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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 


CONFIDENTIAL BUSINESS INFORMATION

FlintGroup

Pigments

November 7, 2008

ToEarl Seibert / Cincinnati / 2080

From/Unit

Loctin/xtn~onHuntington / 2336

Determination of Logio K I-octanoiiwater Partition Coefficient For C. I.

Subject Pigment Blue 61

Joe Ochsner / Huntington / 2301

Bill Witzel / Elizabethtown / 6033

Copie.

Summary: The standard lot of Pigment 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 of 0.03 1, and a population of 5 samples.

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 for reagent grade water Types, 1, 11, 11, and IV. The

UV-visible absorbance was measured at X550 m=0.0001, X600 nm=0.000, X650 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

only trace levels of other 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 of Pigment Blue 61 [ Lot# 20847011 was prepared by

combining several production lots of the 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 of the city water and then the pigment was washed with

deionized water to a conductivity of < I OOjiS. The pigment was then dried at 60'C for 240 hours

and the resulting dried cake was crushed and blended, by tumbling in a container for 2 hours. This

material was then extracted with n-Hexane for seventy-two hours using a Soxhlet extractor. The
extracted material was dried for forty-eight hours at 75'C and was then ground. Aliquots taken

for further testing were ground in a mortar 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 )'550 "m =0.0000,

),00. = 0.0000, 450nm 0.0000. Based on this the material was used without further

purification.

Equipment:

Volumetric flasks: All volumetric flasks used were Class A glassware.

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

25 10 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., 5 inch x 4 gauge needle.

Analytical balance: Sartorius CF, Serial Number 40904946, Last calibrated 09/17/08 by

Kanawha Scale.

Primary Filter: Gelman, FP Vericel Membrane FilterTm. 0.45 jim, Lot#~ 5043504

Secondary Filter: Pall Life Sciences Supor PES Membran-eTM, 0.45pm, Lot # Al10419038.
Procedure:

Solvent saturation I -octanol: 600 ml] of I -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 of de-ionized water was transferred to a triple, 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 for fifteen

minutes at 3 500 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 of 2.5 mg. / liter for water and 23.8 mg. / liter for I1-octanol.

Using this as a basis, a number of samples 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 0 0 

0 .951 0.2650 2.01

0.30801 250

Abla0banot0 P19" GO 61 In -1,0

Calibration data For 1 - Octanol [10 mm cell] R 2 = 0.9995
Absorbance 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 In I-Octanol

800

0 09995

600 ___ - - - -

5,00 -------------- ---- - - ~ -

010 0,100 0200 0300 0400 .500 0 600 0700 0800 010

Absorbance

Pigment saturation of water: 500 ml. of I -octanol saturated water was mixed with 52.1 mg. of the

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 ptm filter and was reserved for further use.

Pigment saturation of I -octanol: 500 ml. of water saturated I -octanol was mixed with 500.1 mg.

of the 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 of bottles for shaking / shaking: Using a 50 ml. syringe with a Pall 0.45 Pim filter 40

ml. of the pigment saturated I1-octanol and using a separate syringe and filter 40 ml. of the

pigment saturate water. Seal the jars 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 of 7200 shakes.
Centrifugation: Load bottles into centrifuge baskets and set for 3500 rpm x 20 minutes and run.

Removal of samples for analysis: The lighter I1-octanol layer is observed to be a bright, light

blue, while the water layer is apparently colorless. A 1.00 ml. aliquot of the 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 a needle, 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 the bottom of the jar the

water layer is drawn into the syringe, carefully leaving a sufficient quantity of water in the jar to

insure that there is no octanol drawn into the syringe. The outside of the needle is then wiped

clean and dry and a small volume of water 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. Eng Data, 1982, 27

451-454.

3. Sujit Banerjee, Samuel H. Yalkowsky, Shri C. Valvani, Water Solubility and Octanol/

Water Partition Coefficients of Organics, Limitations of the Solubility - Partition

Coefficient Correlation, Environmental Science and Technology, 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 of the solubility ( of Pigment Blue 61 ) in

water ad octanol at ambient temperature. Internal Report Number 076513e, June 27,2006.