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# REPORT 

# SANNTtZED DETERMINATION OP TIHE AUTO-IGNITtON TEMPERATURE (LIQUIUS) OP

1,1,3,3-TETRAMEThiYLBUTYLPEROXY PIVALATE

;..-- ~..~ iVOTOX Project ~ NOTOX Substan 4

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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.



### -2-1,1,3,3-TETRAMETHYLBUTYLPI*ROXY PiVAt,ATE 

### iVOTdX i'roject

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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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# ~ Management Dr. lr. H. Willems Head of Chemistry


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-3-C- ~ ,,,.... ~ .. ~ '` 1, 1 ,3, 8 -TETRAMF''HY L BUTYLPFROXY PIVAf.ATE NOT 

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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. .........

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D~ ~ 13 July 1999 z 1 Febcuary 1999 

### 'tfi August 1999

-4-/' `n .'.--•..•,,. ~ 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.



# _5-1,1,3,3-"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
~ Start : 08

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~ "999 St u dy Plan 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.

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

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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. R ESU LTS 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

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### Correlation between auto-ignition temperature and injection volume for TETRAMETHYLBUTYLPEROXY PIVALATE. ,r Ir,.. ......-;,,,,,

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m1,1,3,3-TETRAMETHYI_.B[3TYLPEROXY PIVAI_.ATE NtpTOX Prroject
~~~ f APPENDIX: CERTIFCCATE OF ANALYS[S 

### AKZO NOBEL - ~r ~ 

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### - 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:

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Artalytical documentation ,Aufhorized by , _ _ rVame Function Date Signature



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