Re: Fw: Declassified reviews of studies on Pigment Blue (1324-76-1) Notes Link Ryan Wallace to : Jeffrey Santacroce 05/31/2012 03:45 PM
Cc : Catherine Roman, Scott Sherlock

From: Ryan Wallace/DC/USEPA/US To: Jeffrey Santacroce/DC/USEPA/US@EPA Cc: Catherine Roman/DC/USEPA/US@EPA, Scott Sherlock/DC/USEPA/US@EPA
I reviewed the documents with DCNs 40100000011, 40100000012, and 40100000013. Each of these documents is a review of a study or studies provided by the Color Pigment Manufacturers Association, Inc. (CPMA). The confidential business information (CBI) claims in the studies which these reviews reference were declassified by CPMA in a 4/13/2012 letter from J. Lawrence Robinson, President of CPMA, to Scott Sherlock of EPA. Because the studies referenced in the documents with DCNs 40100000011, 40100000012, and 40100000013 are no longer considered as CBI, the reviews are also no longer considered to be CBI. Ryan P. Wallace, Attorney Advisor Environmental Assistance Division Office of Pollution Prevention and Toxics (202) 564
-8824 wallace.ryan@epa.gov

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## - ntUNITED STATES ENVIRONMENTAL PROTECTION AGENCY WASHINGTON D

.C., 20460

VIA FACSIMILE: 201-437-4801 April 19,2012 Attention: Glenn Merritt (201-437-4000) OFFICE OF PREVE NTION, PESTICIDES AND TOXIC SUBSTANCES

Subject: Follow-up to fax transmission of4/13/12 (ePMAremoval ofCBI claimsregarding identified studies) 

### Dear Mr. Merritt: This is sent to you pursuant our conversation ofseveral minutes ago. In Larry Robinson's fax of April 13th while there is a waiver ofconfidential business information (CBI) claims in the identified studies there is a an assertion ofcopyright protections and some additional text that provides in part ... "Reproduction, reference, summarization, retransmission or other use ofthis copyrighted document.
..including electronic transmission, using the internet oremail
....is strictly prohibited
...." While we understand the basis for the copyright protections, we have a concern that the language in the fax might be interpreted to mean that ePMA is asserting that the studies submitted perthe TSCA activity are not to be made available in an Agency e-docket (electronic docket) orbe included in EPA websites among the collection ofTSCAhealth and safety studies. We are thinking that the identified limitations noted in the fax are not intended to apply to EPA's normal procedures for the handling ofnon-CBI materials submitted by entities subject to TSCA regulations (including the posting ofsuch materials on government websites) and submittedby such entities in order to comply with a TSCA requirement, but are rather intended to limit entities outside the government from the unauthorized use or appropriation ofthe studies. Can you please confirm CPMA's intent? Many thanks.

Scott M. Sherlock, Attorney Advisor Environmental Assistance Division Office ofPollution Prevention and ToxicsSRC TR-10-073

HPV1 TEST RULE
- DATA ADEQUACY ASSESSMENT

- Benzenesulfonic acid,[[4-[[4-(phenylamino)phenyl] [4-(phenylimino)-2,5-cyclohexadien- 1 - ylidene]methyl]phenyl] amino]-, CAS No. 1324-76-1 Toxicity to Plants (Algae) Prepared by: Kendra Moran, Teresa Manyin, and Joan D. Garey Environmental Science Center SRC, Inc. 7502 Round Pond Road North Syracuse, NY 13212
Contract No. EP-W-09-027 Task FGOO7.0.009.004
Submitted to: OPPT/RAD/HPVCB (7403M) U.S. Environmental Protection Agency 1200 Pennsylvania Avenue Washington, D.C. 20460 Elizabeth Margosches, Project Officer Meena Sonawane, Work Assignment Manager David Brooks, Alternate Work Assignment Manager March 15, 2010

FTSCA QNWMTIAL 

# 3USIES JAATION D~ SNOT IfA JTIONA 

### DOES NOT CONTAIN 

### NATIONAL SERTYINFORWTIONJ (E.O. 120a) SECURITY ON 

### (E.O. 1206t' 

### 5,25938HPV1 Test Rule
- Data Adequacy Assessment

Benzenesulfonic acid, [[4-[[4-(.phenylamino)phenyl] [4-(phenylimino)-2,5-cyclohexadien- 1 - ylidene]methyl]phenyl] amino]-, CAS No. 1324-76-1 Toxicity to Plants (Algae)

March 2010

Submitted to: High Production Volume Chemicals Branch Risk Assessment Division Office ofPollution Prevention and Toxics Environmental Protection Agency WAM: Meena Sonawane Alternate WAM: David Brooks 1200 Pennsylvania Avenue, NW

Washington, DC 20460-000 1
Prepared By:

SRC, Inc. Environmental Science Center 2451 Crystal Drive, Suite 804 Arlington, VA 22202PREPARATION OF THE DATA ADEQUACY ASSESSMENT This document contains the review ofa toxicity study conducted in response to the first HPV TSCA Section 4 Test Rule (71 FR 13708, March 16, 2006). Using the applicable test guideline and professionaljudgment as guides, the study was reviewed for adequacy and evaluated for compliance with the test guideline. (The applicable test guideline is not always the test guideline required by the test rule, because some test sponsors requested and received approval from EPA to use a different guideline.) The study was summarized according to a standard format, assessed for adequacy, and assigned a Klimisch reliability code. Ifthe study was determined to be inadequate, a basis for that conclusion is supplied. For studies already assigned Klimisch codes, an explanation is provided ifthe reviewer's assessment ofdata adequacy differed from the pre-assigned Klimisch code. A detailed evaluation ofthe test report and study conduct is provided at the end ofthe summary document in a section entitled "Review ofTSCA Section 4 Final Study Report". Any deviations from the applicable test guideline are described. The study is also evaluated for compliance with Standard Operating Procedures, Good Laboratory Practice Standards, and Quality Assurance procedures, as well as the use ofappropriate controls and test substances. Any deficiencies in the descriptions ofthe study method, test system, animals studied, physical conditions, dosage information, individual animal data, calculations, and statistical analyses are described, and internal inconsistencies within the study report are identified. An overall assessment is provided for each ofthe following: study conduct, data reliability, and data utility.TOXICITY TO PLANTS (ALGAE) Title: Fresh water algal growth inhibition test with C.I. Pigment Blue 61 This study is: E Adequate Not Adequate The duration ofexposure was 72 hours, rather than the ASTM E 121 8-specified 96-hour duration. Additionally, the mean measured concentration ofthe limit test solution (0.422 mg/L) exceeded a previously measured water solubility limit (0.0025 mg/L) although no solvent was used; the same method oftest solution preparation was used in aDaphniatoxicity study and resulted in a mean measured concentration of0.048 mg/L. TEST SUBSTANCE Identity: C .1.Pigment Blue 61 (Benzenesulfonic acid,[[4- [[4-(phenylamino)phenyl] [4- (phenylimino)-2,5 -cyclohexadien- 1 -ylidene]methyl]phenyl] amino]-), CAS No. 1324-76-1 Remarks: 96.83% purity; dark blue powder with granules METHOD Method/guideline followed: OECD TG 201 (2006) Test type: Toxicity to Algae
- Static, Limit Test GLP compliant?: Yes Year study was performed: 2008 Test species Pseudokirchneriella subeapitata (green algae; strain: NIVA CLIL 1). Laboratory cultured with continuous aeration and exposure to light at 23 ± 2'C. Analytical monitoring: Yes. During the limit test, samples for analysis were taken from both the control and the limit concentration at the start, after 24 hours ofexposure and at the end of the test. The sample volume was 2 mL and samples were stored in a freezer until analysis. Exposure duration:72 hours Concentrations tested: Loading rates were 0 (control) and 100 mg/L, which corresponded to mean measured concentrations of0 (control) and 0.422 mg/L. Test method/conditions remarks:Test solution preparation involved a 10-minute treatment period with ultrasonic waves followed by 3 days ofmagnetic stirring of 100 mg/L C.I. Pigment Blue 61 to reach maximum solubility ofthe test substance in the test medium. Subsequently, the aqueous mixture was filtered through a membrane filter (Schleicher and Schuell, 0.45 pim). The resulting filtrate was observed to be clear and light blue. M2 growth media as specified in OECDTG 201 was used in tap water purified by Reverse Osmosis (Milli-Q water). Six replicates in I100-mL glass vessel containing 50 mL test solution were tested for each exposure level under continuous illumination (78 to 82 IE m s2 S) for 72 hours. The initial cell density was 10 4 cells/mL. Cell density (measured spectrophotometrically at 720 nm) was determined at the 0, 24, 48, and 72-hour observations. Additional positive control (potassium dichromate) groups were included in the testing scheme. Water hardness ofdilution water was 24 mg CaCO3/L. Temperature and p1H levels ranged from 21.9 to 23.9'C and 7.9 to 8.2, respectively, at the beginning andthe end ofthe exposure period. Statistical analysis ofthe data was not needed for growth rate reduction as the effects recorded were not significant (<10%). For yield inhibition, ANOVA and a 2 sample t-test were used. RESULTS Endpoint value(s): EC50 (yield) > 0.422 mg/L. Since effects based on yield were considered significant, 0.422 mg/L would be considered the lowest observed effect concentration (LOEC); however, a no observed effect concentration (NOEC) could not be determined. Results remarks: Positive and negative controls responded adequately. The control cell density increased by a factor of227 during the 72-hour exposure. Analysis at test initiation and termination indicated 0.549 mg/L and 0.342 mg/L test substance, respectively, in the test solution. Based on these results, the average exposure concentration was calculated to be 0.422 mg/L. The submitter speculated that undissolved test substance may have been present in test solution since measured concentrations exceed the maximum tested concentration in the daphnid study (0.048 mg/L) and the approximate water solubility (0.002-0.003 mg/L as indicated in the Octanol!Water Partition Coefficient Study). In treated cultures (0.422 mg/L), a 4.3% reduction in growth and a 20.9% reduction in yield were reported, in comparison to control rates. Statistically significant inhibition ofyield was found for the limit concentration. CONCLUSIONS No reduction of growth rate and less than 50% inhibition ofyield were recorded at 0.422 mg/L C.I. Pigment Blue 61 tested. Inhibition may have been affected by light absorption due to the coloring ofthe test substance rather than by toxicity. Based on study methods, BC 2 1 (yield) = 0.422 mg/L. Since effects based on yield were considered significantly different from controls, 0.422 mg/L would be considered the lowest observed effect concentration (LOEC); however, a no observed effect concentration (NOEC) could not be determined. STUDY RELIABILITY [3] Not reliable. The duration of exposure was 72 hours, rather than the ASTM E 1218-specified 96-hour duration. Additionally, the mean measured concentration ofthe limit test solution (0.422 mg/L) exceeded a previously measured water solubility limit (0.0025 mg/L) although no solventwas used; the same method oftest solution preparation was used in aDaphnia toxicity study and resulted in a mean measured concentration of0.048 mg/L. REFERENCE Bouwman, L.M. 2008. Fresh water algal growth inhibition test with C.I. Pigment Blue 61. NOTOX B.V. Testing Facility, NOTOX Project #488234._ _ _ _ _ _ _ _ _ _ _ __.._ . ....

Study Report CITB Project Manager: Catherine Roman Chemical Name: Benzenesulfonic acid, [4-[[4-(phenylamino)pheny] [4-(phenylimino)-2,5-cyclohexadien- 1 - ylidene]methyllphenyl]amino] - GAS Registry Number: 1324-76-1 Report Title: Fresh water algal growth inhibition test with C.I. Pigment Blue 61 Test Sponsor: Color Pigments Manufacturers Association, Inc. Testing Lab: NOTOX B.V. Test Standard: ASTM E 1218 Date Study Received by EPA: 1/18/08 Date Study Due to EPA: 5/17/07 Special Instructions (e.g., regarding approved protocol modifications, etc.):
PartI. Test Report and Study Conduct Enter one ofthe followinp,codes into each ofthe checkboxes 1through 13: Agree [AL. Disagree [D1, Not Applicable rNAl. or Cannot Determine [C1. and add comment, below, as needed [A] 1.The final study report indicates evidence ofgross, unauthorized orundocumented deviation from the EPA test standard requirements, including "shall," "must," or "will" violations. List significant test standard deviations and "shall," "must," or "will" violations in comments below. [D] 2. The final study report indicates evidence ofdeviations from the "should" statements in the study protocol that may have abearing on the study conclusions. List these in comments below. [D] 3.Approved modifications oftest standard or testing protocol (CITB3 PM describe or attach) were not followed or are inadequately documented. [D] 4. There is evidence that laboratory Standard Operating Procedures (SOPs) were inadequately followed. [D] 5.The Statement ofQuality Assurance (QA) inspections, their dates, and findings were missing ornot signed. There is evidence that QA procedures may be inadequate. [D] 6. There is evidence that Good Laboratory Practice Standards (GLPS) were inadequately followed. [D] 7.The test, control, or reference substances are different from that specified in the section 4 test rule or Enforceable Consent Agreement (ECA). [D] 8.Animal identification is inadequate orunclear; use ofunhealthy animals or other factors (e.g., deviations from temperature, lighting, dosing) are apparent. [D] 9.The final study report inadequately describes the study method. [D] 10. The final study report inadequately describes the test system.[D] 11. The final study report inadequately describes the dosage information. [D] 12. The final study report does not accurately reflect the individual animal data (or that ofother discrete observations pertinent to the type ofstudy conducted), or individual data were not provided. [D] 13. The final study report inadequately describes the calculations, interpolations, data transformations, statistical analyses, or modeling parameters used. Part 11. Conclusions Place a check mark beside the summar statement(s) that apply to this review and add comments below as appropriate PartA. To be filled out by Reviewer Study Conduct 1.The study was well-conducted. 

### [ 2. The study was generally well-conducted, with some minor[

deficiencies (list in notes below). 3. The study conduct was significantly deficient or questionable, (give [x]

reasons in notes below). Data Reliability 4. The study results are precise and accurate.[I 5. Appropriate methods were used to determine [x] statistical significance. 6. Ifrepeated, the test results would be expected to be the[ same. Data Utility 7. The data are useful for risk assessment for the endpoint tested. 8. The data are useful for some otherpurpose (e.g., dose-setting). [xi 9. The data are not useful for any purpose (describe in notes below). 

### [ Reviewer Comments (continue on separate page, ifneeded): "Must" violation: The study used a 72-hour duration instead ofthe ASTM E 1218 specified 96-hour duration. Data Reliability: The method oftest solution preparation is questionable because (1)the mean measured concentration ofthe test solution (0.422 mg/L) exceeded the referenced solubility limit of0.0025 mgIL (Clariant, SU-Technology and Innovation Management, Pigment Analytics) and (2) the same method was used in theDaphnia toxicity study and resulted in a mean measured concentration of0.048 mg/L. Therefore, it is unclear ifthe results of the algal toxicity test would be the same ifthe test was repeated. Other notes: Although the initial inoculumn (1x 104 cells/mL) was less than that specified in ASTM E 1218 (2 x 104 cells/mL) and algae nutrient medium was not as specified in ASTM E 1218 (OECD TG 201-specified medium was used instead), it isunlikely that these "should" violations have a bearing on the study conclusion. This is supported by the fact that cell density in control cultures increased by 227x during the 72-hour exposure period, which exceeds the minimum acceptable growth rate. Reviewer Name/Title/BranchlDivision/Ofice: Kendra Moran and Teresa Manyin, SRC Reviewer Signature:,~
PartB. To be filled out by CITH PM Tiered Testing Decision 1.The tiered testing trigger was met, additional testing is indicated. 

### [ (when applicable) 2. The trigger for additional (tiered) testing was.not met.[Study Acceptability 3. The study is acceptable. 

### [ 4. Thestudymay notbe acceptable 

### [ (provide rationale in memo to CITB chief).

43SRC Document Receipt Documents Logged Out to US EPA's CBIC on March 15, 2010 byJ.Garey

CASE No. Document Description JGO3151Oa HPV1 Data Adequacy Review Document Referencing EPA DCN No. 40090000007 and 40090000009 (algae) 

### 5 O 

### 3\ JG031510b HPV1 Data Adequacy Review Document Referencing EPA DCN No. 40090000007 and 40090000009 (Daphnia) 3'M\30\ JG031510c HPV1 Data Adequacy Review Document Referencing EPA DCN No. 40090000007 and 40090000009 (combined repeated-dose) -3 

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