Fw: TSCA test rule EPA–HQ–OPPT– 2007

–0531 requirement for aquatic toxicity (algae) testing - problems encountered in testing 9,10-anthracenedione, CAS # 84-65-1 Paul Campanella to: John Schaeffer, Marcus Aguilar 10/27/2011 10:59 AM
From: Paul Campanella/DC/USEPA/US To: John Schaeffer/DC/USEPA/US@EPA, Marcus Aguilar/DC/USEPA/US
FYI

Paul J. Campanella, Ph.D. Chemical Information and Testing Branch Chemical Control Division U.S. Environmental Protection Agency Washington, D.C. 202-564-8091 ----- Forwarded by Paul Campanella/DC/USEPA/US on 10/27/2011 10:58 AM -----
From: Jerry Cook <JACook@cpc-ga.com> To: Paul Campanella/DC/USEPA/US@EPA Date: 10/27/2011 10:53 AM Subject: TSCA test rule EPA–HQ–OPPT–2007

– 0531 requirement for aquatic toxicity (algae) testing - problems encountered in testing 9,10-anthracenedione, CAS # 84-65-1 

### Dear Dr. Campanella; This email will describe problems encountered in conducting aquatic toxicity (algae) testing on insoluble 9,10-anthracenedione, CASRN 84-65-1 (typically referred to as "AQ"). Chemical Products Corporation (CPC) contracted with Hydrosphere Research, 11842 Research Circle, Alachua, FL 32615-6817 to conduct ASTM 1218-04e1 on 9,10-anthracenedione. CPC further contracted with Case Consulting Laboratories, Inc. to determine the AQ concentration in water samples sent from Hydrosphere Research related to its conduct of ASTM 1218-04e1. Case Consulting Laboratories determined the water solubility of AQ in 2006; the final report which was submitted to EPA to satisfy TSCA test rule EPA-HQ-OPPT-2005-0033 is attached. The water solubility of AQ was determined to be 0.075 mg/l at 20 degrees C. Hydrosphere Research conducted ASTM 1218-04e1 and sent final water samples to Case Consulting Laboratories for determination of dissolved AQ in 6 water samples. Case found no detectable AQ in any of the water samples, Case stated in an email:

### "Peter, We ran all the samples you sent. N o anthraquinone was detected in any of the samples. The limit of detection of the method is somewhere around 50 p pb, so the samples are below that. Best regards, Dave David J. Sinning Vice President
Case Laboratories , Inc

. 622 Rt. 10 Whippany, NJ 07981 Tel. 973-428-9666 Fax 973-887-4419

From: Peter Meyer [ mailto : pmeyer@ hydrosphere

. net ] Sent: Wednesday, September 21, 2011 2:08 PM To: d

. sinning @ case
- labs

. com Subject: Samples going out today David, We are sending the samples today FedEx Std ON to the Whipany address on the COC. As I understand it we do not need to preserve the vials which would also imply that they do not need to be shipped on ice. If this is incorrect let me know. Thanks, Peter ><)))> ~~~ ><}}}> ~~~ ><]]]> ~~~ ><}}}> ~~~ ><)))> 

### Peter R. Meyer, Laboratory Manager Hydrosphere Research 11842 Research Circle Alachua, FL 32615-6817 T (386) 462-7889 F (386) 462-7264 www
. hydrosphere

. net " 

## We are discussing with Hydrosphere Research how best to proceed and

## would appreciate any suggestions you can provide. Thanks, Jerry Cook Mr. Cook, I am forwarding the response to your question that I received from Anne Kim, the lead technical reviewer. I hope this answers the remaining question. If not please contact me and perhaps we can set up a call between your technical staff and Ms. Kim to resolve any additional issues concerning this testing protocol.

Paul J. Campanella, Ph.D. Chemical Information and Testing Branch Chemical Control Division U.S. Environmental Protection Agency Washington, D.C. 202-564-8091 ----- Forwarded by Paul Campanella/DC/USEPA/US on 05/17/2011 11:34 AM

----- From: Anne Kim/DC/USEPA/US To: Paul Campanella/DC/USEPA/US@EPA Cc: John Schaeffer/DC/USEPA/US@EPA, David Brooks/DC/USEPA/US@EPA Date: 05/12/2011 01:05 PM Subject: Re: Fw: TSCA test rule EPA–HQ–OPPT–2007–0531 requirement for aquatic toxicity (algae) testing

Paul, The value 1.35 mg/L, I referenced, came from the HSDB website: http :// toxnet
. nlm

. nih

. gov / cgi

- bin / sis / search / f ? ./ temp / ~ UdRuo 1:1 , as well as from the EPA's EPI Suite model, as an experimental value for CASRN 84-65-1. Please note that the referenced water solubility value is 1.35 mg/L at 25 oC, and the sponsor's measured value is 74.6 μg/L (at 20 oC,pH=7). Of course, it would be fine to use the sponsor's measured water solubility of 74.6 μg/L, but please have the sponsor attach its water solubility study along with the submission of the algal test. This will explain the upper limit of the sponsor's algal study.

Thank you.
Anne Kim Acting Branch Chief, Existing Chemicals Assessment Branch Risk Assessment Division Office of Pollution Prevention and Toxics US Environmental Protection Agency EPA EAST 6334S 1200 Pennsylvania Avenue, NW (7403M) Washington, DC 20460 Phone: 202-564-7631 Fax: 202-564-7450

From: Paul Campanella/DC/USEPA/US To: Anne Kim/DC/USEPA/US@EPA Cc: John Schaeffer/DC/USEPA/US@EPA Date: 05/12/2011 10:15 AM Subject: Fw: TSCA test rule EPA–HQ–OPPT–2007–0531 requirement for aquatic toxicity (algae) testing

Anne, See the response below from Mr. Cook. It appears that a mistake was made in the response that RAD prepared. Can you verify this? And, if the response is incorrect, can you please provide the correct value?

Paul J. Campanella, Ph.D. Chemical Information and Testing Branch Chemical Control Division U.S. Environmental Protection Agency Washington, D.C. 202-564-8091 ----- Forwarded by Paul Campanella/DC/USEPA/US on 05/12/201110:12 AM

----- From: Jerry Cook < jcook @ cpc - us . com > To: Paul Campanella/DC/USEPA/US@EPA Cc: John Schaeffer/DC/USEPA/US@EPA Date: 05/12/2011 09:46 AM Subject: Re: TSCA test rule EPA–HQ–OPPT–2007–0531 requirement for aquatic toxicity (algae) testing

Dear Dr. Campanella; Thank you for the response to my questions sent in your 5/5/2011 email to me below. We understand that we are to test the aquatic toxicity (algae) of 9,10-anthracenedione, CAS # 84-65-1, up to this chemical's water solubility limit according to method ASTM 1218-04e1. However, an incorrect value for the measured water solubility of 9,10-anthracenedione is quoted in the response from your staff. My question and your staff's response: "9,10-anthracenedione is only sparingly soluble in water. Can testing be done at the concentration of a saturated solution? Yes . EPA notes that the measured water solubility is reported to be 1.35 mg/L. The test should be conducted up to the test chemical's water solubility limit....." The measured water solubility of 9,10-anthracenedione is only 74.6 micrograms per liter.

On February 15, 2007, Chemical Products Corporation submitted the studies required by final test rule EPA-HQ-OPPT-2005-0033 for 9,10-anthracenedione, CAS # 84-65-1. One of the tests reported was the measured water solubility of this chemical. The robust summary submitted with the studies states, “5.0 Water Solubility:Method C: 40 CFR 799.6784 (column elution) performed by Case Consulting Laboratories, Inc. and reported in Study No. 3320-02. Test Substance

Identity: 9,10-Anthracenedione (Anthraquinone) manufactured by the Friedel-Crafts process, 99.4% Purity.

Batch 1543-1-GESU5099797, sampled from a commercial shipment. Results Water Solubility (20 oC, pH=7): 74.6 μg/L Method Method/guideline followed: EPA Pesticide Assessment Guidelines Subdivision N, Section 161-1

Type (test type): Aqueous Hydrolysis at pH 5, 7, 9 (25°C)

GLP: Yes

Year: (study performed): 2006 Test Conditions Duration: 9 or 10 days (Two complete runs were conducted).

Statistical Methods: No statistical methods were employed. An excess of the test substance was coated on glass beads (100-200 μm). A jacketed column was charged with this mixture. Water, buffered at pH=7.0, was recycled through the column using a circulating pump and samples were drawn off daily for 9 or 10 consecutive days for analysis using the HPLC method described below. Two complete runs of the experiment were carried out. The first run employed a circulating pump flow rate of 26.4 ml/hour. The second run had a flow rate of 12.8 ml/hour.Results: At a flow rate of 26.4 ml/hour the solubility was determined to be 74.6 μg/L with a standard deviation of 4.5. At a flow rate of 12.8 ml/hour the solubility was determined to be 74.6 μg/L with a standard deviation of 1.5.”

Please confirm that aquatic toxicity (algae) testing of 9,10-anthracenedione is to be conducted up to this chemical's measured water solubility limit of 74.6 micrograms per liter. Thank you, Jerry Cook On 5/5/2011 10:12 AM, Campanella

. Paul @ epamail

. epa . govwrote: Jerry, I believe this response from our staff answers the questions in your letter. we have inserted answers following each question in an attempt to be clear and explicit. Thanks for your patience. Paul Campanella.

(See attached file: Response to Jerry Cook Jerry Cook Qs Regarding Algal Testing for CAS# 84-65-1.pdf)

Paul J. Campanella, Ph.D. Chemical Information and Testing Branch Chemical Control Division U.S. Environmental Protection Agency Washington, D.C. 202-564-8091

Case Consulting Labs AQ solubility determination.pd f