• • • • • • • • • • • • TX425-C75 REPORT SANITIZED DETERMINATION

OF THE FREEZING TEMPERATURE
OF 1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE ( ,---...._. NOTOX Project

\ NOTOX Substance '----./ - Page
1 of 9

·••••••••••••1,1,3,3-TETRAMETHYLBUTYLPEROXYPlVALATECONFIDENTIALITYSTATEMENTNOTOXProject/Thisreportcontainstheunpublishedresu1tsofresearchsponsoredbyAkzoNobelChemicalsB.V..Reproduction,issueordisclosuretothirdpartiesinanyformisnotpermittedwith_outpriorwrittenauthorizationfromthesponsor.Page2 -• • • • 1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE 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 DECO 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 (riFRA}. Title 40 Code of Federal Regulations Part 160. The United States Environmental Protection Agency (TSCA}. Title 40 Code of Federal Regulations Part 792

. Study Director Management • c-'"'' **"2';Kc"~"** J.A.M.W. van Helvoirt .. **-~d-o.f~istry** ( **~-~~** " "'\

) ' **oat~**

Date: •

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## • • 1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE QUALITY ASSURANCE STATEMENT **"~** NOTOX Pro **jec~** --..,?·-· 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 on-site inspection (s) 22 July 1997 protocol inspection (s) 29 May 1997 report audit (s) 31 July 1997 Head of Quality Assurance C.J. MitGhell B.Sc

. '- Date: 

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· REPORTING DATES 22 July 1997 29 May 1997 31 July 1997• •

··- ·-·--------, **~-----** / ....._ 1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE
NOTOX **Proje~**

) **------~·** SUMMARY The determination
of the freezing temperature
of 1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE was based on EEC-Directive 92169 EEC, A.l 'Melting/Freezing temperature (1992) and on OECD Guideline no. 102 'Melting Point/Melting Range' (1981). In a preliminary test it was found that 1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE does not solidify at a temperature
of ·82'C (191 K). From this it was concluded that the freezing temperature
of 1,1,3,3- TETRAMETHYLBUTYL PEROXYPIVALATE is< -82'C (< 191 K)
. - Page 5
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# • 1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE 

### !~ NOT OX Pro **jet~** '---------::" PREFACE Sponsor Study Monitor Testing Facility Study-Director Study Plan TEST SUBSTANCE Identification Chemical name CAS No. Descrirtion Batch Purity Test substance storage Stability under storage conditions Expiry date AKZO Nobel Chemicals B.V. P.O. Box 247 3800 AE AMERSFOORT The Netherlands 

## /...----- ----...._ ; r 

### ' Hambakenwetering

3 5231 DD 's-Hertogenbosch The Netherlands --"""-· 

## --") '-. Start

: 14 July 1997 Completed

: 14 July 1997 1,1,3,3-tetramethylbutyl peroxypivalate Propaneperoxic acid, 2,2-dimethyl-,1,1,3,3- tetramethylbutyl ester {9CI) 22288-41-4 c1ourless **.l_~uid o~errTTl<:ate** 

of Analysis In 

### freezer in the dark Stable Not indicated The sponsor is responsible for the completeness and GLP Compliance
of all test substance data. PURPOSE • The purpose of the study was to eva1uate the freezing temperature
of the test substance

. 

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-- -·-···---------, 1,1,3,3·TETRAMETHYLBUTYL PEROXYPIVALATE GUIDELINES The study procedures described
in this report are based on the following guidelines: Organization for Economic Co-operation and Development (OECD), OECD Guidelines for Testing of Chemicals, Guideline no. 102 'Melting Point/ Melting Range", May 12, 1981. European Economic Community (EEC), EEC-Directive 92169 EEC, Part A, Methods for the determination

of physico-chemical properties, A.l "Melting/Freezing temperature", EEC Publication No. L383, December 1992. 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 Test system Rationale
The test was performed using
a jacketed sample tube with stopper to support

a calibrated thermometer and a brass stirrer, placed in a vacuum flask. Recognized
by the international guidelines
as recommended test system (EEC, OECD)

. VALIDATION
Of THE TEST PROCEDURE The test procedure
as outlined in this report is validated periodically, using n·octane and water. The results are in accordance with the NOTOX criteria for validation. PERFORMANCE
OF THE TEST Preliminary test: An initial trial determination was performed to make an estimation
of the freezing point/freezing range of 1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE.

In this test, approximately

5 ml test substance was stored for 1 hour at a temperature
of 5'C (:278 K), -29'C (244 K) and ·82'C (191 K). After this period, the test substance was visually checked. . Page 7

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## • • 1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE
NOTOX 

### Proj~ '-----L

/ Main study: The main study was not performed. DATA HANDLXNG The difference between the temperature
at the beginning and at the final stage of freezing is within

1 K, therefore, the temperature
at the final stage of freezing is taken as the freezing point. Results are given in degrees centigrade ('C) and in Kelvin (K) • RESULTS Preliminary test: Results are shown in table 1. Table 1. Observations during preliminary test

. Temperature Observations ·c (K) after
1 hour 5 (278) liquid -29 (244)

1 i quid -82 (191) liquid • Main study: 

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## • The main study was not performed. During the preliminary test, it was found that 1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE remained

a liquid without showing any indication of a freezing process. In conclusion, the freezing point of 1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE is< -a2•c (< 191 K)
.

- Page 8 -1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE

**~---** NOTOX Projeq:f

. "--------) CERTIFICATE
OF ANALYSIS 47= AKZONOBEL Certificate of/Analysis :·

. •'·' Pro'cli.iet niima **·rr~d&'ruime** satchnumbar :_ .....

: 1,1,3.3
.- telramethylbutyl peroxy pivalate cl'rigonax 425 . ':'"'--.:=

- **"""-·--~ -~--.**  **A?_a;y~~~ ~~cunlan~tJ.of_y----**  -) . . .

I **~II~~?a~**

\ . . ·.· .. **:~~- Atithoi-l~~d**  hv-···-.--·
-. : ______

_ Nariie:'

.·

- rU:r1cuOn Data-

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