. ~ 

REPORT 

uAMiT12M) 

DETER11ti1NATiON OF THE EXPL,OSIVE. PROPERTIES (LIQUI®S) OP 

1,1,3,3yTETRANfETHYi,13i1TYLPERO1CY PiVALATE 

NarOX PraAf 

NOTOX Substance i 

\, 

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1,1,3,3,-TETRAMFTHYL,BUTYLPEROXY PIVALATE NOI'OX PrQject 

CaNF1DEh1TIAI,iTY S`I"ATENIENT 

This report contains the unpubiishecl results of research sponsored by Akzo Nobel Chernicals 

B.V.. Eteproductiory, issue or disclosure to third parties in any form is not permittted vvithout prior 

written authorizatior} frorri the sponsor. 

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1,1,3,3,-TETFiAMETHYLBUTYLPEROXY PIVALATE NOTOX Project , ~ 

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STAT1=NlENT OF OLP COMPLIANCE 

NflTOX B.V., 's-Hertogenhosch, The Netherlands 

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

with the most recent edition of: 

The OECD Principles of Good Lahoratory 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 

Regu(ations Part 160. 

The United States E'nvironmental Protection Agency (TSCA). Title 40 Code o€ Federaf 

Regulations Part 792. 

Study Director. 

tng. H.J. Krips 

. 

~y. 

~ 

. ~ 

Uate: 

, 

"7 r 

Management 

Dr. lr. H. Willerns 

~~-- Hea~ of Chemistry 

t R ~ 

~ ~'~t3at -~ 

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1,1,3,3,-TETRAlV1ETHYLBUTYLPEROXY PIVALATE NOTOX Project 

QUALjTY ASSURANCE STATENIENT 

NOTaX 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. 

Durirtg the on-site inspections procedures applicable to tnis type of stc!dy were inspected. 

DATES QF QAU INSPECTiONSIAUDITS REPORTING DATES 

on-site inspection (s) 

28 July 1999 

protocol inspection (s) 

10 September 1999 

report audlt {s} 

03 October 1999 

28 July 1999 

10 Septem fjer 1999 

03 October 1999 

Fiead of QuaEity Assurance 

C.J. Mitchel! B,Sc. 

.~~.~. 

„j 

~ 

Date ~~ 

~ 

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_.._~~

. 

1,1,3,3,TETRAMETHYLBUTYLPEROXY PIVALATE NOTOX Project 

. 

SUMMARY 

The determination of the explosive properties of 1,1,3,3, TETRAMETHYLBUTYLPEROXY 

PIVALATE was performed in accordance with EEC-Directive 92/69 EEC, A.14 "Expiosive 

properties" (1992). 

Exposing 1,1,3,3,•TETRAMETHYLBUTYLPEROXY PIVAt.ATE for 300 s to thermal stress 

resulted in fierce reactions. At afl tests using a 6 and 2 mm orifice, a report was heard. No 

deformation of the test tubes was observed. Because no test tube deformation was observed, 

it was concluded that the test substance Is not explosive when exposed to therrnal stress. 

Exposing 1,1,3,3,-TETRAMETHYLBUTYLPEROXY PiVALATE to mechanical stress by shock, 

did not result in any visual changes in the test substarice consistency. No traces ofi a vigorous 

reaction were observed. 

From this it was concluded that the test substance does not react under mechanical stress by 

shock, therefore, has' not to be seen as expfosive. 

In conclusion, 1,1,3,3,-TETRAMETHYLBUTYLPEROXY PIVAt.ATE is not explosive when 

exposed to therma4 or mechanical stress under the conditions of the test. 

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1,1,3,3,-TE T RAMETHYLBUTYt.PEROXY PfVALATE NOTOX Protect: 

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t \` J•! 

PREFACE 

Sponsor AKZO iVobel ChemicaEs B.V. 

P.O. Box 247 

3800 AE Arnersfoort 

The Nethe.r(.ands 

Study Monitor 

Testing Facility NOTOX B.V. 

Hambakenwetering 3 

5231 DD's-Hertogenbosch 

The Neti~ eriands 

- 

~ 

Stuoy Director • 

Study Pian Start : 21 September 1999 

Completed : 23 September 1999 

TEST SUBSTANCE 

identification 

AKZO Nobel trade name 

Chemioal narne 

CAS n o. 

Description 

Satch Number 

Purity 

Test substance storage 

Stability under storage conditions 

E'xpiry date 

1,1,3,3,-TETRAMETHYL,SUTYLPEROXY PiVALATE 

Trigonox 428 

1,1,3,3-Tetramethylhutylperoxy pivalate 

22288-41-1 

firj.uic_. 

` -See--Certificate-of Arialysis 

in freezer in the dark 

Stable 

01 January 2000 

The sponsor is responsible for the completeiiess and GLP Compfiance of afi 

test substance data, 

PURPaSE 

The purpose of the study is to deterrnirie whether or not the test substance presents a danger of 

explosion when subrnitted to the effect of a flame (thermal sensitivity) or to impact (sensitivity to 

mechanical stimufi). 

GUIDELINES 

The study procedures described in this report are based on the zolfowing guideline: 

European Economy Cornmunity (EEC), EEC-Directive 92/69 EEC, Part A, Niethods for the 

deterrnination of physico-chemicai properties, A.14 "Explosive propQrties", EEC Publication No. 

ir383, Decernber 1992. 

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1,1,3,3,-TETRAMETHYLBUTYLPEROXY PIVALATE NOTOX Proect 

ARCHIVING 

Na74X B.V. will arcnive the following data for at ieast 10 years: 

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

withdrawn without the sponsor's written consent. 

TEST SYSTEM AN D RATIONALE 

Thermal sensitivity: 

Steel tubes made by drawing sheet steel, with an internal diameter of 24 mm, a length of 75 mm 

and a wall thickness of 0.5 mm were used. The tubes are supplied by Julius Peters and the 

quality is controlled by the Bundesanstalt fur Materialpriifung BAM, both in Berlin (FRG). 

The open end of the test-tube was provided du(ng #he test with a pressure resistant, circular 

nozzle plate with a central hole. This piate was tirmly secured to the top of the tube with the aid 

of a two-part screw;oint. The nozzle plate is 6 mm thick and made from heat-resistant chrome 

steel). 

Mechanicai_ sensitivity by shock : 

A gravity fallhammer apparatus, cons+sting of a cast steel block with foot and anvil, column, 

guides, drop weight and a release mechanism taccording to the specifications of the 

Bundesanstalt fur Materialprufung (BAM) in f3erlin (FRG), Explosivstoffe Vol. 6(1958) pp. 

178-189, 202-214, and 223-235) was used. 

Mechanical sensitivity by friction : 

Not applicable because 1,1,3,3,-TETRAMETHYLBUTYLPEROXY PIVALATE is a liquid. 

Rationale: 

Recognized by the internationaf guidelines as recornmended test system (EEC). 

VALIDATION OF THE TEST SYSTEM 

The ternperature increase during the thermal sensitivity test is va(idated periodically, using 

dibuty{ phthalate and a calibrated thermocouple. The results are in accordanoe with the criteria 

of the EEC-Directive. 

PREPARATIONS BEFORE THP TEST 

Thermal sensitivity: 

The test substance was filled into the tube to a height of 60 mm (the amount of test substance 

was 27 mi). 

Mechanicai sensitivity by shock: 

Approximately 40 pi test substance was pipetted in a die device consisting of two coaxial steel 

cylinders, one above the other and a holiow steel cylinder as the guiding ring (All specifications 

according to standards of BAM). 

The upper steel cylinder was pressed ddwn until it was at a distance of approximate(y I mm 

from the lower cylinder and was hefd in th3s position. 

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1,1,3,3,-TETRAMETRYLBUTYLPERflXY PIVALATE NQTOX Proje6t. 

PERFORIVIANCE QF TF(E T t✓ ST 

Preliminar~: 

The preliminary test was not perforrrmed: 

Niain study 

Thermal sensitivity: 

The test tube was heated using industrial qua(ity propane delivered through a caiibrated 

pressure controlter (5868; Brfloks lnstrtrrnerit B.V., The Netherlands), the pressure was set to be 

70 mbar. The gas flow was nieasured by means of a calibrated tfiermal mass fEow controller 

(5850E; Brooks lnstrument B.V., The Netherlands). The gas was distributed by a manifold to 

four burners. The four burners consumed 3.01 of the propane per minute. The construction of 

the "! Frners is as rrecified in the directive: 

Two series of three tests were performed, the first series using a noz,7-le-plate with a hole of 

6 mm diarrreter, the second using a hole of 2 mm diameter. 

Submission of the test substance to thermal stress was terminated after 300 s. 

Mechanical sensitivity: 

In the speGified impact apparatus, six tests were performed dropping a 10 kg mass from (}.4 m. 

DATA HANdLING 

Therrrtal sensitivity; 

TYre test substance is eoncluded to be explosive wherc in otie of the tests, the test Wbe bi,rst ir?ta 

three or mnre fragments. 

SVlechanical sensitivity: 

Tfre test substance is cor7cfuded to be explosive when in one of the six tests, the test substance 

shows a vigorous reaction (i.e. bursting into flames, crepitation or reports). 

RESULTS 

Thermal sensitivity: 

A summary of the nbservation.s is outlined in Table 1, the resufts are outlineci in l -abfe 2. 

Exposing the test substance for 300 s to thermal stress resulted in fierce reactions. 

At ail tests using a 6 and 2 mm orifice, a report was heard. No deformation of the test tubes was 

observed. Because no test tube deformation was observed, it was concluded that the test 

substance is not explosive when exposed to ti7ermal stress. 

Mechanical sensiti'vity by sbock: 

A summary af the resuEts is given in Table S. 

Exposing the test substance to rnechanica( stress by shock, did not resuft in any visual changes 

in the test .3ubstance consistency. No traces of a vigorous reaction v+rer'e observed. 

From this it was concluded that the test substance does not react under mecnanical stress by 

shock, therefore, has not to be seen as explosive. 

in cor3clusion, 1,1,3,3,-TBTRAMi`THYLBUTYZPEROXY PIVAt.ATE is not explosive wherr 

exposed to thermal or mechanical stress under the conditions of the test. 

: 
~1,1,3,3,-TETRAMETHYLBUTYLPEROXY PIVAI ~ ATE I~OTOX Proje t; 

Table I Summary of Qbservations during the submission of 1,1 t3,3,- 

TETRAMETHYLBUTYL,PEROXY PIVALATE to thermal s#ress. 

Qiameter of 

orifice 

mm 

Time till 

reaction 

s j 

Observations 

6 23 lncreasing #lames 

28 report 

33 decreasing flames 

6 20 Increasing flames 

26 report 

29 decreasing flames 

6 21 )ncreasing flames 

30 report 

37 decreasing flames 

2 20 Increasing flames 

28 report 

35 decreasing flames 

2 23 Increasing flames 

29 reporfi 

33 decreasing flames 

2 20 Increasing flames 

23 report 

30 decreasing flames 

I Total heating time 300 seconds, none of the test tube showed any deformation. 

Table 2 Summary of the results of the exposure of 

TETRAMETMYl.BUTYLPEROXY PJVALATE to thermal stress. 

Test ho orifice bf the 

nozzle plate 

reaction explosion 

-t 6 mm re ort no 

2 6 mm re ort no 

3 6 mm re ort no 

4 2 mm re ort no 

5 2 mm re ort no 

6 2 mm re ort no 

mz 
1,1,3,3,-TETRAMETHYL.BUTYLpERQXY PIVALATE NQTOX Project 

Tahle 3 Summary of the results of the exposure of 1,1,3,3,- 

TETRAMETHYLBUTYLPEROXY PiVALATE to mechanical stress (shock) 

Test no reaction ex losion 

I -- no 

2 -- no 

3 °- no 

4 -- no 

5 -- no 

6 n o 

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1,1,3,3,-TETRAME'THYLBUTYLPEROXY PIVALATE NC7TOX Pro;eci; f 

APPENDIX: CERTlFlCATE UF ANALYSIS 

AKZO NOBEL - ♦ - ♦ ~ ~ ~ 

Central Research 

page 1 of 2 

tcs-33t 

luct name' : 1,1,3,3-te#ramethyEbutyl peroxypivaiate 

ie name ; TrigoDo 25 

~.~ 

:h number : 

Te,st resutts: 

~. 

! 

., 

., 

t. 

-.,. 

File code 

Analyticai documentation ( f 

~ 

Authorized by,,rName 

Function 

DaEe 

Signature 

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1,1,3,3,7'ETRAMETHYLBUTYLPr=ROXY PIVALATE NOTOX Prole t 

AKZONOBEL 

.Central Research 

page 2 of 2 

Triaonox 425 batcfi 

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