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. No anthraquinone was detected in any of the 

samples. The limit of detection of the method is somewhere around 50 ppb, 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/~UdRuo1:1, 

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 05/12/2011 
10:12 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.gov wrote:

 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.pdf