Re: Fw: Declassified reviews of studies on Pigment Blue (1324-76-1) Notes Link

Ryan Wallace to

: Jeffrey Santacroce 

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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1200 Pennsylvania Ave. NW 

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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY 

WASHINGTON D.C., 20460 

VIA FACSIMILE: 201-437-4801 

April 19,2012 

Attention: Glenn Merritt (201-437-4000) 

OFFICE OF 

PREVENTION, PESTICIDES AND 

TOXIC SUBSTANCES 

Subject: Follow-up to fax transmission of 4/13/12 (ePMA removal ofCBI claims regarding 

identified studies) 

Dear Mr. Merritt: 

This is sent to you pursuant our conversation of several minutes ago. In Larry Robinson's fax of 

April 13th while there is a waiver of confidential business information (CBI) claims in the 

identified studies there is a an assertion of copyright protections and some additional text that 

provides in part ... "Reproduction, reference, summarization, retransmission or other use of this 

copyrighted document. .. including electronic transmission, using the internet or email .... 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 per the 

TSCA activity are not to be made available in an Agency e-docket (electronic docket) or be 

included in EPA websites among the collection of TSCA health 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 of non-CBI materials submitted by entities subject to TSCA 

regulations (including the posting of such materials on government websites) and submitted by 

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 of the studies. 

Can you please confirm CPMA's intent? Many thanks. 

Scott M. Sherlock, Attorney Advisor 

Environmental Assistance Division 

Office of Pollution Prevention and Toxics 


SRC 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

SE RTYINFORWTIONJ (E.O. 120a) SECURITY ON (E.O. 1206t'

5,25938
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)

March 2010

Submitted to:

High Production Volume Chemicals Branch

Risk Assessment Division

Office of Pollution 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 22202
PREPARATION OF THE DATA ADEQUACY ASSESSMENT

This document contains the review of a 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 professional judgment 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. If the study

was determined to be inadequate, a basis for that conclusion is supplied. For studies already

assigned Klimisch codes, an explanation is provided if the reviewer's assessment of data

adequacy differed from the pre-assigned Klimisch code.

A detailed evaluation of the test report and study conduct is provided at the end of the

summary document in a section entitled "Review of TSCA 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 of appropriate controls and test substances.

Any deficiencies in the descriptions of the 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 of the 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 of exposure was 72 hours, rather than the ASTM E 121 8-specified 96-hour

duration. Additionally, the mean measured concentration of the 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 of test solution preparation was used in a Daphnia toxicity study and

resulted in a mean measured concentration of 0.048 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 of exposure 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 of 0 (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 of magnetic stirring of 100 mg/L C.I. Pigment

Blue 61 to reach maximum solubility of the 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 OECD
TG 201 was used in tap water purified by Reverse Osmosis (Milli-Q water).

Six replicates in I100-mL glass vessel containing 5 0 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 104 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 of dilution 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 and the end of the exposure period.

Statistical analysis of the data was not needed for growth rate reduction as the effects recorded

were not significant (<1 0%). 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 of 227 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 of yield was found for

the limit concentration.

CONCLUSIONS

No reduction of growth rate and less than 50% inhibition of yield 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 of the test substance rather than by toxicity. Based on study methods, BC2 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 of the 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 of test solution preparation was used in a Daphnia toxicity study and

resulted in a mean measured concentration of 0.048 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.):

Part I. Test Report and Study Conduct

Enter one of the followinp, codes into each of the checkboxes 1 through 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 of gross, unauthorized or undocumented 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 of deviations from the "should" statements in the study protocol

that may have a bearing on the study conclusions. List these in comments below.

[D] 3. Approved modifications of test 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 of Quality Assurance (QA) inspections, their dates, and findings were missing or not 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 or unclear; use of unhealthy 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 of other discrete

observations pertinent to the type of study 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

Part A. 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. If repeated, 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 other purpose (e.g., dose-setting). [xi

9. The data are not useful for any purpose (describe in notes below). [

Reviewer Comments (continue on separate page, if needed):

"Must" violation: The study used a 72-hour duration instead of the ASTM E 1218 specified 96-hour duration.

Data Reliability: The method of test solution preparation is questionable because (1) the mean measured

concentration of the test solution (0.422 mg/L) exceeded the referenced solubility limit of 0.0025 mgIL (Clariant,

SU-Technology and Innovation Management, Pigment Analytics) and (2) the same method was used in the Daphnia

toxicity study and resulted in a mean measured concentration of 0.048 mg/L. Therefore, it is unclear if the results of

the algal toxicity test would be the same if the test was repeated.

Other notes: Although the initial inoculumn (1 x 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 is unlikely 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:,~

Part B. 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. Thestudy may not be acceptable [

(provide rationale in memo to CITB chief).

43
SRC Document Receipt

Documents Logged Out to US EPA's CBIC on March 15, 2010 by J. Garey

CASE No. Document Description

JGO3151Oa HPV1 Data Adequacy Review Document Referencing EPA DCN No. 40090000007 and

40090000009 (algae) O 5 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 pa. .\-

Document count: 3