### 2 

## Itemized below are the specific comments presented by D AS , summarized in I talics and followed by EFED ’s response

.
1. The Problem Formulation state s on Page 8, Environmental Fate Characterization “T he 5

- OH degradate was also formed in the anaerobic aquatic study, at a maximum of 34% AR, as was the additional degradate TAAA (diclosulam triazoloacetic acid), which was present at a maximum of 34% AR in the aqueous phase.”

DAS ’s Comment : The 5

- OH degradate was formed in the anaerobic aquatic study at a maximum of 41.3% AR and TAAA (diclosulam triazoloacetic acid) was formed at a maximum of 41.5% AR in the total system (MRID 44192604). This correction does not affect the final assessment but should be changed to accurately reflect the behavior of diclosulam in an anaerobic aquatic system.

EFED Response : EFED acknowledges that the maximum %AR values for degradates 5

- OH and TAAA formed in the anaerobic aquatic study originally stated in the PF (34% f or each) were in error

. Th ese errors will be corrected in the Preliminary Risk Assessment (PRA)

.
2. The Problem Formulation states on page 10, Transformation Products : “the additional degradate TPSA (triazolopyrimidine sulfonic acid) was detected at 0.5 and 8.8% in the aquatic and soil photolysis studies,respectively.”

DAS ’s C omment :

“ The TPSA degradate was detected at 8.8 and 4.9% in the aquatic and soil photolysis studies, respectively. These corrections do not affect the final assessment but should be changed to accurately reflect the behavior of diclosulam and its metabolites

. ”

EFED’s R esponse: EFED acknowledges that the maximum %AR values for TPSA in the aquatic and soil photolysis studies as originally stated in the PF (0.5 and 8.8% respectively) were in error. The se errors will be corrected in the PRA

. 3. The Problem Formulation states on page 10, Transformation Products: “Although not reported as detected in any fate studies, 2,6

- dichloroaniline is also expected to be formed as

a con sequence of the 5 conversion of diclosulam to TPSA. A positional isomer of 2,6

- dichloroaniline is 3,5

- dichloroaniline, which is an identified degradate of other pesticides, and as such as been named a residue of concern.”

DAS’s C omment:

“ The aniline ring was labeled in the hydrolysis, soil and aqueous photolysis, aerobic soil metabolism, and the aerobic and anaerobic aquatic metabolism studies and 2,6

- dichloroaniline was not identified in any of these studies as a metabolite, as was noted by the EPA. 2,6

- D ichloroaniline was also not seen in the Nature of Residue studies on hen, goat or peanut. Given the lack of evidence to support 2,6

- dichloroaniline as a metabolite, we do not believe that 2,6

- dichloroaniline or its positional isomer 3,5

- dicholoroaniline sh ould be

### 3 

## considered residues of concern for diclosulam. Furthermore, we urge that EPA not make a residue of concern designation based only on the fact that 3,5

- dicholoroaniline is a degradate of other pesticides, as that does not mean it is a degradate for diclosulam. ”

EFED’s R esponse: As also noted by DAS, in its Problem Formulation EFED stated

“

A lthough not reported as detected in any fate studies, 2,6

- dichloroaniline is also expected to be formed as a consequence of the conversion of diclosulam to TPSA. A positional isomer of 2,6

- dichloroaniline is 3,5

- dichloroaniline, which is an identified degradate of other pesticides, and as such has been named a residue of concern

. ” In this statement , the reference to dichloroaniline s as “residue of concern” pertains specifically to the “other” pesticides referred to. At this time, as no dichloroanilines have been identified as major degradates of diclosulam, these compounds are not considered to be residues of concern for diclosulam. If the statement in que stion appears in the PRA, its language will be amended to make this point more clearly.

4. Page 11, Table 4. Diclosulam and Its Major Environmental Degradates

DAS’s C omment: After a review of the studies referenced, some errors in Table 4 were noted. DAS proposes Table 4 be replaced with the following corrected table.

EFED’s R esponse: Upon review of the original data , EFED agrees with the registrant’s proposed edit s, and has modif ied the degradate information table accordingly (below)

. The updated values reflect the maximum %AR detected in individual samples, rather than the maximum %AR averaged over all samples from a given time point

. For the anaerobic aquatic study (MRID 44192604), EFED found slightly different %AR values for the 5

- OH and TAAA degradates in the study report than the values the registrant proposed . In Table 4 the values updated based upon the registrant’s suggestions are footnoted . Values updated based upon re

- examination of the anaerobic aquatic metabolism study r eport are footnoted separately

.

### 4 

## Table 4. Diclosulam and Its Major Environmental Degradates
Code Name/ Synonym Chemical Name Chemical Structure Study Type Ref. (MRID) Maximum %AR (day) A Final %AR (study length)
PARENT Diclosulam

SMILES: ClC1=C(C(=CC=C1)Cl) N[S](=O)(=O)C3=N[N] 2C(=NC(=CC2=N3)F)O CC N

- (2,6

- dichlorophenyl)

- 5

- ethoxy

- 7

- fluoro[l,2,4]triazolo

- [l,5

- c] pyrimidine

sulfonamide

MAJOR TRANSFORMATION PRODUCTS 5

- OH
hydroxy diclosulam

SMILES: ClC1=C(C(=CC=C1)Cl) N([S](=O)(=O)C3=N[N ]2C(=NC(=CC2=N3)F) OCC)[H] N

- (2,6

- dichlorophenyl)

- 5

- hydroxy

- 7

- fluoro

- [l,2,4]triazolo[l,5

- c]

- pyrimidine

- 2

- sulfonamide Hydrolysis 43441043 4.3 C (4), pH 9 only 4.3 C (4) Aqueous photolysis 43441044

-- -- Soil photolysis 44192603 1.6 (26) 1.5 (30)

Aerobic soil 43441045 44045201 16.6 (140) 13.2 (182)
Aerobic aquatic 44103530 3.0 C (32) 3.0 C (32)

Anaerobic

aquatic 44192604 40.1 D (252) water 5.0 D ( 70 ) sediment 40.8 D (365) Total

TFD A,B 44630601 44103531 -- 9 (8) -- n.d. (148) 8

- Cl
chlorohydroxy diclosulam

SMILES: ClC1=C(C(=CC=C1)Cl) N([S](=O)(=O)C3=N[N ]2C(=NC(=C(C2=N3)Cl )F)O[H])[H] N

- (2,6

- dichlorophenyl)

- 8

- chloro

- 7

- fluoro

5(6H)

- oxo[l,2,4]triazolo[l,5

- c]

- pyrimidine

- 2

- sulfonamide Hydrolysis 43441043

-- -- Aqueous photolysis 43441044

-- -- Soil photolysis 44192603

-- --
Aerobic soil 43441045 44045201 15 (182) 15 (182)
Aerobic aquatic 44103530

-- -- Anaerobic

aquatic 44192604

-- --

### 5 Code Name/ Synonym Chemical Name Chemical Structure Study Type Ref. (MRID) Maximum %AR (day) A Final %AR (study length)

TFD A,B 44630601 44103531 -- 5 (42) -- n.d. (148) TAAA

diclosulam triazoloacetic acid or XDE

- 564 triazoloacetic acid

SMILES: ClC1=C(C(=CC=C1)Cl) N([S](=O)(=O)C2=N[N ](C(=N2)CC(=O)O[H])[ H])[H] N

- (2,6

- dichloropheny1)

- 3

- [1,2,4]triazoloacetic acid

- 5

- sulfonamide Hydrolysis 43441043 59.8 C (4) 59.8 C (4) Aqueous photolysis 43441044 -- --
Soil photolysis 44192603

-- --
Aerobic soil 43441045 44045201 -- -- Aerobic aquatic 44103530 2. 4 C (32) 2. 4 C (32)

Anaerobic

aquatic 44192604 3 6

. 8 D (365) water 4 .9 D (365) sediment 41.5 D (365) Total

TFD A,B 44630601 44103531 -- 5 (61) -- n.d. (148) ASTP
aminosulfonyltriaozlopy rimidine

SMILES: N([S](=O)(=O)C2=N[N ]1C(=NC(=CC1=N2)F) OCC)([H])[H] 5

- ethoxy

- 7

- fluoro[l,2,4]triazolo[l, 5

- c]pyrimidine

- 2

- sulfonamide Hydrolysis 43441043

-- -- Aqueous photolysis 43441044

-- -- Soil photolysis 44192603 9.7 C (2 0 ) 9 .0 C (30)

Aerobic soil 43441045 44045201 15.8 (56) 8.1 (182)
Aerobic aquatic 44103530

-- -- Anaerobic

aquatic 44192604

-- --

TFD A,B 44630601 44103531 10 (119) 39 (7) n.d. (364) 4 (150) TPSA
triazolopyrimidinesulfon ic acid

SMILES: [S](=O)(=O)(C2=N[N]1 C(=NC(=CC1=N2)F)O CC)O[H] 5

- ethoxy

- 7

- fluoro[l,2,4]triazolo[l, 5

- c]pyrimidine

- 2

- sulfon ic acid Hydrolysis 43441043

-- -- Aqueous photolysis 43441044 8.8 (30) 8.8 (30)
Soil photolysis 44192603 4.9 C (30) 4.9 C (30)

Aerobic soil 43441045 44045201 -- -- Aerobic aquatic 44103530

-- --

### 6 Code Name/ Synonym Chemical Name Chemical Structure Study Type Ref. (MRID) Maximum %AR (day) A Final %AR (study length) Anaerobic

aquatic 44192604

-- --

TFD A,B 44630601 44103531 -- 7 (14) -- n.d. (148) Imidate SMILES: ClC1=C(C(=CC=C1)Cl) N([S](=O)(=O)C2=N[N ](C(=N[H])OCC)C(=N2 )CC(=O)O[H])[H] 2

- (3

- (N

- (2,6

- dichlorophenyl )sulfamoyl)

- 1

- (ethoxy(imino) methyl)

- 1H

1,2,4

- triazol

- 5

- yl)acetic acid Hydrolysis 43441043 28.1 C (2) 21.6 C (4) Aqueous photolysis 43441044

-- -- Soil photolysis 44192603

-- --
Aerobic soil 43441045 44045201 -- -- Aerobic aquatic 44103530

-- -- Anaerobic

aquatic 44192604

-- --

TFD B 44630601 44103531 -- -- CO 2 Carbon dioxide Hydrolysis 43441043

-- -- Aqueous photolysis 43441044

-- -- Soil photolysis 44192603 11. 7 C (30) 11. 7 C (30)

Aerobic soil 43441045 44045201 45.4 (365) 45.4 (365)
Aerobic aquatic 44103530 0. 7 C (32) 0

. 7 C (32)
Anaerobic

aquatic 44192604

-- --

TFD A,B 44630601 44103531 -- --
A n.d. means “not detected”. B Terrestrial field study percentages represent the ratio of degradate concentration to the maximum parent concentration, both in the top layer of soil. C Values updat ed in agreement with registrant’s suggestions

. D Values updated based o n re

- examination of study report

.

## 5. Pages 6

- 7, Drinking Water Exposure Assessments Maximum EDWCs for diclosulam are shown below. Maximum EDWCs for diclosulam from page 7 of the EFED Problem Formulation

Drinking Water Source (Model Used) Use (rates modeled) Maximum Estimated Drinking Water Concentration (EDWC) Acute ( μg/L ) Chronic ( μg/L ) Cancer ( μg/L ) Surface water (SWCC: MSsoybeanSTD scenario, ground

application) 0.0315 lb a.i./A/yr 4.44 0.874 0.261

Groundwater (PRZM

GW) 0.0315 lb a.i./A/yr (soybeans, NC Norfolk loamy sand soil:

cotton) 15.8 11.0 11.0



## DAS’s C omment: The memorandum communicating the Diclosulam Drinking Water Assessment for Registration Review dated March 19, 2015 was obtained from EPA and reviewed. DAS notes that the assessment is described as a screening

- level assessment that used the exposure models SWCC, version 1.106, PRZM

- GW and SCI

- GROW, version 2.3 to estimate concentrations of diclosulam in drinking water derived from surface water and groundwater sources. Alth ough we question the accuracy of these predictions, assuming that they are much larger than those that would be measured in actual environmental samples as is typical for the output from these screening

- level models and scenarios, DAS agrees that the model s were used appropriately in a conservative, lower tier of risk assessment because the dietary risk assessment passed and no exposure refinements were necessary to develop realistic EDWCs suitable for higher

- tier quantitative risk assessment.

EFED’s R esponse: EFED thanks the registrant for their comment.

6. The Problem Formulation states on page 8, with regard to the field dissipation study (MRID 44103531): The study was found not to meet Subdivision N Guidelines, in part because complete data were not provided for soil samples below the 15 cm depth, thus data were insufficient to determine the extent of leaching for parent and degradates.

DAS’s C omment: I

t is not clear why the study did not meet Subdivision N Guidelines. The data presented in Table XXI of the study report clearly show the extent of leaching for parent and all degradates with significant formation fractions. DAS requests the DER for this study be provided so that we can give a more detailed response, or that more detail is provided on how EPA determined the guidelines were not met

.

## Page 8 of 10 EFED’s R esponse: The DER in question states that “ complete tabular data were not reported for soil samples below the 0

- to 15

- cm depth , ” and mentions additional reasons why the study does not meet guideline requirement s

. For example , the study was n o t conducted under typical use conditions, the c ompound was not applied at max imum label rate s , and storage stability data were inadequate. In response to DAS’ request, OPP will provide a copy of this DER to the registrant

.
7. The PF states, in the Stressors of C oncern section: “ ECOSAR (v 1.11) results indicate that the 5

- OH and 8

- Cl degradates may exhibit toxicity to daphnid that is similar to that of parent diclosulam .”

DAS’s C omment: It is generally recognized that ECOSAR toxicity predictions are highly uncertain for pesticides and their degradates due to the lack of such examples in the data set used to develop the predictive models

. Regardless, parent toxicity is low for all animals tested, and even if the toxophore remains in the degradates, it is unlikely they will exhibit greater toxicity than the parent molecule.

EFED’s R esponse: EFED uses ECOSAR, a computer program developed within the regulatory constraints of the Toxic Substances Control Act (TSCA) that uses structure

- activity relationships, chemical class

- specific regression equations between log K OW 

## and measured toxicity values, and acute

to

- chr onic ratios 2



## . As stated in EFED’s Problem Formulation, high levels (up to 51%) of residues in the aerobic soil metabolism study were unextracted and uncharacterized, and the possibility that some of these could have consisted of parent diclosulam cannot be ruled out. Therefore, i n accordance with EFED’s guidan ce for addressing unextracted residues 3



## , EFED plans on including unextracted residues together with the parent compound in the ecological aquatic exposure modeling unless data are provided which identif y the unextracted residues or demonstrate that adequat e measures were used to try to extract the residues.
Further, as stated in the guidance 3 

## “ If additional evidence is not available, the registrant has the option of conducting an additional study on the single soil or sediment with high levels of unextracted residues, using a range of solvents with different dielectric constants, including the solvents used in previously submitted studies for comparison. If the information provided for the single soil or sediment indicate that the unextracted resi dues can be considered strongly sorbed, then this information may be inferred to apply to any other soils or sediments with high unextracted residues, in most cases. If the additional data for the single soil or sediment indicate that unextracted residues cannot be considered strongly sorbed, then data may be needed for additional soils or sediments with high unextracted residues ”

.
8. DAS’s C omment: The DER for MRID 44192605 (mallard duck) appears to have different verified statistical results from those rep orted in the study report for the lower doses of 50, 125, and

2 ECOSAR is found at: http://www.epa.gov/oppt/newchems/tools/21ecosar.htm 3 http://www2.epa.gov/pesticide

- science

- and

- assessing

- pesticide

- risks/guidance

- addressing

- unextracted

- pesticide

- residues

## Page 9 of 10 500 ppm tested in phase II of the study for the eggshell thickness endpoint. Table 5 in the study report indicates statistically significant differences from the control were found at p < 0.01 f or the 125 and 500 ppm doses, but no significant difference was found for the 50 ppm dose using Dunnett’s test. However, in the DER table giving verified statistical results (Phase II

– Statistically Significant Endpoints), levels at which the effect was observed according to Dunnett’s test were 50, 125, and 500 ppm. It is not clear whether this difference is due to a recalculation or is simply an error in summarizing the test report findings. DAS requests that EFED assess the DER and study report to deter mine the reason for the difference between the findings of the reviewer and study authors. If the original reported NOAEC of 50 ppm is verified, DAS further requests that EFED accept the NOAEC, upgrade the study classification from supplemental to acceptab le, and waive the request for a new mallard reproduction study.
EFED’s Response: EFED routinely conducts an independent statistical analysis of data submitted to the Agency, and these independently determined results are reported in the Data Evaluation R ecord (DER). In response to the registrant’s comment, EFED examined the DER for MRID 44192605 and confirmed that the statistical results were correctly reported by the reviewer. EFED’s analysis was conducted using Statistical Analysis Software (SAS) and the standard alpha

- level ( α ) of 0.05. As further verification, EFED re

- analyzed the data for eggshell thickness (Phase II) using recently implemented statistical software ( CETIS ) and again confirmed a significant difference between the negative control and all treatment groups, including the 50 ppm dose group using Dunnett’s test ( p <0. 03 ) and William’s test ( p <0.05). The CETIS statistical report is attached to this memo. There is uncertainty regard ing which alpha

- level was used by the registrant to identify statistically significant differences, as this wa s not identified in the statistical methods section of the report, and different values we re indicated in the text (p<0.01) versus the tables (p<0 .05). Ultimately , EFED reiterates the need for a new avian reproduction toxicity study with mallard duck since

a definitive NOAEC was not identified in the original study.

9. DAS’s C omment: The risk assessment schemes described in the new guidance are inten ded for produ cts that are applied to foliage and those that are applied to soil or as seed treatments. Diclosulam is applied only to soil, has been shown not to be systemic (soybean nature of residue study, MRID 44103504), and is unable to be transported t o pollen and nectar. The previously submitted acute contact honey bee study reported an LD 50 

## >25 μg a.i./bee, practically non

toxic (MRID 43441019). A new acute oral honey bee study for a combination product (diclosulam + halauxifen

- methyl) reported an LD 50 

## >217 μg product/bee, or >124 μg diclosulam/bee. This study can be submitted, if requested. Furthermore, please note that diclosulam is only sold on peanuts, and on average, is only used on approximately 200,000 acres of peanuts a year, with the amount o f acres treated remaining relatively flat over the past 5 years. Based on the limited use pattern, and the small acres, the risk of pollinator exposure to diclosulam is negligible. In this particular case, additional data should not be required to perform a risk assessment, as bees/pollinators would not be exposed to diclosulam based on the fact diclosulam is soil applied to a small acreage of peanuts, is non

systemic and is deemed practically non

- toxic from an acute contact perspective. Due to the nature o f the molecule, additional data or label mitigation will not have an impact on overall

## Page 10 of 10 pollinator health within the US. In summary, there is no reasonable potential for exposure to the pesticide identified and, according to the guidance, no requirement to conduct a risk assessment. Even if exposure were possible, it is highly unlikely toxicity would be found in additional testing. The recommended studies are not needed, and DAS requests they be waived from further consideration.

EFED’s Re s ponse : As state d in the Problem Formulation, w hile an acute contact toxicity study on honey bees has been submitted, an acute oral toxicity study on honey bees is needed , as well as an acute larval honey bee toxicity study, a chronic adult honey bee toxicity study and a chronic larval honey bee toxicity study. Exposure to soil dwelling bees may occur as the result of diclosulam use on peanuts

. A 2012 census by the USDA National Agricultural Statistics Service (Crop Production and Crop Values) reported 1,042,000 bearing acres of peanuts in the United States. According to a USDA publication on the attractiveness of various crops to pollinators 4



## , peanut crops are attractive under certain conditions to honey bees ( Apis mellifera ) , bumble bees ( Bombus sp), and solitary bees ( e.g ., Lasioglossum sp. , Megachile sp. , Anthidium sp. , and N o mia sp. ) Bumble bees and solitary bees commonly nest in the ground or, as with Anthidium sp., use soil (mud) in the construction of their nests 5



## . Other s oil

- dwelling bees, such as the s outheastern blueberry bee ( Habropoda laboriosa ) are prevalent in the southeastern U.S. 6 

## where diclosulam is used. As stated in the pollinator guidance 7 

## , EFED’s pollinator toxicity data use the honey bee ( Apis mellifera ) as a surrogate for non

- Apis bees. Honey bee semi

- field test and a study on f ield residues in pollen and nectar as well as f ield testing for pollinators (with TEP ; 850.3040 ) are held in reserve depending on the results of the acute and chronic larval and adult honey bee studies. In the absence of data, EFED will be unable to complete a quantitative risk assessment for terrestrial invertebrates (specifically, insect pollinators).

Attached: CETIS Results Output for Avian Reproduction Study

4 USDA

. 2015. Attractiveness of a gricultural c rops to p ollinating b ees for the c ollection of n ectar and/or p ollen. Available

on on

- line at: http://www.ree.usda.gov/ree/news/Attractiveness_of_Agriculture_crops_to_pollinating_bees_Report

FINAL.pdf

. 5 European Food Safety Authority, 2013. EFSA Guidance Document on the risk assessment of plant protection products on bees (Apis mellifera, Bombus spp. and solitary bees). Appendix D. EFSA Journal 2013; 11(7):3295, 266 pp., doi: 10.2903/j.efsa.2013.3295. 6 http://www.fs.usda.gov/Internet/FSE_DOCUMENTS/stelprdb530 6468.pdf 7 http://www2.epa.gov/sites/production/files/2014

- 06/documents/pollinator_risk_assessment_guidance_06_19_14.pdfReport Date: 02 Nov-15 11:15 (p 1 of 4) Test Code: 129122 44192605 | 20-8625-1640 

### CETIS Analytical Report

OCSPP 850.2300 Chronic Avian Reproduction Wildlife International

Analyzed: 02 Nov-15 10:53 Endpoint: 10 Eggshell Thickness CETIS Version: CETISv1.9.0 Analysis ID: 00-2929-1491 Analysis: Parametric-Control vs Treatments Official Results: Yes

Sample ID: 01-6783-6092 Sample Date: 23 Dec-94 Receipt Date: Code: 44192605

Sample Age: 24h Source: DowElanco Station: Client: EPA OCSPP EFED Project: Herbicide Material: Diclosulum Batch ID: 00-4883-7859 Start Date: 24 Dec-94 Ending Date: Test Type: Chronic Avian Repro

Duration: n/a Protocol: OCSPP 850.2300 Chronic Bird Diluent: Brine: Species: Anas Platyrhynchos Source: Whistling Wings, Inc. Analyst: M. Clock-Rust

Age:

Comments: Rerunning eggshell thickness for MRID 44192605 to respond to registrant's comments regarding the determined NOAEC. No NOAEC was found in first phase, and so a second phase was initiated. This data is the from the second phase of the study. 44192605

Test Stat Critical P-Value Decision(α:5%) MSD vs Control Control II Dunnett Multiple Comparison Test P-Type DF 2.344 2.101 0.019 0.0292 Significant Effect 50* Negative Control 27 CDF 3.949 2.101 0.019 3.2E-04 Significant Effect 125* 27 CDF 6.955 2.101 0.018 6.3E-07 Significant Effect 500* 28 CDF NOEL LOEL TU TOEL Alt Hyp Data Transform PMSD 50 50 4.66% n/a C > T Untransformed <

ANOVA Table
Source Sum Squares Mean Square DF F Stat P-Value Decision(α:5%) Between 0.0294919 0.0098306 3 17.19 <1.0E-37 Significant Effect Error 0.0320263 0.0005719 56

0.0615182 59 Total

Distributional Tests
Attribute Test Test Stat Critical P-Value Decision(α:1%) 1.558 11.34 0.6689 Equal Variances Variances Bartlett Equality of Variance Test 0.9814 0.9459 0.4909 Normal Distribution Distribution Shapiro-Wilk W Normality Test

Mean Min Max Median Count Code Std Err Conc-ppm CV% %Effect 95% LCL 95% UCL 10 Eggshell Thickness Summary

0.3944 0.351 0.427 0.3925 0 14 0.005683 5.39% 0.00% 0.3822 0.4067 N 0.3736 0.34 0.42 0.37 50 15 0.005299 5.49% 5.28% 0.3622 0.385 0.3593 0.309 0.401 0.359 125 15 0.006591 7.10% 8.90% 0.3452 0.3735 0.3336 0.268 0.372 0.337 500 16 0.00681 8.17% 15.43% 0.319 0.3481

Code Conc-ppm 10 Eggshell Thickness Detail Rep 1 Rep 2 Rep 3 Rep 4 Rep 5 Rep 6 Rep 7 Rep 8 Rep 9 Rep 10 0 N 0.427 0.372 0.391 0.409 0.393 0.402 0.389 0.427 0.4 0.372 0.351 0.383 0.414 0.392 50 0.381 0.37 0.364 0.406 0.358 0.42 0.386 0.376 0.34 0.361 0.37 0.381 0.346 0.375 0.37 125 0.395 0.359 0.359 0.357 0.342 0.337 0.384 0.309 0.32 0.364 0.354 0.401 0.357 0.374 0.378 500 0.345 0.334 0.345 0.354 0.317 0.339 0.372 0.345 0.268 0.358 0.329 0.372 0.335 0.313 0.314 0.297

CETISTM v1.9.0.18 002-350-533-0 QA:________ Analyst:________Report Date: 02 Nov-15 11:15 (p 2 of 4) Test Code: 129122 44192605 | 20-8625-1640 

### CETIS Analytical Report

OCSPP 850.2300 Chronic Avian Reproduction Wildlife International

Analyzed: 02 Nov-15 10:53 Endpoint: 10 Eggshell Thickness CETIS Version: CETISv1.9.0 Analysis ID: 00-2929-1491 Analysis: Parametric-Control vs Treatments Official Results: Yes

Centered Untransformed

Rankits

-0.01

-0.02

-0.03

-0.04

-0.05

-0.06

-0.07 0.00 0.01 0.02 0.03 0.04 0.05

-0.5 -1.0 -1.5 -2.0 -2.5 0.0 0.5 1.0 1.5 2.0 2.5 10 Eggshell Thickness

Conc-ppm Reject Null

0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 0.45

0 N 50 125 500 Graphics

CETISTM v1.9.0.18 002-350-533-0 QA:________ Analyst:________Report Date: 02 Nov-15 11:15 (p 3 of 4) Test Code: 129122 44192605 | 20-8625-1640 

### CETIS Analytical Report

OCSPP 850.2300 Chronic Avian Reproduction Wildlife International

Analyzed: 02 Nov-15 11:13 Endpoint: 10 Eggshell Thickness CETIS Version: CETISv1.9.0 Analysis ID: 20-5233-6485 Analysis: Parametric-Control vs Ord.Treatments Official Results: Yes

Sample ID: 01-6783-6092 Sample Date: 23 Dec-94 Receipt Date: Code: 44192605

Sample Age: 24h Source: DowElanco Station: Client: EPA OCSPP EFED Project: Herbicide Material: Diclosulum Batch ID: 00-4883-7859 Start Date: 24 Dec-94 Ending Date: Test Type: Chronic Avian Repro

Duration: n/a Protocol: OCSPP 850.2300 Chronic Bird Diluent: Brine: Species: Anas Platyrhynchos Source: Whistling Wings, Inc. Analyst: M. Clock-Rust

Age:

Comments: Rerunning eggshell thickness for MRID 44192605 to respond to registrant's comments regarding the determined NOAEC. No NOAEC was found in first phase, and so a second phase was initiated. This data is the from the second phase of the study. 44192605

Test Stat Critical P-Value Decision(α:5%) MSD vs Control Control II Williams Multiple Comparison Test P-Type DF 2.344 1.673 0.015 <0.05 Significant Effect 50* Negative Control 27 CDF 3.949 1.748 0.016 <0.05 Significant Effect 125* 27 CDF 6.955 1.772 0.016 <0.05 Significant Effect 500* 28 CDF NOEL LOEL TU TOEL Alt Hyp Data Transform PMSD 50 50 3.93% n/a C > T Untransformed <

ANOVA Table
Source Sum Squares Mean Square DF F Stat P-Value Decision(α:5%) Between 0.0294919 0.0098306 3 17.19 <1.0E-37 Significant Effect Error 0.0320263 0.0005719 56

0.0615182 59 Total

Distributional Tests
Attribute Test Test Stat Critical P-Value Decision(α:1%) 1.558 11.34 0.6689 Equal Variances Variances Bartlett Equality of Variance Test 0.9814 0.9459 0.4909 Normal Distribution Distribution Shapiro-Wilk W Normality Test

Mean Min Max Median Count Code Std Err Conc-ppm CV% %Effect 95% LCL 95% UCL 10 Eggshell Thickness Summary

0.3944 0.351 0.427 0.3925 0 14 0.005683 5.39% 0.00% 0.3822 0.4067 N 0.3736 0.34 0.42 0.37 50 15 0.005299 5.49% 5.28% 0.3622 0.385 0.3593 0.309 0.401 0.359 125 15 0.006591 7.10% 8.90% 0.3452 0.3735 0.3336 0.268 0.372 0.337 500 16 0.00681 8.17% 15.43% 0.319 0.3481

Code Conc-ppm 10 Eggshell Thickness Detail Rep 1 Rep 2 Rep 3 Rep 4 Rep 5 Rep 6 Rep 7 Rep 8 Rep 9 Rep 10 0 N 0.427 0.372 0.391 0.409 0.393 0.402 0.389 0.427 0.4 0.372 0.351 0.383 0.414 0.392 50 0.381 0.37 0.364 0.406 0.358 0.42 0.386 0.376 0.34 0.361 0.37 0.381 0.346 0.375 0.37 125 0.395 0.359 0.359 0.357 0.342 0.337 0.384 0.309 0.32 0.364 0.354 0.401 0.357 0.374 0.378 500 0.345 0.334 0.345 0.354 0.317 0.339 0.372 0.345 0.268 0.358 0.329 0.372 0.335 0.313 0.314 0.297

CETISTM v1.9.0.18 002-350-533-0 QA:________ Analyst:________Report Date: 02 Nov-15 11:15 (p 4 of 4) Test Code: 129122 44192605 | 20-8625-1640 

### CETIS Analytical Report

OCSPP 850.2300 Chronic Avian Reproduction Wildlife International

Analyzed: 02 Nov-15 11:13 Endpoint: 10 Eggshell Thickness CETIS Version: CETISv1.9.0 Analysis ID: 20-5233-6485 Analysis: Parametric-Control vs Ord.Treatments Official Results: Yes

Centered Untransformed

Rankits

-0.01

-0.02

-0.03

-0.04

-0.05

-0.06

-0.07 0.00 0.01 0.02 0.03 0.04 0.05

-0.5 -1.0 -1.5 -2.0 -2.5 0.0 0.5 1.0 1.5 2.0 2.5 10 Eggshell Thickness

Conc-ppm Reject Null

0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 0.45

0 N 50 125 500 Graphics

CETISTM v1.9.0.18 002-350-533-0 QA:________ Analyst:________