# • 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 - Page 1 of 10 - 

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### 0 1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE NOTOX Project -------, ) 

### 0 CONFIDENTIALITY STATEMENT

• This report contains the unpublished results of research sponsored by Akzo Nobel Chemicals B.V.. Reproduction, issue or disclosure to third parties • in any form is not permitted without prior written authorization from the

sponsor. 

# (J3`ciTv

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0

- Page 2 — 

### 0Study Director Management
• In 

### Q

r J iLi. 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\ - Page 3 - 

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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)

• 24 July 1997 24 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. 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 O 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 

### 0 AKZO Nobel Chemicals B.V. P.O. Box 247 3800 AE AMERSFOORT The Netherlands Study Monitor Testing Facilities 

# •
4 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 

# • Study Director

Principal Scientist Study plan ”chiticahT — ilniversity)

_ Start : 24 July 1997 Completed : 24 July 1997 TEST SUBSTANCE 

# • • 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 -

per444 1 1-cate of Analysis In freezer in the dark Stable Not indicated



# • 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. - Page 6 - 

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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 

# •
0 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 • (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. 

# • 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 

# • • 1CS-331 . • Peodifat 'Trade:name BatOnumber : - tetramethylbutyl peroay pivafate

:-Tricienox 425 

# • • Aria!Oa! docuthontatter? Flie code

. -.. • Adthothed fluiD rtiectlee Date . " Shipieite 

# •

MUMS 

## - Page 10 - 

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