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REPORT 

SAIVITIZED 

® DETERMINATION OF THE FLAStf-F'O.INT OF 

1,1,3,3-TETRAMPTHYLBUTYL PEftOXYPIVALATB 

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NOTOX Project 

NOTOX Substancel 

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1,1,3,3-TETRAMETHYLBUTYL PER?XYPIVALATE NdTOX Project 

~ CDNFYDENTIALITY'STASEMENT 

This rep4rt contains the unpublished results of research sponsored by Akzo 

Nohel Chemicals B.V.. Reproduction, issue or disclflsure to third parties 

~ in any form -is not permitted without prior written authorization from the 

sponsor. 

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1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE NOTOX Project, 

STATEMENT OF GLP COMPLIANCE 

NOTOX B.V., 's-Nertogenbosch, 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 Cotle 

of Federal Regulations Part 160. 

The United States Environmental Protection Agency (TSCA). Tit1e 40 Code of 

Federal Regulations Part 792, 

E Study Director Management 

I n g. Ji. l-- IFeTps e J.A.M.W. van Helvoirt 

Head--of_ Ghemistry 

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1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE NOTOX Proje<t 

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QUALITY ASSURANCE STATEMENT 

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

This report was audited by the NOTOX Quality Assurance Unit to ensure that 

the methods and results accurately reflect the raw data. 

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

During the on-site inspections procedures applicable to this type of study 

were inspected. 

DATES OF QAU INSPECTTONS/AUDITS REPORTING DATES 

on-site inspection (s) 

14 July 1997 14 July 1997 

protocol inspection (s) 

29 May 1997 29 May 1997 

report audit (s) 

11 August 1997 11 August 1997 

Head of Quality Assurance 

C.J. Mitche7l B.Sc. 

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1,1,3,3•TETRAMETHYLBUTYL PEROXYPIVALATE NOTOX Projec( 

SUMMARY 

The determination of the flash-point of 1,1,3,3-T£TRAMETHYLBUTYL 

PEROXYPIVALATE was performed using a Pensky-Martens closed cup flash-point 

apparatas, in accordance with EEC-Directive 92/69 EEC, A.9 'Flash-point" 

(1992) and DIN £N 22719: "Bestimmung des Fiammpunktes Verfahren nach PenskyMartens im geschlossenen Tiegel'; August 1985. 

The flash-point of 1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE is <1°C when using 

a Pensky-Martens closed cup flash-point apparatus. 

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1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE NOTOX Project 

• PREFACE 

Sponsor AKZO Nobel Chemicals B.V. 

P.O. Box 247 

3800 AE AMERSFOORT 

TheNethe~Iands 

Study Monitor C a 

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Testing Facility NOTOX B.V. 

Hambakenwetering 3 

5231 DD 's-Hertogenbosch 

The Netherlands 

Study Director 

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Study Plan 

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Start '-34"~uly 1997 

Completed : 30 July 1997 

TEST SUBSTANCE 

Identification 1,1,3,3-tetramethylbutyl peroxypivaiate 

Chemical name Propaneperoxic acid, 2,2-dimethyl-,1,1,3,3- 

tetramethyibutyl ester (9CI) 

CAS No. 22288-41-4 

Description olourles s liquid 

Batch 

Purity ee Gert`3f"icate of Analysis 

Test substance storage In freezer in the dark 

Stability under storage 

conditions Stable 

Expiry date Not indicated 

The sponsor is responsibie for the completeness and DLP Compliance of a11 

test substance data. 

PURPOSE 

The purpose of the study was to evaluate the flash-point of the test 

substance. 

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1,1,3,3-TETRAM6THYLBUTYL PEROXYPIVALATE NOTOX Projec` 

n GUIDELINES 

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

guidelines: 

European Economic Community (EEC), EEC-Directive 92169 EEC, Part A, 

Methods for the determination of physico-chemical properties, A.9 °Flashpoint', EEC Publication No. L383, December 1992. 

DIN EN 22719: "Bestimmung des Flammpunktes Verfahren nach Pensky-Martens 

im geschlossenen Tiegel'; August 1985. 

ARCHIVING 

NOTOX B.V. wi11 archive the following data for at ieast 10 years: 

protocol, report, test substance reference sample and raw data. 

TEST SYSTEM AND RATIONALE 

® Test system A Pensky-Martens closed flash-point tester (according 

to DIN EN 22719). 

Conditions The apparatus was placed in a fume-cupboard. The window 

of the cupboard was left open to reduce the draft to a 

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minimum. 

Rationale Recognized by the international guidelines as 

recommended test system (EEC, DIN). 

VALIDATION OF THE TEST PROCEDURE 

The test procedure as outlined in this report is validated periodically, 

using p-xylene (zur synthese; Merck, FRG). 

The results are in accordance with the NOTOX criteria for validation. 

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1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE NOTOX Project ~4 

i PERFORMANCE OF THE TEST 

Preparations 

The cup of the flash-point apparatus was filled with the sample to be 

4 tested to the level indicated by the filling mark. The lid, with a 

thermocouple for detection of the flash point and a resistance thermometer 

for measuring the sample temperature, was placed on the cup. Thereafter, 

the cup was placed in the heating block. 

Performance of the test 

The test substance was heated in the apparatus with a temperature rise of 

approximately 5-6 0 C/m9n. The samp1e was stirred while being heated. 

The test flame was applied so that the flame was lowered into the vapour 

space of the cup in 0.5 s, left in its lowered position for 1 s, and 

quickly raised to its high position. The sample was not stirred while the 

test flame was applied. 

Preliminary test 

The test substance temperature was 15°C at the start of the test. 

Starting at 18°C, a test flame was applied at each 2°C temperature rise. 

~ Main study 

The test substance temperature was 10°C, 3°C and 0°C at the start of test 

one, two and three, respectively. 

Starting at 12°C, 4°C and 1°C a test flame was applied at each 1°C 

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temperature rise. 

The test was performed in triplicate. 

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DATA HANDLING 

The flash-point is the lowest temperature at 101.3 kPa, at which the test 

liquid in a closed test vessel evolves vapours, under the conditions 

definetl in the test method, in such amount that a flammable vapour(air 

mixture will be produced in the test vesseT. 

The (lowest) flash-point temperature was corrected'for the atmospheric 

pressure. 

Corrected flash-point = C+ 0.25 (101.3 - p) 

where: C = (iowest) observed flash-point [°C] 

p = ambient barometric pressure [kPa] 

The corrected flash-point is reported in °C and rounded off to 1°G. 

RESULTS 

Preliminary test: 

Flash-point: i8°C 

Main study: 

Table 1: Determined flash-points during the main study. 

Test number Flash-point 

[°C] 

Lowest Flash-point 

[°C] 

1 12 

2 4 1 

3 1 

The atmospheric pressure on the day of the test, was 102.0 kPa. 

The lowest flash-point was corrected for the atmospheric pressure. 

11 Corrected flash-point = <1 + 0.25(101.3-102.0)°C 

In conclusion, the flash-point of 1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE 

is <1°C under the conditions of the test. 

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1 , 1 ,3,3-TETRAMETHYL6UTYL PEROXYPIVALATE NOTOX Project

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❑ CERTIFICATE OF ANALYSIS 

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AKZO NOBEL 

 Cenrml Reseorch 

fCS332 

Pioduct name : t,t,3,3 - tetramethyl6ulyl peroxy pivalale 

"Trade name --T.rignnox425 

8atc,hnumber ~1 

Arie(yHcal doeumenfa9on 

Ffla eode 

/iuthorizsd bo----, 

Name ' 

Funcfion 

Dafu ' 

Stpnahira 

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