Assessment of Purity (Interim Results)

Report for

Project Number: 13714

Prepared by

Alison M. McGuire BSc CSci CChem FRSC

Compliance Services International ‐ Europe

Pentlands Science Park, Penicuik

Nr. Edinburgh, EH26 0PZ

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www.ComplianceServices.com
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1 EXECUTIVE SUMMARY

The objective of this work was to evaluate the purity of two batches of

(Batches 12166 and 12342).

The purity has been determined by subtracting the percentage of impurities detected due to the

unavailability of a reference standard for   

The following techniques have been used to assess the purity of   

 Liquid Chromatography with Mass Spectroscopy (LC‐MS)

 Gas Chromatography with Mass Spectroscopy (GC‐MS)

Supporting Data

 Proton and Boron Nuclear Magnetic Resonance (

1

H and 11B NMR) (Batch 13337)

 X‐Ray Diffraction (XRD) (Batch 13337)

Based on the manufacturing process it was considered that the following impurities could

theoretically be present in   







Scans were performed using the techniques identified above and no other substances were found to

be present. was found to be present at ca. , was found to be

present at ca. , and   was not found (<0.1%).  These figures are suggestive of a

purity of   Work is ongoing to confirm these interim results.

1.1 Chemical Characteristics  

Name:

Chemical Structure:

CAS Number:

Chemical Formula:

Molecular Weight: 469

Physical State: White crystalline powder

Arrival Date: 11 Jan 2012 (Batch 12166)

19 March 2013 (Batch 12342)

Expiry Date: 10 April 20141 (Both batches)

Storage Conditions: Room temperature (15‐30°C)

1 Assigned by the testing laboratory.

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Name:

Chemical Structure:

CAS Number:

Chemical Formula:

Molecular Weight: 138.120697

Physical State: colourless to white crystals

Name:

Chemical Structure:

CAS Number:

Chemical Formula:

Molecular Weight: 185.349503

Physical State: Colourless to yellow liquid

Name:

Chemical Structure:

CAS Number:

Chemical Formula:

Molecular Weight: 61.833

Physical State:

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White crystalline solid
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1.2 Determination  

(Smithers Viscient Letter Report, SABoTBA Ref.3200166, 12 December 2013, Appendix I)

  

LC‐MS analysis found ca.   w/w .

e

GC‐MS analysis found ca.   w/w .

1.3 Determination  

(University of Sheffield 1H and 11B NMR Spectra, Appendix II; Ceram X‐Ray Diffraction

Quantitative Phase Analysis Report, Appendix III)

From the results of the NMR analysis it can be concluded that there is no   present at levels

≥0.1%.   

A sample of   was fortified at this level and measured using both proton and   NMR to

confirm that the instrument could accurately measure   at this concentration.  A peak was

observed when fortified (5.6 ppm 1

H; 24.962 ppm 11B), confirming that the method is sufficiently

sensitive for .  No   peak was detected in the   sample unfortified with

, thus demonstrating that there is no   present in the sample at .

X‐ray diffraction did not determine the presence of any   at levels (the instrument

limit of detection).

2 Conclusion

Based upon interim data the purity of SABoTBA can be described as shown below:‐ 

Chemical Substance Percentage w/w

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Appendix I Letter Report from Smithers Viscient

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Appendix II University of Sheffield 1

H and 11B NMR Spectra

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-0.5 ppm

 Sample ref. -13337-II in CDCl3

Current Data Parameters

NAME Nov21

EXPNO 501

PROCNO 1

F2 - Acquisition Parameters

Date_ 20131121

Time 9.20

INSTRUM drx500

PROBHD 5 mm BBI 1H-BB

PULPROG zg30

TD 65536

SOLVENT CDCl3

NS 32

DS 4

SWH 5995.204 Hz

FIDRES 0.091480 Hz

AQ 5.4657526 sec

RG 128

DW 83.400 usec

DE 6.00 usec

TE 298.0 K

D1 0.10000000 sec

TD0 1

======== CHANNEL f1 ========

NUC1 1H

P1 7.68 usec

PL1 -3.00 dB

SFO1 500.1323530 MHz

F2 - Processing parameters

SI 32768

SF 500.1300177 MHz

WDW no

SSB 0

LB 0.00 Hz

GB 0

PC 1.00

F2 - Spectrum reference

SR 17.74 Hz

F2 - Digital resolution: Hz per point

HZpPT 0.182959 Hz

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10.5 10.0 9.5 9.0 8.5 8.0 7.5 7.0 6.5 6.0 5.5 5.0 4.5 4.0 3.5 3.0 2.5 2.0 1.5 1.0 0.5 0.0 -0.5 ppm

 Sample ref. doped with at 0.1% in CDCl3 + a drop of DMSO

Current Data Parameters

NAME Nov29

EXPNO 524

PROCNO 1

F2 - Acquisition Parameters

Date_ 20131129

Time 16.46

INSTRUM drx500

PROBHD 5 mm BBI 1H-BB

PULPROG zg30

TD 65536

SOLVENT CDCl3

NS 32

DS 4

SWH 5995.204 Hz

FIDRES 0.091480 Hz

AQ 5.4657526 sec

RG 128

DW 83.400 usec

DE 6.00 usec

TE 298.0 K

D1 0.10000000 sec

TD0 1

======== CHANNEL f1 ========

NUC1 1H

P1 7.68 usec

PL1 -3.00 dB

SFO1 500.1323530 MHz

F2 - Processing parameters

SI 32768

SF 500.1300177 MHz

WDW no

SSB 0

LB 0.00 Hz

GB 0

PC 1.00

F2 - Spectrum reference

SR 17.72 Hz

F2 - Digital resolution: Hz per point

HZpPT 0.182959 Hz

Proton Nuclear Magnetic Resonance (1H NMR) (Batch 13337) Fortified with 0.1% 

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 Sample ref. -13337-II in CDCl3

Backwards linear prediction parameters: NCOEF = 2048 TDOFF = 32

-70 -80 ppm

5

Current Data Parameters

NAME Nov21

EXPNO 700

PROCNO 1

F2 - Acquisition Parameters

Date_ 20131121

Time 9.15

INSTRUM drx500

PROBHD 5 mm BBI 1H-BB

PULPROG zg

TD 65402

SOLVENT CDCl3

NS 129

DS 0

SWH 32051.281 Hz

FIDRES 0.490066 Hz

AQ 1.0203212 sec

RG 256

DW 15.600 usec

DE 6.00 usec

TE 298.0 K

D1 0.10000000 sec

TD0 1

======== CHANNEL f1 ========

NUC1 11B

P1 25.00 usec

PL1 -3.00 dB

SFO1 160.4620000 MHz

F2 - Processing parameters

SI 32768

SF 160.4615790 MHz

WDW EM

SSB 0

LB 5.00 Hz

GB 0

PC 1.40

F2 - Spectrum reference

SR -421.00 Hz

F2 - Digital resolution: Hz per point

HZpPT 0.978127 Hz

Boron Nuclear Magnetic Resonance (11B NMR) (Batch 13337)

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 Sample ref. doped with at 0.1 % in CDCl3 + Drop of DMSO

4210832n Backwards linear prediction parameters: NCOEF = 2048 TDOFF = 32

5 -50 -55 -60 -65 ppm

9627184

Current Data Parameters

NAME Nov29

EXPNO 725

PROCNO 1

F2 - Acquisition Parameters

Date_ 20131129

Time 16.04

INSTRUM drx500

PROBHD 5 mm BBI 1H-BB

PULPROG zg

TD 65402

SOLVENT CDCl3

NS 760

DS 0

SWH 32051.281 Hz

FIDRES 0.490066 Hz

AQ 1.0203212 sec

RG 256

DW 15.600 usec

DE 6.00 usec

TE 298.0 K

D1 0.10000000 sec

TD0 1

======== CHANNEL f1 ========

NUC1 11B

P1 25.00 usec

PL1 -3.00 dB

SFO1 160.4620000 MHz

F2 - Processing parameters

SI 32768

SF 160.4615790 MHz

WDW EM

SSB 0

LB 5.00 Hz

GB 0

PC 1.40

F2 - Spectrum reference

SR -421.00 Hz

F2 - Digital resolution: Hz per point

HZpPT 0.978127 Hz

Boron Nuclear Magnetic Resonance (11B NMR) (Batch 13337) Fortified with 0.1% 

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Appendix III Ceram X‐Ray Diffraction Quantitative Phase Analysis Report

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MICROSTRUCTURE ANALYSIS REPORT

Client:

Ceram Reference: (135995)-25352 

For the Attention of:

Date Logged:

Date of Tests: 21-Nov-2013 22-Nov-2013 to

20-Nov-2013

Report Date: 22-Nov-2013

Purchase Order No.: 7679-ANJ

Work Location: Ceram UK

Test Method:

Description: Examination by X-Ray Diffraction

Methods M7, M9 and M30

Please find attached the results for the sample(s) recently submitted for analysis.

Opinions and interpretations expressed herein are outside the scope of UKAS Accreditation.

2

Author

Dr Giles Blundred

Page 1 of 2 pages

is taken for the accuracy of the sampling unless this is done under our own supervision. This report shall not be reproduced in part without the written

This report is issued in accordance with the Conditions of Business of Ceram Research Limited and relates only to the sample(s) tested. No responsibility

approval of Ceram Research Limited, nor used in any way as to lead to misrepresentation of the results or their implications.

Ceram is the trading name of Ceram Research Limited. Registered in England No. 1960455 Registered Office as above.

0013

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Ceram Reference: (135995)-25352 

Customer Reference: – 13337 - II 

Description: 

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Quantitative Examination by X-Ray Diffraction

An organic colour developer sample was submitted for Quantitative Phase Analysis by X-Ray Diffraction in order to 

assess the presence of The sample was evaluated in accordance with UKAS 

accredited in-house methods, M7, M9 and M30. Due to the unknown structure of the target compound a spinel 

standard was added to the sample to act as an internal standard. 

Your Reference – 13337 - II 

Phase Content

Not detected

End of Test Report

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