REPORT

DETERMINATION OF THE RELATIVE SELF-IGNITION TEMPERATURE

OF TKA 40278 (CG1827)

Data Requirement / Test Guidelines:.

EEC Directive 92/69, A.16

Mrs. Alessandra Tognucci

Stud Com leflon Date:

March 04, 2003

RCC Ltd

Environmental Chemistry &

Pharmanalytics

CH-4452 Itingen/Switzerland

CIBA SPECIALTY CHEMICALS INC.

CH - 4002 Basel/Switzerland

RCC Study Number..’_

845427

Page 1 of 12

260
Page2

REPORT

RCC Study Number 845427

TKA 4~0278 (CGt 827~))

GLP CERTIFICATE

’ The Swiss GLP Monitoring Authorities

Statement of GLP Compliance

It is hereby confirmed that

dudng the pedod of

the following Test Facilities of

August15- 17,2000

. ..August~8-29,2001 and’.

.... Apd115,2002

RCC Ltd

4452 Itingen

Switzerland

were inspected by the Federal Office of Publio Health, the Swiss /~enoy for the

Environment, Forests and Landscape and the Intercentonal Office for the Control of

Medicines with respect to the compliance with the Swiss legislation on Good Laboratory

Practice.

Test Facilities

. Toxicology Division

. Environmental Chemistry and

Pharmanalytics Division

. Microbiological DiagnostiCS by

Biotechnology & Animal Breeding Division

areas of expertise*

TOX, ACC, MUT

ACC, ECT, ENF, EMN,

PCT,RES,OTH (Animal

metabolism)

OTH (Microbiology)

The inspection was performed in agreement with the OECD Guidelines ~or National GLP

inspections and Audits. It was found that the aforementioned test facilities were operating in

compliance with the Swiss Ordinance re~atlng to Good Laboratory practice [RS 813.016.5] st

the t~me they ware Inspected.

Federal Of~ce of Public Health

The Director

Prof. Th. Zeltner

Bern, May 2002

261
Page 3

REPORT

RCC Study Number 845427

GOOD LABORATORY pRACTICE

STATEMENT OF COMPLIANCE

RCC Study Number:

Test Item:

study Director:

Title:

845427

TKA 40278 (CGI 827)

Mrs. Alessandra Tognucci

Determination of the Relative Self-Ignition Temperature

of TKA 40278 (CGI 827)

" cem liance with the Swiss Ordinance relating to Good

This study was conducted. ~. P ^r~ ,~,~n rD~ ~t3 016.5  ̄ This Ordinance is based on I~orator~ Practice, adopted i-eDruary z . ~uu~, L ...... ]

the OECD Principles of Good Laboratory Practice, as revised in 1997 and adopted November

26t~, 1997 by decision of the OECD Council [C(97)186/Final].

The purity of the test item is excluded from the statement of compliance (purity available in

Analytical Certificate No. 14026512-1; Ciba Specialty Chemicals Inc.).

Study Director:

262
Page 4

RCC Study Number 845427 REPORT

TKA 4.~0278 (CGI 827)

SIGNATURES

Study Director:

~ Tognucci

D~te:

Management: Dr. JSrn Schreitm(~ller

263
RCO Study Number 845427

"~KA 40278 (CG1827)

Page 5

REPORT ~

QUALITY’ AssURANCE UNIT

RCC Ltd, Environmental Chemistry & Pharmanalytics, CH-4452 Itingen / Switzerland

STATEMENT

RCC Study Number:

Test Item:

845427

TKA 40278 (COl 827)

Mrs. Alessandra Tognucci

Study Director: Determination of the Relative Self-lgn|tion Temperature

Title: of TKA 40278 (CGI 827)

The general facilities and activities are inspected periodicallY and the results are reported to

the responsib~e persOn and the management.

Study procedures were periodically inspected. The study plan and this report were audited by

the Quality Assurance Unit. The dates are given beloW: __

~ Dates of Reports to the study

Dates and Types of QAU Inspections Director and to the Management

September 16, 2002 Study Plan

December 17, 2002 Process based

(Sample Preparation)

February 27, 2003 Final report

This statement also confirms that this final report

September 16, 2002

December 17, 2002

February 27, 2003

reflects the raw data.

Quality Assurance:

Mrs. Diana Bergin

264
Page 6

RCC Study Number 845427 REPORT

TKA 40278 (CGI 827)

CERTIFICATION OF GLP

AND VERIFICATION OF THE REPORT

The statement of Compliance with Good Laboratory Practice found in this report, and signed

by the Study Director is truthful and accurate, and this report as provided by the testing

facility is complete and unaltered.

Signature of the Sponsor:

Date:

265
Page 7

REPORT

RCC Study Number 845427

TKA 40278 (CGI 8~2T/

CONTENTS

GLP CERTIFICATE ........................................................................................................

2

STATEMENT OF cOMPLIANCE ....................................................................................

3

sIGNATURES ................................................................................................................

4

QUALITY ASSURANCE UNIT ........................................................................................

5

CERTIFICATION OF GLP AND VERIFICATION OF THE REPORT ..............................

6

CONTENTS ....................................................................................................................

7

PREFACE .......................................................................................................................

8

DATA REQUIREMENT / TEST GUIDELINES .......................................

9

SUMMARY OF sTUDY pLAN AMENDMENTS ................................................

9

1 PURPOSE ...............................................................................

2 MATERIALS AND METHODS .............................................................................

10

2.1 TEST ITEM .................................................................................................

10

10

2.2 PRINCIPLE ................................................................................................ 11

2.3 STUDY DESIGN .........................................................................................

2.31 Test System .................."’"’~ ............................................... 11

 ̄ ns before the lest .............................................. re arat o 11 23.2 P P ............

233 Measurements ..................................................

2.4 DATA HANDLING ......................................................................................

11

3 RESULTS ............................................................................................................

12

266
Page 8

REPORT

RCC Study Number 845427

"I’KA 40278 (OGI 827~

PREFACE

GENERAL

Title:

Sponsor:

Monitoring Scientist:

Test Facility:

Determination of the Relative Self-ignition Temperature

of TKA 40278 (CGI 827)

CIBA SPECIALTY CHEMICALS INC.

CH-4002 Basel/Switzerland

Dr. Moung Sook Lee

RCC Ltd Environmental Chemistry & Pharmanatytics

Zelgliweg 1

CH-4452 itingen/Switzerland

RESPONSIBILITIES

Study Director:

Deputy Study Director:

Technical Coordinator:

Head of RCC Quality Assurance:

Mrs. Alessandra Tognucoi

Dr. Ute Schmiedel

Mr. Christoph Wild

Mrs. Iris W~thrich

SCHEDULE

Experimental starting date:

Experimental completion date:

Study completion date:

January 09,2003

January 10,2003

March 04, 2003/ssa

ARCHIVlNG

RCC Ltd, CH-4452 itingen/Switzerland will retain the study plan, raw data, a sample of test

item and the final report of the present study for at least ten years.

No data will be discarded without the sponsor’s consent.

267
RCC Study Number 845427 REPORT Page 9

TKA 40278 (CG1827)

DATA REQUIREMENT / TEST GUIDELINES

This study followed the procedures indicated by the following internationally accepted

guidelines and recommendations:

EEC Directive 92/69 EEC, Part A, Methods for the determination of physico-chemical

properties, A.16: "Relative self-ignition temperature for solids", EEC Publication No. L383,

December 1992.

SUMMARY OF STUDY PLAN AMENDMENTS

There were no amendments to the study plan.

268
RCC Study Number 845427 REPORT Page 10 TKA 40278 (CGI 827)

1 PURPOSE

The purpose of the study was to provide preliminary information on the auto-flammability of

TKA 40278 (CG 827) at elevated temperatures.

2

2.1 TEST ITEM

Data as provided by the sponsor.

Identity:

Product Name:

Batch:

Purity:

Appearance:

Expiration date:

MATERIALS AND METHODS

TKA 40278

CGI 827

KL 01/02

See Analytical Certificate, Study No. 14026512-1

Ciba Specialty Chemicals Inc.

Solid, slightly yellow

August 30, 2004

2.2 PRINCIPLE

A certain volume of the test item is placed in an oven at room temperature; the

temperature/time curve relating to the conditions in the centre of the sample is recorded while

the temperature of the oven is increased to 400 °C at a rate of about 0.5 °C/rain. The

temperature of the oven at which the sample temperature reaches 400 °C by self-heating is

called the self-ignition temperature for the purpose of this test.

Whether the heat development is due to a reaction of the test item with oxygen or due to

exothermic decomposition is not relevant for the test. Self-heating, with the possible

consequence of self-ignition, occurs, when the rate of heat production exceeds the rate of

heat loss to the surroundings.

269
Page 11

REPORT

RCC Study Number 845427

TKA 40278 (CG1827)

2.3 STUDY DESIGN

2.3.1

Oven:

Wire mesh cube:

Test System

A temperature programmed laboratory oven (type L 3/S, Nabertherm

Labotherm, Controller S 27)

A piece of stainless steer wire mesh with 0.045 mm openings was cut,

folded and secured with wire into an open topped cube with dimensions

of 2X2x2cm.

Thermocouples:

Recorder:

TestotermoThermocouples, type NiCr

A two channe~ recorder (type Testo 901, Testoterm)

2.3.2 Preparations before the Test

The cube was completely filled with the test item. The sample was then suspended in the

centre of the oven at room temperature. One thermocouple was placed at the centre of the

cube and the other between the cube and the oven wall to record the oven temperature.

2.3,3 Measurements

The temperatures of the oven and the sample were continuously recorded while the

temperature of the oven was increased to approximately 400 °C at a rate of about 0.5 °C/rain.

The appearance and physical state of the test item after the test were determined and are

specified in this report.

2.4 DATA HANDLING

The self-ignition temperature, as obtained by this method, is the minimum ambient

temperature expressed in [°C] at which a certain volume of a substance ignites under defined

conditions.

Temperature measurement data and any heat effects observed between room temperature

and about 400 °C were evaluated.

If an exothermic reaction of the test item appears, the sample thermocouple shows a sharp

temperature rise above the oven temperature. The temperature of the oven at which the

sample reaches 400 °C by self-heating is appointed as the self-ignition temperature of the

test item.

270
RCC Study Number 845427 REPORT Page 12

TKA 40278 (CGI 827)

3 RESULTS

The determination of the relative self-ignition temperature of the test item was performed

according to the EEC Directive 92/69, Part A, Methods for the determination of physicochemical propert’es; A.16 ’Relative self-ignition temperature for solids", EEC Publication No.

L383, December 1992.

The correlation between the temperature of the oven and the sample temperature of TKA

40278 (CGI 827) is shown in the figure below.

Using a linear increase in temperature of about 0.5 °C/min, TKA 40278 (CGI 827) showed no

relevant exothermic reaction. TKA 40278 (CGI 827) has a melting point at about 84 °C. As

the above mentioned guideline only applies to solids, the temperature range between 84 °C

and 400 °C is not relevant for the present test item. At the end of the measurement TKA

40278 (CGI 827) was run out of the sample cube due to melting and was coloured black.

In conclusion, TKA 40278 (CG! 827) Is not auto-flammable, according to the criteria as

described in the guideline.

Figure: Temperature/time relationship between TKA 40278 (CGI 827) and the oven

temperature during the relative self-ignition temperature measurement

500

4OO

300

~200

100

_~--- Sample Temp" [°C]I ~

0 200 400 600 800

Time [mini

271