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REPORT 

SANNTtZED 

DETERMINATION OP TIHE AUTO-IGNITtON TEMPERATURE (LIQUIUS) OP 

1,1,3,3-TETRAMEThiYLBUTYLPEROXY PIVALATE 

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iVOTOX Project ~ 

NOTOX Substan

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1,1,3,3-TETRAMETNYLBUTYLPER(JXY P1tfALATE NOTO}C Praject~ 

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Ct)Ni±IaENTEALfTY STATEMENT 

This report contains the unpubiished results of research sponsored by Akzo Nobe! Chemieals 

B.V.. Reproduc#ion, issue or disclosure fio thtrd parfiies in any form is not perrnitted without prror 

written authorizatlori from the sponsor. 

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1,1,3,3-TETRAMETHYLBUTYLPI*ROXY PiVAt,ATE iVOTdX i'roject 

`~-~~.._._....~ 

STATE#V1ENT OF GLP CO/IPLIANCE 

NOTOx B.V.,'s-Hertogenbosch, The Netherlands 

The study described in this report has been correctly reported and was conducted in compliance 

with the most recent edition of: 

The OECD Principles of Good Laboratory Practice 

which are essentially in conformity with: 

The United States Food and Drug Administration. Title 21 Code of Federal Regulations Part 58. 

The United States Environmental Protection Agency (FIFRA). Title 40 Code of Federal 

Regulations Part 160. 

The United States Envlronmental Protection Agency (TSCA). Title 40 Code of Federal 

Regulations Part 702. 

Study Director 

9ng. H.J. Krips ' 

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~ 

DateA 

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Management 

Dr. lr. H. Willems 

Head of Chemistry 

~ ~ 

Da\ 

\ 

~ 

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1,1 ,3,8-TETRAMF''HYLBUTYLPFROXY PIVAf.ATE NOTOX ProJec~ ! 

QUALITY ASSURANCE STATEMENT 

NOTOX B.V., 's-Hettogenboscn, The Netheriands 

This report was audited by the NOTOX Quality Assuranco Unit to ensure that the methods and 

results accurately t'eflect the raw data. 

The dates of Quality Assurance inspections and audits are given below. 

During the on-site inspections procedures applicabte to this type ofi study were inspected. 

DATES OF QAU 1NSPECTIONS/AUDlTS REPORTlNC DATES 

on-site inspection (s) 

13 July 1999 

protocol fnspection (s) 

11 February 1999 

report.audit (s) 

16 August 1999 

Head of Quality Assurance 

C.J. Mitcheil B.So. 

w,_ .w. ......... __ 

D~ ~ 

13 July 1999 

z 1 Febcuary 1999 

'tfi August 1999 

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1,1,3,3-TETRAiVIETHYLBUTYLPEROXY PtVALATE NO'i"O3C Project: ~ 

SUMMARY 

The determination of the auto-ignition temperature of 1,1,3,3-TETRAMETHYLBUTYLPEROXY 

PIVALATE was performed in accordance with EEC-Directive 92/69 EEC, A.15 "Auto-ignition 

temperature (liquids and gases)", (1992) and DIN 51794 "Bestimmung der Zundtemperatur", 

(1978). 

Test substance was injected into a test vessel at a temperature range between 240°C and 

490°C. The test was performed in 3-fold. 

A lowest auto-ignition temperature of 436°C was found, with an injection volume of 70 pl and a 

time lag of 08 s. 

ln conclusion, 1,1,3,3-TETRAMETHYLSUTYLf'EROXY PIVALATE is auto-ignitable with an 

auto-ignition temperature of 435°C. 

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1,1,3,3-"TETRAMETHYLBUTYLPEROXY F'IVALATE NOTOX Projdct 

PREFACE 

Sponsor AKZO Nobel Chemicals B.V_ 

P.O. Box 247 

3800 AE Amersfoort 

The Netherlands 

Study Monitor ~ 

Testing Facility NOTOX B. . 

Hambakenwetering 3 

5231 DD's-Hertogenbosch 

The Netheriands 

Study Director ~ 

Study Plan Start : 08 uiy ~"999 

Compieted : 09 .1uly 1999 

TEST SUBSTANCE 

Identification 1,1,3,3-TETRAMETHYLBUTYLPEROXY PfVALATE 

AKZO Nobel trade ns;me Trigonax 425 

Chemicai name 11,3,3,Tetramethylbutylperoxy pivat ate 

CAS no. 22288-41-1 

Description C©.taurinss liquid 

Batch Number C,y.; w= 

Purity SeeCe-Rifrcate of"anaiysis 

Test substance storage In €reezer in the dark 

Stability under storage 

conditions Stahle 

irxpiry date 01 danuary 2000 

The sponsor rs respor:sible fQr the completeness and GLP Compliance of ali fest substance 

data. 

PURPOSE 

The determination of the degree of auto-rgnitability in terrns of the auto-ignition temperature. 

GUIDELINES 

The study procedures described in this report are based on the following guidelines: 

European Economlc Community (EEG), EEC-flirective 92169 EEC, Part A, Methods for the 

determination o€ physico-chemical properties, A.15 "Auto•ignition temperature {liquids and 

gases}", EEC Publication No. L383, December 1992. 

DIN 51794 "Bestimrnung der Zundtemperatur", January 1978. 

IEC standard 79-4 "Electricai apparatus for explosive gas atrnospheres, Part 4, iVlethod of test 

for ignition temperature", 1975. 

sm 
1,1,3,3-TETRAMETHYLBUTYLPEROXY PIVALATE NOTOX Proje.`ct ; 

~...T..-..__._... 

ARCHIVING 

NdTOX B.V. will archive the following data for at least 10 years: 

protocol, report, test substance reference sample and raw data. Thereafter, no data wili be 

withdrawn without the sponsor's written consent. 

TEST SYSTEM AND RATIONALE 

Apparatus Self-ignition test apparatus (Sommer und Runge; Berlin, FRG) 

in accordance with DIN 51794 and IEC standard 79-4. 

Rationale Recognized by the international ,guidelines as recommended 

test system (EEC, DIN, IEC). 

CAL1t3RATSON OF THE TEST SYSTFNI 

The test procedure as outlined in this report is validated periodically, using n-heptane (zur 

analyse; Merck, FRG). The resuits are in accordance with the criteria of DIN 51794 and IEC 79-4. 

PERI;ORMANCE OF THE TEST 

Test procedure 

Samples were injected by means of a variable volumetric pipette to assure a rapid injection. 

The time lag between injection and ignition was measured for alt tests. 

Approximately 5 minutes after each test substance injection, the test vessel was fiushed 

comp[etely with clean air (AGA, Amsterdam, The Netherlands). 

After flushing, a sufficient time interval was ailowed to ensure that the flask temperature was 

stabilized at the desired test temperature before the next sample was injected. 

Preliminary test 

Starting at 200°C, every 20°C, 70 pl test substance was pipetted into the test vessel. 

The temperature rise was about 5°C/min. 

Going down from 490°C, the auto-ignition temperature was determined in temperature steps of 

5°C using the same injection voIume. 

Main studv 

The auto-ignition temperature was determined going down in steps of 2°C. In the first test, 50, 

70 and 100 pl test substance was injected at a temperature range of 458-444, 458-436 and 

458-450°C, respectively. In the second test, 50, 70 and 100 pI test substance was injected at a 

temperature range of 450-446, 446-436 and 460-448°C, respectively. ln the third test, 50, 70 

and 100 pl test substance was injected at a temperature range of 458-438, 456-432 arid 

460-450°C, respectively. 

Each test was performed using a clean test vessel. 

On each day of testing, the atmospheric pressure was rneasured. 
1,1,3,3-TETRAIVIETHYLBUTYLPEROXY PIVALATE NOTOX Project 

DATA HANl.7L 1NG 

The auto-ignition temperature is the Iowest temperature at which the test substance wifi ignife 

wnen mixed with air under the conditions defined in the test method. 

Deviatior7s meet the criteria as outiined in the protocol (repeatahility < 20°C when ari autoignition #emperature > 300°C is determined). 

In accordance with,DfN 51794, the lowest temperature at which ignition occurs in the test was 

rounded down to the tiearest 5°C and is given as the final auto-ignifion temperatut'e. 

RESULTS 

f'relirriinary test 

Starting at 200°C and testing every 20°C, a flame was observed at 480°C. 

Going down from 490°C and testing every 5°C, an autc-ignifiion temperature of 445°C was 

determined. 

Main study 

Figure 1 shows the correlation hetween injected test substance volume and the auto-ignition 

ter-operature for all tests<. 

The auto-ignition temperature for 1,1,3,3-TETRAi1AETHYLBUTYLPEROXY PIVALATE was 

436°C (lowest determined auto-ignition temperature), with an injection volume of 70 pi and a 

tirne iag of 08 s(see Table 1). 

The atmospheric pressure varied between'028 and 1030 hl'a. 

In conolusion, 1,1,3,3-TETRAMETHYLBUTYLF'EROXY PIVALATE is auto-ignitahEe, with an 

auto-ignition temperatiire of 435°C. 

Table I Summary of the results of the main study 

Test number Auto-ignition lnjected Time lag 

Temperature volume 

°C 1 s' 

'rest 1 448 50 08 

440 70 09 

454 10Q 04 

Test 2 450 50 08 

440 70 08 

452 100 07 

Test 3 442 50 07 

436 70 08 

454 100 06 

: 
I 

Figure 1 

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435 

450 

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430 

0 20 40 60 80 100 120 140 160 

Injected votume (jiI) 

—~-- Test 1 - - I- - Test 2 Test 3 

Correlation between auto-ignition temperature and injection volume for 

TETRAMETHYLBUTYLPEROXY PIVALATE. 

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1,1,3,3-TETRAMETHYLBUTYLPEROXY PIVAi.ATE NOTOX Project 

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1,1,3,3-TETRAMETHYI_.B[3TYLPEROXY PIVAI_.ATE NtpTOX Prroject ~~~ f 

APPENDIX: CERTIFCCATE OF ANALYS[S 

AKZO NOBEL - ~r ~ - t A , ~► ~- 

Centra! Research 

page 1 af 2 

tcs..33t 

Product name : 1,1,3,3-tetramethyIbufyI peroxypivalate 

Trade narrie ; _T-r~gonox 4 25 

Batch numlber 

~ 

T@st t"eSu1tS: 

> FEte code 

Artalytical documentation 

,Aufhorized by , _ _ 

rVame 

Function 

Date 

Signature 

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1,1 PNALATE NOT[ X . 

. cwntroyaeseonch 

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paneumu 

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