank values and uncorrected values for the
treated samples. It should be indicated whether corrections have
been made for blanks and recoveries. When GLC is the method of
analysis, corrections should not be made for blanks due to discrete
peaks (at the retention time of the pesticide sought) in the
chromatograms of untreated controls.
It is preferable to summarize the data in tables showing crop,
residue found, dosage, interval from treatment, number of applica-
tions made, and formulation used. However, the tabulated data
should be keyed for ready reference to the raw data and sample
history sheets. The sample history sheets should note rainfall,
sample treatment (washed, brushed, trimmed, etc.), sample collec-
tion and analysis dates, storage conditions, and other factors
which might affect the residue levels.
The raw data should include standard curves, optical absorbance
readings, or copies of appropriately labeled gas chromatograms. It
is desirable that at least some of the chromatograms show the
analyst's sample dilution factors, sample equivalent injected, and
the way in which GLC peaks were quantitated. Photographs of tbin-
layer chromatography plates, paper chromatograms, or radioautographs
of plants treated with labeled pesticides should be furnished when
such evidence is necessary for the evaluation of the data.
A statistical treatment of data may be used to express the
precision and accuracy of the analytical results when sufficient
data make such treatment valid. The null hypothesis technique is
useful in calculating the confidence level at which a set of values
from control samples do not differ significantly from a set of
values from treated samples. A graphical representation of residues
versus time (decline or dissipation rate curves) is also desirable.
This is usually plotted on semi-log coordinates with time (days
after treatment) as the linear function.
§171-16 Translation of Data.
Data on tissue storage in rats, dogs, or other small animals
used in toxicology studies will not be accepted in lieu of residue
data on livestock. Data will not be translated from other meat
animals to poultry. However, within the poultry group, data on
chickens will usually be accepted in lieu of data on turkeys. Data
on residues in milk from dairy cows will usually apply as well to
dairy goats. Because of the higher fat/body weight ratio in hogs,
data on concentration of pesticides in the body fat of hogs may not
be applicable to goats or other animals of lower total body fat con-
tent.
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38
In some cases it may be possible to combine the radioactive
livestock metabolism study and the livestock feeding study. How-
ever, this is usually not desirable because of the need to dose
more animals for longer periods of time with radiolabeled material.
A list of similar crops for which residue data may be trans-
lated is given in the Regulations, 40 CER180.34(e) • Pesticides
which are absorbed into the plant or animal may be excluded from
this translation of residue data [Section 180.34(c)] .
The crop grouping scheme described in CFR 40 180.34(f) in-
cludes information on crop group tolerances. Utilizing the crop
group concept described can allow for tolerances on all crops in a
group of related crops based on data only for the representative
crops in a group.
Acknowledgements
Dr. Robert J. Hummel and Dr. Charles L. Trichilo and Messrs.
Robert S. Quick, George Beusch, and Donald Reed reviewed and made
significant contributions to the development of Subdivision 0.
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39
TABLE I
Categories and Representative Types
of Food Handling Establishments.
Category
Representative Types
Food Service ^
Est ab li shine nt s
Restaurants, Cafeterias, Taverns,
Delicatessens, Mess Halls, School
and Institutional Dining Areas,
Hospitals, Mobile Canteens,
Vending Machines, Groceries and
Markets.
Manufacturing^
Establishments
Candy Plants, Ice Cream Plants,
Spaghetti or Macaroni Plants, Food
Mix Plants, Breaskfast Cereal Plants
Bakeries, Breweries, Wineries,
Soft Drink Bottling Plants, Pizza
Plants.
Processing^ Meats, Poultry, and Seafood
Establishments Slaughtering and/or Packing Plants,
Dairies and Dairy Products Plants,
Spice Plants, Edible Fats and Oils
Plants, Fruit and Vegetable Cannerie
Pickle Factories, Beverage (Coffee,
Tea) Plants, Frozen Fresh Food Plant
Grain Mills.
1 Any food handling establishment whose principal business involves the
sale of food directly to the consuming public. The manufacture and/or
processing of food by such an establishment is only incidental to
achieving its principal business objective.
2 Any food handling establishment whose principal business involves
the production and/or packaging of man-made foods which are normally
intended for sale through or by food service establishments. Such foods
are generally composed of two or more ingredients which have been altered
in such a manner as to change their basic identity.
3 Any food handling establishment whose principal business involves the
the upgrading and/or preservation of raw agricultural commodities in such
a manner as to maintain their essential identity. Such establishments
may sell their product directly to the consuming public and/or food ,
service or food handling establishments.
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TABLE II
Raw Agricultural Commodities and Feeds Derived From Field Crops
CROP
RAC
PROCESSED
COMMODITIES
PERCENT OF LIVESTOCK DIET<1)
FEED
CATTLE
BEEF DAIRY
POULTRY
TURKEY &
BROILERS
LAYING
HENS
SWINE
BOARS & FINISHING
SOWS ANIMALS
Alfalfa
Forage
Seed
Hay
Meal
Forage(G)
Seed
Hay
Meal
50
30
25
25
80 |
nu(3>
NU
I
| NU
NU
10 |
20
20
I 10
10
80 j
NU
NU
| NU
NU
80 |
5
5
I 50
I
5
Almond
Nutmeat
Hulls
Hulls
25
25
NU
NU
NU
NU
Apples
Fruit
Pomace, wet
Pomace, dry
Juice
Pomace, dehy
50
25
NU
NU
NU
Apricots
Fruit
Artichoke
Fresh
Asparagus
Avocados
Bananas
Fresh
Fresh
Fresh
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TABLE II (Continued)
1
1
1
1
1
1
PERCENT OF
LIVESTOCK
DIET
I
I
|
1
| CROP
RAC
PROCESSED j
1
| FEEDS
| CATTLE
POULTRY
1
SWINE |
1
COMMODITIES j
I
1
1
1
I
| BEEF DAIRY
TURKEY &
LAYING
BOARS
& FINISHINGl
1
I
1
BROILERS
HENS
SOWS
ANIMALS j
1
| Barley
Grain
Germ |
I
| Grain
1
| 80 50
50
50
80
1
40 |
1
Forage
Milling |
| Forage(G)
| 20 40
NU
NU
NU
NU |
1
Hay
products |
| Hay(G)
j 25 60
NU
NU
NU
NU |
1
1
1
Straw
| Straw(G)
1
1
j 10 10
I
I
NU
NU
NU
NU j
1
1
1
| Bean
Seed and pod,
Cannery |
1
I Seed
I
| 20 20
10
15
25
1
20 |
1
succulent
residue |
| Vine(G)
| 20 35
NU
NU
NU
NU |
1
Seed, dry
I Cannery
I
1
1
Vine
I residue
| 20 20
NU
NU
10
10 |
1
1
Hay
1 Hay(G)
1
| 20 35
I
NU
NU
NU
NU |
I
1
| Beet, garden
Root
1
1
I
I
I
I
1
1
Greens
1
1
I
I
I
I
1
| Blackberries
1
Berry
1
1
1
I
I
I
I
I
I
1
| Boysenberry
1
Berry
1
1
I
I
I
I
I
I
1
| Blueberry
1
Berry
1
1
1
I
I
I
I
I
I
1
I Broccoli
1
Fresh
1
1
1
I
I
I
I
I
I
1
| Brussels
Fresh
1
1
I
I
I
I
| Sprouts
I
1
1
I
I
I
I
-------
TABLE II (Continued)
CROP
RAC
PROCESSED
COMMODITIES
PERCENT OF LIVESTOCK DIET
FEEDS
CATTLE
BEEF DAIRY
POULTRY
TURKEY &
BROILERS
LAYING
HENS
SHINE
BOARS & FINISHING
SOWS ANIMALS
Buckwheat
Grain
Forage
Hay
Straw
Bran
Milled
products
Grain
Forage(G)
Hay(G)
Straw(G)
Milled bypdts
50
25
25
10
25
50
70
60
10
25
70
NU
NU
NU
10
50
NU
NU
NU
5
80
NU
NU
NU
10
90
NU
NU
NU
5
Cabbage
Fresh, with
wrapper
leaves
Fresh, w/o
wrapper
leaves
Cacao bean
Bean
Roasted bean
Cocoa powder
Chocolate
Cantaloupe
Fresh
Carob bean
Carrot
Casaba
Cauliflower
Bean
Root
Fruit
Fresh
>
-------
TABLE II (Continued)
CROP
RAC
PROCESSED
COMMODITIES
PERCENT OF LIVESTOCK DIET
FEEDS
CATTLE
BEEF DAIRY
POULTRY
TURKEY & LAYING
BROILERS HENS
SWINE
BOARS & FINISHING
SOWS ANIMALS
Celery
Fresh
Cherries
Sweet
Sour
Chicory
Leaves
U>
Citrus
Whole fruit
Dried Pulp
Peel
Oil
Molasses
Juice
Pulp, dehy
Pulp, wet
Molasses
33
20
15
33
10
10
NU
NU
NU
NU
NU
NU
1
10
NU
1
10
NU
Clover
Fresh
Hay
Fresh
Hay
25
25
50
80
NU
NU
NU
NU
10
NU
5
NU
Cocoanut
Cocoanut
(meat and
liquid com-
bined)
Copra (dried
meat)
Oil
Meal
Copra Meal
15
15
15
10
NU
NU
Coffee
Green bean
Roasted bean
Instant
-------
TABLE II (Continued)
1
1
1
1
1
1
1 1
1 1
1 |
1
1
1
PERCENT OF
LIVESTOCK
DIET
I
I
I
1
| CROP
1
| RAC
1 1
| PROCESSED |
1
| FEEDS
1
CATTLE
POULTRY
I
SWINE |
1
1
| COMMODITIES j
1
1
I
1
1
1 1
1
| BEEF
DAIRY
TURKEY &
LAYING
BOARS
& FINISHING!
1
1
1 1
1
|
BROILERS
HENS
SOWS
ANIMALS |
1
| Collards
1
1
| Greens
1
1 1
1 1
1 1
1
1
1
1
1
I
I
I
I
1
| Corn, field
1
I Grain
1 1
I Crude oil |
1
| Grain
1
| 80
50
70
70
80
I
85 |
1
I Forage
I Refined oil |
| Forage
| 25
10
NU
NU
NU
NU |
1
| Silage
j Milled j
| Silage
1 25
10
NU
NU
NU
NU |
1
1
I Fodder
1
I products |
1 1
| Fodder
1
1 25
1
10
NU
NU
NU
NU |
I
1
| Corn, pop
1
| Grain
1 1
1 1
1
| Forage(G)
1
1 25
10
NU
NU
NU
I
NU |
1
I Forage
1 1
| Fodder(G)
| 30
50
NU
NU
NU
NU |
1
1
I Fodder
1
1 1
1 1
1
1
1
1
I
I
1
| Corn, sweet
1
| Sweet corn
1 1
I Cannery |
1
| Forage(G)
1
| 25
10
NU
NU
NU
I
NU |
1
| Forage
I waste |
| Cannery
I
1
1
1
1
1 1
1 1
| waste
1
1 30
1
50
NU
NU
NU
NU |
I
1
I Cotton
1
I Seed
1 1
| Meal |
1
| Meal
1
1 15
15
10
3
5
I
5 I
1
I Forage
I Hulls |
| Seeds
I 25
20
NU
NU
10
10 |
1
1
| Soapstock |
j Hulls
I 15
5
NU
NU
NU
NU |
1
1
I Crude oil |
| Soapstock
I 5
5
5
5
5
5 |
1
1
1
1
I Refined oil |
1 1
| Forage(G)
1
j 20
I
40
NU
NU
NU
NU |
I
1
| Cowpeas
1
I Seed
1 1
1 1
1
| Seed
I
I 25
70
10
10
10
I
10 |
1
1 Hay
1 1
1 Hay
I 20
20
NU
NU
5
5 I
1
1
I Forage
1
1 1
1 1
| Forage
!
I 30
I
100
NU
NU
NU
NU |
I
1
| Cr^bapple
1
I Fruit
1
1 1
1 1
1 1
1
1
1
I
I
I
I
I
I
i
-------
TABLE II (Continued)
1
1
1
1
1
|
1 II
1 II
1 1 1
PERCENT OF LIVESTOCK DIET
1
1
I
1
I CROP
1
I RAC
I l l
I PROCESSED ||
FEEDS
| CATTLE | POULTRY
1
SWINE |
1
i
| COMMODITIES j j
1 1
1
1
i
1 II
| BEEF DAIRY |TURKEY & LAYING
BOARS & FINISHING|
1
i
1 II
| |BROILERS HENS
SONS ANIMALS |
1
I Cranberry
1
i
I Berry
1
1 II
1 II
1 II
1 1
1 1
1
1
1
1
| Crenshaw
1
1
I Fruit
1
1 II
1 II
1 II
1 1
1 1
1 1
1
1
1
1
| Cucumbers
1
1
I Fruit
1
1 II
1 II
1 II
1 1
1 1
1 1
1
1
1
1
I Currants
1
1
I Fruit
1
1 II
1 II
1 II
1 1
1 1
1 1
1
1
1
1
| Damsons
1
1
| Fruit
1
1 II
1 II
1 II
1 1
1 1
1 1
1
1
1
1
| Date
1
1
I Fruit
1
1 II
1 II
1 II
1 1
1 1
1 1
1
1
1
1
| Dewberries
1
1
| Berry
1
1 II
1 II
1 II
1 1
1 1
1 1
1
1
1
1
1 Eggplant
1
1
I Fruit
1
1 II
1 II
1 II
1 1
1 1
1 1
1
1
1
1
| Elderberry
1
1
I Berry
1
1 II
1 II
1 II
1 1
1 1
1 1
1
1
1
1
| Escarole
1
1
| Fresh
1
1 II
1 II
1 II
1 1
1 1
1 1
1
1
1
-------
TABLE II (Continued)
1
1
1
1 1
1 1
| |
PERCENT OF
LIVESTOCK
DIET
I
I
I
1
I CROP
RAC
1 1
| PROCESSED |
FEEDS
CATTLE
POULTRY
I
SWINE |
I
j COMMODITIES |
I
I
1 1
BEEF
DAIRY
TURKEY &
LAYING
BOARS
& FINISHING|
i
1 1
BROILERS
HENS
SOWS
I
i
1 Figs
1
Fresh
1 1
| Dried |
1 1
I
I
I
1
I Flax
Seed
1 1
| Meal (linseed)|
Meal
15
25
3
3
5
I
5 I
1
Straw
| Hulls |
Straw(G)
10
10
NU
NU
NU
NU |
1
1 1
Hulls
20
10
NU
NU
10
10 |
1
1
1 1
1 1
Seeds
10
10
3
3
20
20 |
I
1
| Garlic
1
Bulb
1 1
1 1
1 1
I
I
I
1
| Gooseberries
1
Berry
1 1
1 1
1 1
I
I
I
1
| Grapes
Fruit
1 1
| Raisin |
I
I
1
| Pomace, wet |
Pomace, wet
30
20
3
3
10
10 |
1
| Pomace, dry |
Pomace, dry
30
20
5
5
20
20 |
1
| Raisin waste |
Raisin waste
10
10
NU
NU
NU
NU |
1
I Juice |
I
1
| Grass
Fresh
1 1
1 1
Fresh
75
70
NU
NU
NU
I
NU |
1
1
Hay
1 1
1 1
Hay
70
70
NU
NU
NU
NU |
I
-------
TABLE II (Continued)
CROP
RAC
PROCESSED
COMMODITIES
PERCENT OF LIVESTOCK DIET
FEEDS
CATTLE
BEEF DAIRY
POULTRY
TURKEY &
BROILERS
LAYING
HENS
SWINE
BOARS & FINISHING
SOWS ANIMALS
Guar
Seed
Forage
Milled
products
Seed
Forage(G)
Meal
10
20
10
10
40
15
15
NU
15
15
NU
15
10
NU
10
10
NU
10
Hops
Fresh
Dried
Spent hops
Spent hops
NU
NU
NU
NU
Horseradish
Root
-j
Huckleberries
Berry
Jerusalem
artichoke
Root
Kale
Fresh
Kiwi
Fruit
Kohlrabi
Kumquats
Fresh
Fruit
-------
TABLE II (Continued)
CROP
RAC
PROCESSED
COMMODITIES
PERCENT OF LIVESTOCK DIET
FEEDS
CATTLE
BEEF DAIRY
POULTRY
TURKEY & LAYING
BROILERS HENS
SWINE
BOARS & FINISHING
SOWS ANIMALS
Leeks
Stalk
Lentils
Fresh
Forage
Hay
Forage
Hay
20
20
35
35
NU
NU
NU
NU
NU
NU
NU
NU
Lespedeza
Fresh
Hay
Fresh
Hay
80
70
80
70
NU
NU
NU
NU
NU
NU
NU
NU
Lettuce
Fresh, with
wrapper
leaves
Fresh, w/o
wrapper
leaves
Loganberries
Berry
Lupine
Mangoes
Forage
Hay
Fruit
Forage
Hay
50
25
80
80
NU
NU
NU
NU
NU
NU
NU
NU
-------
TABLE II (Continued)
CROP
RAC
PROCESSED
COMMODITIES
PERCENT OF LIVESTOCK DIET
FEEDS
CATTLE
BEEF DAIRY
POULTRY
TURKEY & LAYING
BROILERS HENS
SWINE
BOARS & FINISHING
SOWS ANIMALS
Melons
Fresh
Millet
Grain
Milled
products
Grain
25 25
20
50
50
25
Mint
Hay
Spent hay
Oil
Spent hay
25
60
NU
NU
NU
NU
Mungbean
Bean
Sprouts
Mushroom
Head &' stem
Mustard
Greens
Seeds
Seeds
10
15
15
10 10
Nectarines
Fruit
Nuts
Nutmeat
-------
TABLE II (Continued)
CROP
RAC
PROCESSED
COMMODITIES
PERCENT OF LIVESTOCK DIET
FEEDS
CATTLE
BEEF DAIRY
POULTRY
TURKEY &
BROILERS
LAYING
HENS
SWINE
BOARS & FINISHING
SOWS ANIMALS
Oats
Grain
Hay
Straw
Forage
Hulls
Milled
products
Grain
Hay(G)
Straw(G)
Forage(G)
Hulls
20
25
10
20
5
50
60
10
40
NU
25
NU
NU
NU
NU
20
80
40
NU
NU
NU
NU
NU
NU
NU
NU
NU
NU
NU
NU
Okra
Fruit
Olives
Fruit
Oil
Onion, bulb
Bulb
i •
Onion, green
Papayas
Parsley
Parsnip
Whole p>lant
Fruit
Leaves
Roots
Roots
30
30
10
10
-------
TABLE II (Continued)
PERCENT OF
LIVESTOCK
DIET
j CROP
RAC
PROCESSED |
| FEEDS
| CATTLE
POULTRY
SWINE |
COMMODITIES |
1
| BEEF
DAIRY
TURKEY &
LAYING
BOARS
& FINISHING|
1
BROILERS
HENS
SOWS
ANIMALS |
| Passion
Fruit
1
1
| fruits
1
1
| Pawpaws
Fruit
1
1
1
| Peaches
Fruit
1
1
1
| Peanuts
Nutraeat
Meal |
| Meal
1
1 15
25
10
10
10
10 |
Vines
Crude oil |
| Vines(G)
I 20
40
NU
NU
NU
NU |
Hay
Soapstock |
1 Hay(G)
I 25
60
NU
NU
NU
NU |
Hulls
Refined oil |
| Hulls
j 5
Nu
NU
NU
NU
NU |
| Soapstock
I 5
I
5
5
5
5
5 |
| Pears
Fruit
I
I
I
I Peas
Seed and pod,
| Seed, dehy
I
I 30
25
10
40
20
20 |
succulent
| Vines(G)
I 25
40
NU
NU
NU
NU |
Vines
j Hay (G)
I 25
40
NU
NU
NU
NU |
Straw
I
Dried seed
I
I
| Peppermint
Hay
Oil |
| Spent hay
I
I 25
60
NU
NU
NU
NU |
Spent hay |
I
I
-------
TABLE II (Continued)
1
1
1
1
1
1
1
1
1
PERCENT OF
LIVESTOCK DIET
1
1
1
1
1
1
1
1
|
1
1 1
1 |
CATTLE
POULTRY
1
SWINE |
I
1
| CROP
1
1
| RAC
1
PROCESSED |
COMMODITIES |
1 1
| FEEDS |
1 1
BEEF DAIRY
TURKEY & LAYING
BROILERS HENS
1
BOARS & FINISHINGl
SOWS ANIMALS |
1
| Peppers
1
1
| Fruit
1
1 1
1 1
1 1
1
1
1
| Pimentos
1
1
| Fruit
1
1 1
1 1
1 1
1
1
1
1
| Pineapple
1
1
1
| Fruit
| Forage
1
Bran |
Juice |
1 1
| Bran |
| Forage(G) |
1 1
40 40
20 40
NU 5
NU NU
1
20 20 |
NU NU j
1
1
| Pistachio
1
1
| Nutmeat
1
1 1
1 1
1 1
1
1
1
1
| Plantain
1
1
| Whole fruit
1
1 1
1 1
1 1
1
1
1
1
| Plum
1
1
| Fruit
1
Prune |
1 1
1 1
1 1
1
1
1
1
I Potato
1
1
1
1
| Tuber
1
1
1
Granules |
Chips |
Dr ied |
1 1
| Cull potatoes|
1 1
1 1
1 1
30 30
7 20
1
50 50 |
1
1
1
1
| Pumpkin
1
1
| Fruit
1
1 1
1 1
1 1
1
1
1
1
I Quinces
1
1
I Fruit
1
1 1
1 1
1 1
1
1
1
1
| Radish
1
1
| Fresh
1
1 1
1 1
1 1
1
1
1
-------
TABLE II (Continued)
1
1
|
1
1 1
1 1
1 |
*
PERCENT OF
LIVESTOCK
DIET
I
I
|
1
1
1
1
1
1
1 1
1 1
1 |
CATTLE
POULTRY
1
SWINE.;., I
' I
1
| CROP
l
1
| RAC
1
1 1
| PROCESSED |
I COMMODITIES |
FEEDS j
BEEF
DAIRY
TURKEY &
BROILERS
LAYING
HENS
BOARS
SOWS
& finishing!
ANIMALS |
I
I Rape
1
I Seed
1 1
| Meal |
1 Oil |
Meal j
15
10
7
2
5
1
5 I
1
1
| Raspberry
1
1
I Berry
1
1 1
1 1
1 1
1
1
1
1
| Rhubarb
1
1
I Freqh
1
1 1
1 1
1 1
1
1
1
1
| Rice
1
1
1
1
1
I Grain
I Straw
1
1
1
1 1
| Polished rice|
j Hulls j
I Milled j
I products |
1 1
Grain, w/hulls|
Straw(G) |
Milled bypdts |
25
10
25
25
NU
25
40
NU
40
20
NU
20
NU
NU
NU
1
NU |
NU |
NU j
1
1
1
| Rutabagas
1
1
I Roots
1
1 1
1 1
1 1
1
1
1
1
1 Rye
1
1
1
1
1
| Grain
I Forage
I Straw
1
1
1 1
I Milled |
| products |
1 1
1 1
1 1
Grain |
Milled bypdts |
Forage(G) |
Straw(G) |
75
50
20
10
40
25
40
NU
5
5
NU
NU
5
NU
NU
NU
20
NU
NU
NU
1
25 |
NU |
NU |
NU |
1
1
| Safflower
1
1
I Seed
1
1 1
| Meal |
1 Oil j
Seed |
Meal |
10
15
NU
20
10
10
5
5
NU
20
1
NU |
20 j
1
| Sainfoin
1
1
| Forage
1 Hay
1 1
1 1
1 1
Forage |
Hay |
50
25
80
80
NU
NU
NU
NU
NU
NU
1
NU |
NU |
1
I Salisfy
1
1
I Fresh
1
1 1
1 1
1 1
1
1
1
-------
TABLE II (Continued)
1 1
1 1
1 1
1 1
| |
1
1
1
PERCENT OF
LIVESTOCK
DIET
I
I
I
1 1
1 1
1 1
1 1
1 1
1 |
1
1
1
1
I
CATTLE
POULTRY
SWINE 1' |
'i I
1 1
I CROP |
RAC
1 1
| PROCESSED |
1
| FEEDS
1
1
TURKEY &
LAYING
BOARS
1
& FINISHING|
1 1
¦
| COMMODITIES |
i
| BEEF DAIRY
BROILERS
HENS
SOWS
ANIMALS |
1 1
| Sesame |
1 1
Fresh
1 1
1 1
1 1
I
I
1
1
1
1
1
1
1 1
| Shallots |
1 1
Fresh
1 1
1 1
1 1
l
I
i
1
1
|
1
1
1
1 1
| Sorghum, grain|
Grain
1 1
I Flour |
l
| Grain
1
| 80
40
60
60
80
1
90 |
1 1
Forage
1 1
| Fodder(G)
1 25
50
NU
NU
NU
NU |
1 1
Fodder
| Milled pdts |
j Silage(G)
1 25
50
NU
NU
30
30 |
1 1
Silage
1 1
1 Hay(G)
1 25
60
NU
NU
NU
NU |
1 1
1 1
Hay
1 1
1 1
1
1
1
1
1
1
1 1
1 1
| Sorghum, sweet|
Seed
1 1
1 1
I Syrup |
1
1
| Forage(G)
1
1
| 80
50
NU
NU
NU
1
1
NU |
| (sorgo) |
Forage
| |
j Fodder(G)
j 80
50
NU
NU
NU
NU |
1 1
1 1
Fodder
1 1
1 1
1
1
1
1
1
1
1 1
I Soybean |
Seed
1 1
I Meal |
1
| Seed
1
1 10
25
20
50
20
1
20 |
1 1
Forage
| Hulls |
| Meal
I 25
25
30
20
20
20 |
1 1
Hay
| Soapstock |
| Hulls
| 20
10
NU
NU
10
5 1
1 1
Straw
I Crude oil |
| Ensiled
I 25
40
NU
NU
NU
NU |
1 1
1 Refined oil j
1 Hay(G)
I 10
40
NU
NU
NU
NU |
1 1
1 1
I Straw(G)
I 10
NU
NU
NU
NU
NU |
1 1
1 1
I Forage(G)
I 20
40
NU
NU
NU
NU |
1 1
1 1
1 1
1 1
| Soapstock
1
I 5
I
5
5
5
5
5 1
1
1 1
| Spearmint |
Hay
1 1
I Spent hay |
1
I Spent hay
I
I 25
60
NU
NU
NU
1
NU |
1 1
1 1
1 Oil j
1 1
1
1
I
I
1
1
1 1
I Spices |
1 1
Fresh
1 1
| Dried |
1 1
1
1
1
I
I
I
1
1
1
-------
TABLE II (Continued)
1
1
1
1
1
1
1 1
1 1
1 |
PERCENT OF
LIVESTOCK
DIET
#
1
1
i
1
I CROP
1
| RAC
1 1
| PROCESSED |
FEEDS
CATTLE
| POULTRY
i
SWINE |
I
1
| COMMODITIES j
I
1
l
1
1 1
BEEF
DAIRY
|TURKEY &
LAYING
BOARS
&
FINISHING!
I
1
1 1
|BROILERS
HENS
SOWS
ANIMALS |
I
| Spinach
1
1
| Fresh
1
1 1
1 1
1 1
I
I
I
1
1
1
1
| Squash
1
1
| Fresh
1
1 1
1 1
1 1
I
I
I
J
1
1
1
1
| Strawberry
1
1
I Fresh
1
1 1
1 1
1 1
I
I
I
1
1
1
I Sugar beet
1
| Root
1 1
I Pulp, dehy. |
Leaves(G)
20 '
20
I
| NU
NU
NU
1
NU |
1
I Tops
| Molasses |
Molasses
20
10
I 4
4
5
5 |
1
1
1
I
| Sugar, refined|
1 1
Pulp,dehy.
25
30
I NU
I
NU
15
5 |
1
1
I Sugarcane
1
I Cane
1 1
I Molasses |
Molasses
20
10
I
I 3
4
10
10 |'
1
I Forage
| Sugar, refined|
Bagasse
5
5
I NU
NU
NU
NU |
1
1
1
1
| Bagasse |
1 1
Forage(G)
20
40
I NU
I
NU
NU
NU j
I
1
| Sunflower
1
| Seed
1 1
I Meal |
Meal
30
20
I
I 15
15
10
I
10 , |
1
| Forage
1 Hulls j
Meal, w/o hulls
15
25
I 15
5
10
20 |
1
1
I Oil, crude |
Forage(G)
20
40
I NU
NU
NU
NU |
1
1
1
1 /
j Oil, refined |
1 1
Hulls
5
5
| NU
I
NU
NU
NU |
I
-------
TABLE II (Continued)
CHOP
RAC
PROCESSED
COMMODITIES
PERCENT OF LIVESTOCK DIET
FEEDS
CATTLE
BEEF DAIRY
POULTRY
TURKEY & LAYING
BROILERS HENS
SWINE
BOARS & FINISHING
SOWS ANIMALS
Tea
Leaves
Dried
-1—
10
NU
Tomato
Fruit
Pomace, wet
Pomace, dry
Puree
Catsup
Juice
Pomace, wet
Pomace, dry
20
25
10
25
3
NU
2
NU
10
NU
Trefoil
Forage
Hay
Forage
Hay
50
25
80
80
NU
NU
NU
NU
NU
NU
NU
NU
Turnip
Root
Tops
Roots(G)
Tops(G)
20
5
10
5
NU
NU
NU
NU
NU
NU
NU
NU
Vetch
Forage
Hay
Forage
Hay
20
20
60
40
NU
NU
NU
NU
NU
NU
NU
NU
Water cress
Watermelon
Fresh
Fruit
-------
TABLE II (Continued)
I I
I I
I i
1
1
PERCENT OF
LIVESTOCK
DIET
j CROP
RAC
1 1
| PROCESSED |
1
| FEEDS \
CATTLE
POULTRY
SWINE |
1 COMMODITIES |
1 1
1 1
1 1
BEEF
DAIRY
TURKEY &
LAYING
BOARS
& FINISHING|
1 1
1 1
BROILERS
HENS
SOWS
ANIMALS |
| Wheat
Grain
1 1
| Milled |
1 1
| Grain |
50
50
70
50
80
, . 90 |
Forage
| products |
| Forage(G) |
25
70
NU
NU
NU
J NU |
Hay
1 1
I Hay(G) |
25
60
NU
NU
NU
NU |
Straw
1 1
j Straw(G) |
10
10
NU
•NU
NU
NU |
1 1
1 1
| Milled bypdtsl
1 1
25
25
10
5
10
5 t
| Youngberries
Berry
1 1
1 1
1 1
1 1
1 1
1 1
(1)
(2)
(3)
Maximum percent of diet on a dry weight basis
NU - Not Used
G - Under control of the grower and thus subject to label restrictions against feeding
------- |