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# 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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- Page 1 of 12-1,1,3,3,-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.

-2-1,1,3,3,-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
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### tng. H.J. Krips

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~

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### Uate:

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### "7 r Management Dr. lr. H. Willerns

~~ -- Hea

~ of Chemist ry

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### -3-1,1,3,3,-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.

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Date ~~



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

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### 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.

-5-1,1,3,3,-TE T RAMETHYLBUTYt.PEROXY PfVALATE NOTOX Protect:

, ~ 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. 

### TES T S 

### YSTEM AN D RA 

### TIONA L 

### E 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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4 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.

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### 1,1,3,3,-TETRAMETHYLBUTYLPEROXY PIVAI

~ 

### ATE I

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### OTOX Proje t;

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

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

mz1,1,3,3,-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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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:

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File code
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Analyticai documentation (

~Authorized by,,r

### Name Function DaEe Signature

- 1 1 -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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