## REPORT

DETERMINATION OF THE RELATIVE SELF-IGNITION TEMPERATURE OF TKA 40278 (CG1827) Data Requirement / Test Guidelines:. EECDirective 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



### 260Page2 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



### 261Page 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:



### 262Page 4

RCC Study Number 845427 REPORT TKA 4.~0278 (CGI 827) 

## SIGNATURES

Study Director: ~ Tognucci

D~te:

Management: Dr. JSrn Schreitm(~ller



### 263RCO 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



### 264Page 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:



### 265Page 7 REPORT RCCStudy 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



### 266Page 8 REPORT RCCStudy 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.

267RCC 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.



### 268RCC 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.



### 269Page 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.



### 270RCC 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 performedaccording 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