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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, PESTICIDESAND TOXIC SUBSTANCES



### Subject: Follow-up to fax transmission of4/13/12 (ePMA

### removal ofCBI claimsregarding identified studies) 

### DearMr. Merritt: This is sent to you pursuant ourconversation 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 ofcopyrightprotections and some additional text that provides in part ... "Reproduction, reference, summarization, retransmission or otheruse ofthis copyrighted document.
..including electronic transmission, using the internet oremail
....is strictly prohibited
...." While we understand the basis for the copyrightprotections, 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 bemade available in an Agencye-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 ongovernment 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. Canyou please confirm CPMA's intent? Many thanks.

Scott M. Sherlock, Attorney Advisor Environmental Assistance Division Office ofPollution Prevention and ToxicsCONFIDENTIAL BUSINESS INFORMATION 

# FlintGroup Pigments November 7,2008 ToEarl 

### Seibert /Cincinnati /2080

From/Unit Loctin/xtn~onHuntington 

## /2336 Determination of Logio KI-octanoiiwater 

### Partition Coefficient For C.I. Subject 

### Pigment Blue 61 Joe Ochsner / Huntington /2301 BillWitzel / Elizabethtown /6033 Copie. Summary: The standard lot ofPigment Blue 61 was examined to determine the octanol /water partition coefficient. The procedures used for this determination were those outlined in the US EPA publication "Product Properties Test Guidelines - OPPTS 830.7550 Partion Coefficent (nOctanol /Water), Shake Flask Method." The average value for Logic Koiw = 3.999, with a standard deviation of0.031, and apopulation of 5samples. Experimental: Materials: Water: The water used in the study was deionized, reagent grade, supplied by RICCA Chemical Company, Catalog #9150-1, Lot #2808057. The water was purified by activated carbon treatment, reverse osmosis, de-ionization, UV-irradiation, and 0.2 micron filtration and was certified to meet ASTM D 1193 specifications forreagent grade water Types, 1,11, 11, and IV. The 

### UV-visible absorbance was measured at X 5 50 m=0.0001, X 6 00 nm=0.000, X 65

0 nm=0.0000.
I1-Octanol: The octanol used in the study was supplied by Sigma - Aldrich, Catalog #293245, Lot# 03836LH, and was HPLC grade, certified to be >99%pure. The material was analyzed by direct sample introduction, LCIMS using Marshall University's LCQ mass spectrometer, with onlytrace levels ofother compounds being found. Further analysis using the Marshall University Saturn 2000 GC/MS indicated that the material was >99.69% octanol, with the remainder being: Water 0.13%, branched octanols = .12%, total heptanols =0.05, octanols = 0.01%. The 

### UVvisible absorbance was measured at X5Onm = 0.0001, %600nmi = 0.0001, X65Onm = 0.0000. Based on this the material was used without further purification. C.I. Pigment Blue 61: The standard lot ofPigment Blue 61 [Lot# 20847011 was prepared by combining several production lots ofthe pigment, reslurrying them in city water to blend and homogenize them, and then filtering the blended material. The blended material was washed with city water until conductivity reached that ofthe city water and then the pigment was washed with deionized water to aconductivity of< I OOjiS. The pigment was then dried at 60'Cfor 240 hours and the resulting dried cake was crushed and blended, by tumbling in a container for 2hours. This material was then extracted with n-Hexane for seventy-two hours using a Soxhlet extractor. Theextracted material was dried for forty-eight hours at 75'C and was then ground. Aliquots taken for further testing were ground in amortar and pestle and were blended by mixing prior to use Methanol: The methanol used was Burdick and Jackson High Purity solvent grade, catalog number NP230-20, Lot / CX272. The UV-visible absorbance was measured at )' 5 50"m =0.0000, ),00. = 0.0000, 450nm 0.0000. Based onthis the material was used without further purification. Equipment: Volumetric flasks: All volumetric flasks used were Class Aglassware. Beakers and other glassware: Beakers, and other general glassware were standard PyrexTM lab ware obtained from VWR and Ace Glass. Sample bottles: Sample bottles were 120 ml. soft glass with Teflon lined metal tops. Mixing apparatus: Solvent mixing and equilibration was done using a Barant Mixer with a pitched blade, four blade turbine. This was followed by ultrasonic treatment using a Branson 2510 ultrasonic batch. Shaker: Burrell Wrist Action Shaker Model 75. Centrifuge: Heraeus Instruments Labofuge 400. UV-Visible Spectrometer: Shimadzu UV-1201 [for measurements in octanol] UV
- Visible Spectrometer: Cary 50 Bio [for measurements in water] Sample cells: 10 mm cells, Beckmann matched, no serial number available. 100 mm cell, VWR SpectroTm Lot# 080505. Syringe: Beckton
- Dickinson 50 cc., 5inch x 4gauge needle. Analytical balance: Sartorius CF, Serial Number 40904946, Last calibrated 09/17/08 by Kanawha Scale. Primary Filter: Gelman, FP Vericel Membrane FilterTm. 0.45jim, Lot#~5043504 Secondary Filter: Pall Life Sciences Supor PES Membran-eTM, 0.45pm, Lot #Al10419038.Procedure: Solvent saturation I-octanol: 600 ml] ofI-octanol was transferred to a triple, methanol washed one liter beaker, which had been oven dried; to this was added 100 ml. of the reagent grade deionized water. This was then stirred for twenty-four hours at 

### 450 rpm. The beaker was then sonicated for one hour and the resulting mixture was divided into parts and centrifuiged for fifteen minutes at 3500 r.p.m. The water saturated octanol was then decanted and stored for further use. Solvent saturation water: 1000 ml ofde-ionized water was transferred to atriple, methanol washed two liter beaker, which had been oven dried; to this was added 200 ml. of the reagent grade I-octanol. This was then stirred for twenty-four hours at 450 rpm. The beaker was then sonicated for one hour and the resulting mixture was divided into parts and centrifuged forfifteen minutes at 3500 r.p.m. The octanol saturated water was then decanted and stored for fuirther use. Calibration curves: In their internal document number 076513e, Clariant had provided solubility values for C.I. Pigment Blue 61 of2.5 mg. / liter forwater and 23.8 mg. / liter for I1-octanol. Using this as a basis, anumber ofsamples were prepared by weighing finely ground PB-61 into 500 ml. volumetric flasks and diluting with either neat octanol or neat water. These were then sonicated to insure dissolution and aliquots were taken and further diluted to prepare a number of samples at the desired concentration ranges. These diluted samples were then measured at 596 nim [known ?~for Pigment Blue 61]. Using the measured values the calibration curves shown below were derived. Calibration Data For Water [100mmn cell] i= 0.9955 Absorbance Conc. (pgIL) 0.0000 0.00 0 .13 00 0 .951 0.2650 2.01 0.30801 250

Abla0banot0 P19" GO 61 In -1,0

Calibration data For 1 - Octanol [10mm cell] R2 = 0.9995Absorbance Conc. (mg/L) 0.000 00 0.132 1.01 0.2501 204 0.359 2.95 0.499 408 0.8071 6.81
Absorbance of Pigment Blue 61 InI-Octanol

800 0 09995

600
___ - - - - 5,00 -------------- ---- - - 

### ~

-

010 0,100 0200 0300 0400 .500 0600 0700 0800 010
Absorbance Pigment saturation ofwater: 500 ml. of I-octanol saturated water was mixed with 52.1 mg. ofthe Pigment Blue 61 standard and this was agitated at 450 rpm for sixteen hours. This sample was then placed in the ultrasonic bath for one hour. The sample was then filtered through a Gelman 0.45ptm filter and was reserved for further use. Pigment saturation of I-octanol: 500 ml. ofwater saturated I-octanol was mixed with 500.1 mg. ofthe Pigment Blue 61 standard and this was agitated at 450 rpm for sixteen hours. This sample was then placed in the ultrasonic bath for one hour. The sample was then filtered through a Gelman 0.45[lim filter and was reserved for further use. Preparation ofbottles for shaking / shaking: Using a 50 ml. syringe with a Pall 0.45 Pim filter 40 ml. ofthe pigment saturated I1-octanol and using a separate syringe and filter 40 ml. ofthe pigment saturate water. Seal thejars and tape the lids to secure. Load the bottles onto the Burrell shaker and secure. Set arm to widest travel and shake at 60 Hz. for 120 minutes (2 x 60) for a total of7200 shakes.Centrifugation: Load bottles into centrifuge baskets and set for 3500 rpm x 20 minutes and run. Removal ofsamples for analysis: The lighter I1-octanol layer is observed to be abright, light blue, while the water layer is apparently colorless. A 1.00 ml. aliquot ofthe octanol layer is pipetted into a 50 ml. volumetric flask and is then diluted to the mark with methanol. Using a 50 ml. Beckton
- Dickinson syringe, equipped with aneedle, the water layer is removed. This removal is done by filling the syringe with air and gently expelling it while penetrating the octanol layer, thus insuring that no octanol enters the needle. Once at thebottom ofthejar the water layer is drawn into the syringe, carefully leaving a sufficient quantity ofwater in thejar to insure that there isno octanol drawn into the syringe. The outside ofthe needle is then wiped clean and dry and a small volume ofwater is expelled to clean the syringe needle. The remaining sample is then placed in a marked bottle for analysis. Analysis: The octanol samples were analyzed using the Shimadzu UV-visible at Flint Group Huntington, with a 10 mm cell. The water samples were taken to Marshall University and were analyzed using a Gary 50 Uv - Visible spectrometer and a.100 mm. cell. Results are given below. Octanol Results Water Results Sample # Absorbance Cono ( mg/L) Absorbance Conc ( microg/L) 1 0.066 24.4 0.3100 2.448 2 0.070 26.1 0.369 2.919 3 0.071 26.6 0.307 2.424 4 0.067 24.9 0.3090 2.440 5 0.068 25.3 0.323 2.552

Results and Discussion: The measured concentration pairs were divided and the base 10 log was taken as specified in 

### OPPTS 830.7550. Sample # Kww Log10 Ko/w 1 9986.119 3.999397 2 8953.138 3.951975 3 10956.66 4.039678 4 10192.03 4.008261 5 9911.024 3.996119

Avg.= 3.999 Std.Dev. 0.031 References:L US EPA Product Properties Test Guidelines OPPTS 830.7550 Partition Coefficient (n-Octanol /Water), Shake Flask Method. 2. Y.B. Tewari, M.M. Miller, S.P. Wasik, and D.E. Martire, Aqueous Solubility and octanolI Water Partition Coefficent of Organic Compounds at 25.0*C, J. Chem. EngData,1982, 27 451-454. 3. Sujit Banerjee, Samuel H. Yalkowsky, Shri C.Valvani, Water Solubility and Octanol/ Water PartitionCoefficients ofOrganics, Limitations ofthe Solubility
- Partition Coefficient Correlation, EnvironmentalScienceandTechnology, 14, No. 10, 1980,1227-1229. 4. ASTM Standard E 1147-92 Standard Test Method for Partition Coefficient (n-OctanolI Water) estimation by Liquid Chromatography. 2005 5.Rainer Az and Martina Mahler, Determination ofthe solubility (ofPigment Blue 61) in water ad octanol at ambient temperature. Internal Report Number 076513e, June 27,2006.