COMPANY SANITIZED

SANITIZED Page 1 of 8 

Report date 22.09.2011 

Material: "Battery Material" 

The aim of the measurement: particle size distribution etc 

Results: 

Reduction of particle size by grinding is clearly detectable. The pore size is reduced by 

about a factor changing from by SEM evaluation. The 

morphology changes from . 

The crystalline structure , and the crystal size . 

From a suspension of 10 g/l solids in water (10,000 ppm), 

This document is the property of the sponsor and may be used only for that purpose intended by the sponsor. Every other or 

additional use, exploitation, reproduction, publication or submission to other parties requires the written permission of the 

sponsor, with the exception of the recipient regulatory agency acting within the limits of its administrative authority pursuant to 

applicable law (e.g., TSCA). The use of these studies/documents for regulatory, registration or other commercial purposes, 

including but not limited to Registration, Evaluation, Authorization and Restriction of Chemical Substances (REACH), without the 

express written permission of the sponsor is unauthorized and strictly prohibited.

EPA-HQ-OPPT-2009-0922
COMPANY SANITIZED

SANITIZED Page 2 of 8 

22/09/2011

Size:

1): SEM 

The samples were imaged using SEM on representative areas. In the milled sample, 

, and, thus, 

.

SEM Sample 1: 
COMPANY SANITIZED

SANITIZED Page 3 of 8 

22/09/2011

SEM Sample 2: 
COMPANY SANITIZED

SANITIZED Page 4 of 8 

22/09/2011

2) Size characterization by HG-Porosimetry:

Hg-Porosimetry Sample 1: 
COMPANY SANITIZED

SANITIZED Page 5 of 8 

22/09/2011

Hg-Porosimetry Sample 2: 
COMPANY SANITIZED

SANITIZED Page 6 of 8 

22/09/2011

3) Size distribution from Malvern-Mastersizer:

Presentation of Results 

System Parameters

Focal Length: Beam Length: Module: Obscuration: 

Presentation: 

Analytical Model: Residual: 

Modifications: Suppress Result Channels:

Sample Name: Nr. Measured: 6 Sept 2011 10:05

File: Measurement Nr: Analyzed: 6 Sept 2011 10:05

Path:

Comment: 

Result Statistics

Distribution Type: Concentration: Density: Specific Surface Area. = 

Mean Diameter: D (v, 0.5) = D (v, 0.9) = 

Span: Uniformity: 

Size

(um) 

Volume

Under (%) 

Size

(um) 

Volume

Under (%) 

Size

(um) 

Volume

Under (%) 

Size

(um) 

Volume

Under (%) 
COMPANY SANITIZED

SANITIZED Page 7 of 8 

22/09/2011

Crystallinity: 

4) XRD-Xray Powder Defractometry:

Due to the grinding of the sample the peak width in the measured diffraction patterns appears to

change slightly. While the sample has 

an average crystal size of the ground sample 

has only an average crystal size of This result is derived from an exemplary 

FWHM evaluation only of the strongest diffraction line at about determined. The sample 
COMPANY SANITIZED

SANITIZED Page 8 of 8 

 22/09/2011

Solubility: 

5) X-ray fluorescence:

Pretreatment: 

Sample was dispersed in H2O and 

then fractionated by preparative ultracentrifugation. The supernatant was used to assess the 

solubility by X-ray fluorescence analysis. 

In addition, was used to assess by elemental analysis any 

possible contaminations by the grinding process. 

Overview analysis by X-ray fluorescence 

The X-ray fluorescence is a method for qualitative and quantitative determination of all elements 

with atomic numbers from 11 (Na), where the detection sensitivity depends both on the matrix 

and the specific element.