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TX 425-C75 

fla 

REPORT 

SANITIZED 

DETERMINATION OF THE BOILING TEMPERATURE OF 

1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE. 

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NOTOX Project( 

NOTOX Substance 

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

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CONFIDENTIALITY STATEMENT 

• This report contains the unpublished results of research sponsored by Akzo 

Nobel Chemicals B.V.. Reproduction, issue or disclosure to third parties 

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

sponsor. 

(J3`ciTv 

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Study Director Management 

• In Qr JiLi. Krips J.A.M.W. van Helvoirt 

Head of Chemistry , 

Date:\ 

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

STATEMENT OF GLP COMPLIANCE 

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 (FIERA). Title 40 Code 

of Federal Regulations Part 160. 

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

Federal Regulations Part 792. 

• Principal Scientist 

DE-a-3- van Ekeren 

• (1:— ----- 

Oat\ 

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1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE NOTOX 

• 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 INSPECTIONS/AUDITS REPORTING DATES 

on-site inspection (s) 

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24 July 1997 24 July 1997 

protocol inspection (s) 

29 May 1997 29 May 1997 

report audit (s) 

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11 August 1997 11 August 1997 

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Head of Quality Assurance 

C.J. Mitchell B.Sc. 

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1,1,3,3-TETRAMETNYLBUTYL PEROXYPIVALATE NOTOX Projedi 

SUMMARY 

The determination of the boiling temperature was based on the following 

guideline: 

• EEC-Directive 92/69 EEC, Part A, Methods or the determination of physicochemical properties, A.2 "Boiling temperature°, EEC Publication No. L383, 

December 1992. 

Using a differential scanning calorimeter (DSC), both test substance and a 

reference were heated, using one single heat source. The difference between 

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the enthalpy change which occurs was recorded. 

At temperatures above about 57°C (330 K) the test substance reacts or 

decomposes. Boiling of 1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE was not 

observed. 

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

PREFACE 

Sponsor 

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AKZO Nobel Chemicals B.V. 

P.O. Box 247 

3800 AE AMERSFOORT 

The Netherlands 

Study Monitor 

Testing Facilities 

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NOTOX B.V. 

Hambakenwetering 3 

5231 DD 's-Hertogenbosch, The Netherlands 

The test was performed at the 

Thermodynamic Centre Utrecht 

Utrecht University 

Padualaan 8 

84—M-Utrach47—Th Netherlands 

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Study Director 

Principal Scientist 

Study plan 

”chiticahT—ilniversity) 

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Start : 24 July 1997 

Completed : 24 July 1997 

TEST SUBSTANCE 

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Identification 

Chemical name 

CAS No. 

Description 

Batch 

Purity 

Test substance storage 

Stability under storage 

conditions 

Expiry date 

1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE 

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

tetramethylbutyl ester (9CI) 

22288-41-4 

(—Colourless liquid 

N---bee—L-per44411-cate of Analysis 

In freezer in the dark 

Stable 

Not indicated 

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The sponsor is responsib 

test substance data. 

le for the completeness and GLP Compliance of all 

PURPOSE AND PRINCIPLE 

The purpose of the study was to evaluate the boiling temperature/boiling range 

of the test substance. Therefore, both test substance sample and reference 

were heated, using one single heat source. The difference between the enthalpy 

change which occurs was recorded. 

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

GUIDELINES 

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

guidelines: 

European Economic Community (EEC), EEC-Directive 92/69 EEC, Part A, Methods 

for the determination of physico-chemical properties, A.2 'Boiling 

temperature', EEC Publication No. L383, December 1992. 

Organization for Economic Co-operation and Development (OECD), OECD guidelines 

for Testing of Chemicals, guideline no. 103: 'Boiling point', July 27, 1995. 

ARCHIVING 

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

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

TEST SYSTEM AND RATIONALE 

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The test was performed 

DSC-50Q): 

. Detection limit: 

Sample container: 

- Reference: 

using a Differential Scanning Calorimeter (Shimadzu 

approx. 10 pW 

aluminium; closed with a lid in which a small hole was 

drilled. 

sample container filled with alumina. 

The test system is recognized by the international guidelines as recommended 

test system (EEC) 

TEST SUBSTANCE TREATMENT 

The test substance was used untreated. 

PERFORMANCE OF THE TEST 

Preliminary test: 

An amount of 5.00 mg test substance was heated from 24 to 95°C (297 - 368 K) 

with a rate of 20°Chnin. 

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1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE NOTOX 

Main study: 

The main study was not performed because boiling of the test substance was not 

observed. 

• Conditions: 

The preliminary test was performed under a flow of air (about 100 ml/min). 

After the experiment, the mass of the sample was measured and the sample was 

inspected visually. 

• DATA HANDLING 

The standard boiling temperature is defined as the temperature at which 

the vapour pressure of a liquid is the same as the standard pressure 

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(101.325 kPa). 

From a DSC-curve, the boiling temperature of a pure substance is evaluated as 

the cross point of the extrapolated base line and the linear part of the 

rising section of the evaporation peak. 

• The results are given in degrees Celsius (°C) and Kelvin (K). 

RESULTS 

0 Preliminary test: 

The DSC-curve which was registered during the preliminary test is plotted in 

Figure 1. At temperatures above about 57°C (330 K) an exothermic effect was 

observed. This effect is probably caused by reaction or decomposition of the 

test substance. During the test the sample lost 4.73 mg (95%) of its mass. 

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Main study: 

The main study was not performed because boiling of the test substance was not 

observed. 

• Conclusion: 

At temperatures above about 57°C (330 K) the test substance reacts or 

decomposes. Boiling of 1,1,3,3-TETRAMETHYLB1JTYL PEROXYPIVALATE was not 

observed, 

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1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE 

DSC 

mW 

NOTOX Projeei _ 

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20.00 40.00 60.00 

Temp[C] 

80.00 100,00 

Figure 1 DSC-curve of 1,1,313-TETRAMETHYLBUTYL PEROXYPIVALATE 

• Preliminary test. 

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1,1,3,3-TETRAMETNYLBUTYL PEROXYPIVALATE NOTOX Projecr 

CERTIFICATE OF ANALYSIS 

AKZO NOBEL Cenificate of Analysis 

Central Research 

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1CS-331 

. • Peodifat 

'Trade:name 

BatOnumber 

: - tetramethylbutyl peroay pivafate 

:-Tricienox 425 

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Aria!Oa! docuthontatter? 

Flie code 

. -.. • Adthothed 

fluiD 

rtiectlee 

Date." 

Shipieite 

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MUMS 

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