### . r,.

~ 

### ......._._- ~._~

• TX 425-C75 

### C.



# • 

# REPORT



# SANITiZED DETERMINAl"ION OF THE VAPOUR PRFSSIlRE OF 

## 1,2,3,3-TETRAMETHYLBUTYL PEROXYPIYALATE 

# • 11

Y 

## hIOTOX Projee ~ 

### ~ 

### NOTOX Substanee,_ ~ 

## ---._..... ~ 

## . - Page 1 af 12 - 

# • •
• 

# • C7,



# •

### 1,1, 3, 3-TETRANIETHYLBUTYL PEROXYPxVAL ATE NOTOX Project ;

~ 

### CONFIaENTIALITY STATEMENT

This report contains the unpublished results cf research sponsored by Akzo 

### Nohel Chemicals B.V.. Reproduction, lissue or disclosure to third parties in any form is not permitted vwlthout prior written authorization from the ~ 

### sponsor.

.


### 0 

## i L)t.. !._# ,: w ~ . t

1- 

### 1

~


### 13

1 ` 

### 1

LiJ

El


## E - Page 2 °

~

# 0

® 1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE NOTOX Projec t 

# ~ e STATEMENT OF GLP COMPLIANCE 0 NOTOX B.V., 's-Hertogenbosch, The Netherlands

The study described in this report has been correctly reported and was w 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 (FIFRA). Title 40 Code 

### of Federal Regulations Part,160. • The United States Environmental Protection Agency (TSCA). Title 40 Code of

Federal Regulations Part 792. ql Study Director

In~ J--fErips `- 

### Management J.A.M.W, van Helvoirt 

### ,— , 

### Head f—Cl.emiltry

LJ Da e • Date\

_ ~ ._..a -- ~ 

### Principal Scientist _ 

### Drs. A.C.G. van Genderen


# o 

# c /



### Date 

# 1 ~ Page 3


# •

## ® 1,1,3,3-TETRAMEFHYLBUTYL PEROXYPIVALATE NOTOX Proje;ct 

# ~
4 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 aud9ts are given below.

During the on-site inspections pracedures applicable to this type of study 

### were inspected.
• DATES OF QAU INSPECTIONS/AUDITS REPORTING LIATES 

### on-site inspection (s) 24 July 1997 24 July 1997 

### i protocol inspection (s) 29 May 1997 29 May 1997 report audit (s) R 27 August 1997 27 August 1997 

# i Head of Quality Assurance



### C.J. Mitchell B.Sc. • ~-~'~~' ~ 

# ---._-
~



### Da
~ 

### te .,



### i - Page 4 -


### 0

## C

, 

# ; .---_

1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE NOTOX Proje6` 

# a SUMMARY

The determination of the vapaur pressure was based on the following guidelines: European Economic Community (EEC),EEC directive 92/69 EEC, Part A, Methods for the determination of physico-chemical prnperties, A.4 "Vapour pressure", EEC Publication No. L383, December 1992. Organization for Economic Co-operation and Develapment (flECD), OECD guidelines for testing chemicals, Guideline No.104: "Vapaur pressure curve ° , adopted May 12, 1981. Using-the Static Technique, the vapour pressure of 1,1,3,3- TETRAMETHYLBUTYL PEROXYPIVALATE at 20°C was determined to be: p(20°C) = 300 ± 20 Pa = 2.25 ± 0.15 mm Hg. V, I.0



### U

❑ 

## 0

0 

# .;, u

❑ 

### Page 5 ❑

❑



## F,

## • 1,1,3,3-TETRAMETHYLBl1TYL PEl20XYPTVALATE NOTOX Projee 

# ~ ~

• PREFACE 

# • • Sponsor AKZO Nobel Chemicals B.V. P.O. Box 247 3800 AE AMERSFOORT The Netherlands Study Monitor 

# ~ Testing Facilities NOTOX B.V. Hambakenwetering 3 5231 DD 's-Hertogenbosch, The Netherlands

r. The test was performed at the Thermodynamic Centre Utrecht Utrecht University Padualaan 8 3584 C Utrecht, The Netherlands f `~-- - -~ ----- ~ ,s Study Director Principal Scientist • Study plan

TEST SUBSTANCE • .—

Identification Chemical name CAS No. • Description

Batch Purity Test substance storage Stability under storage conditians • Expiry date Drs. A.C.G. van Genderen (Utrecht University) Start : 13 August 1997 Completed : 13 August 1997
1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE Propaneperoxic 

### acid, 2,2-dimethyl-,1,1,3,3- tetramethylbutyl ester (9CI) 22288-41-4 _—Golourless liquid 

# Q See_C.er—ti-f°i - cate 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. 

# • • Page 6

•

# n

Li

~ .~



# n
❑



# n

~ 

# C ..----- ~



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

## ~ ct
PURPOSE AND PRINCIPLE The purpose of the study was to evaluate the vapour pressure of the test substance at 20 0 G. The vapour pressure is a function of the temperature and is specified in Pascal (Pa) or in mm Hg. One mm Hg equals 133.322 Pa. In the static process, at thermodynamic equilibrium, the vapour pressure established in a closed system is determined at a specific temperature. The measured results (ln p) are plotted versus the reciprocai temperature (in Kelvin) and 

### yield a rectilinear curve for the limited temperature range. GUIDEL-INES 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.4 °Vapour pressure', EEC Publication No. L383, December 1992. Organization for Economic Go-operation and Development (OECD), OECD guidelines for testing chemicals, Guideline No.104: 'Vapour pressure 

### curve°, adopted May 12, 1981. • 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 The Static Technique was used to determine the vapour pressure. 

### Recognized by the international guidelines as recommended test system (EEC, OECD). CALIBRATION OF THE TEST SYSTEM The Static Technique is calibrated periodically using the primary pressure standard type 6-201-0001 (CEC Division of Bell & Howell company, California, USA). - Page 7 ❑



## C3

❑

11

# • -

~ 

# .

1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE NOTOX Pro 

## ~ ect 

# `~ 

# ---_----' ~

• PERFORMANCE OF THE TEST

Static vapour pressure measurements were made with a capacitance manometer fitted with a 133 kPa capacitive sensor. The reference pressure at the right-hand side of the diaphragm of the pressure sensor was kept below • lD -4 Pa. The temperature of the sample was measured with a platinum

resistance thermometer. The sample vessel was cleaned, dried and filled with approximately 6.8 g of-the test substance. After attaching the vessel to the measuring set-up, it was evacuated during about 1 minute. The measurements were started at 24.08 °C. After measurement 14 the 

## ~ temperature of the thermostatic bath in which the sample vessei is

immersed was raised to 28.32 "C, after measurement 22 to 31.45 °C and finally after measurement 31 to 34.91 °C. A total of 52 measurements was performed. p DATA HANDLING

Because the measured vapour pressures were > 0.1 Pa, no correction according to Bennett and Tompkins (Trans Faraday Sac., 1957, 53, 185) for thermal transpiration was made. ` The test substance was considered to show ideal behaviour. Thus the vapour

pressure curve was derived according to Clarke and G1ew (Trans. Faraday Soc., 1966, 62, 539). The vapour pressure at 20°C was calculated from the vapour pressure curve.

~ RESULTS

The Static Technique was used for the determination of the vapour pressure at 20°C. • At the beginning of the test, the vapour pressure of the test substance

decreased slightly every next measurement, due to the removal of volatile impurities. After measurement 9 this decrease became negligible and the vapour pressure was stable. So from that moment on, the collected data were used for the final result. During the measurements at the third temperature the values of the vapour • pressures at subsequent measurements became higher, without doubt due to a

beginning decomposition of the test substance. Therefore only the value of the vapour pressure at the beginning of this series is used. This effect of increasing values became even more pronounced at the highest temperature and therefore the data collected at this temperature could not be used for the final result. • For each temperature, a selected number of ineasurements was used for the

calculations. These measurements are shown in the appendix added tD the report and plotted in Figure 1. The results of the calculations are summarized in Tab1e 1.

## ♦ - Page 8 -

•

# • 7 i „__` ~ ° o



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

`~~ 

# _.

5.5 0 10 20 30 40 6o measurement number 

### Figure 1 Graphical presentation of the vapour pressure measurements

(ln p versus number of ineasurements) of 1,1,3,3-TETRAMETHYLBUTYL 

### PEROXYPIVALATE. Table 1 Determination of the vapour pressure of 1,1,3,3-TETRAMETHYLBUTYL

PEROXYPIVALATE at 3 different temperatures, using the Static Technique. 

### Measurementt Temperature Mean vapour pressure ± 2csn-1 °C tn(p) Pa 10 - 14 24.08 5.95 1• 0.02 382 ± 8 17 - 22 28.32 6.16 ± 0.02 474 ± 10 24 31.45 6.36 580 ' A seiected number of ineasurements (see the appendix) was used for calculations. Note: The calculations were performed using not rounded values. 

# c
0 Page 9 - 

## 11


# n
C ❑


# i

## • 1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE NOTOX ProjeFt ~
~ The resulting values given in Table 1 were piotted against the reciprocal temperature IT
- 'j (in Kelvin; see Figure 2), taking into account the calculated error. ❑



## ~ 6.5

~ InipIPal 6,6

~

` 5.5 3.25 

### A 3.30 3.35 

### M.m Figure 2 Vapour pressure curve (ln p versus T -1 ) of 1,1,3,3-

TETRAMETHYLBUTYL PEROXYPIVALATE.

~ Fitting these data according to Clark & Glew gives a value of 299.3 Pa with

20.5 Pa for 2o n _1 (i.e. 6.6 °a) for the vapour pressure of the test substance at 20°C, The maximum deviation between the ftt and the data points is always less than about 1.6 %. Errors made in estimating the mean value per temperature series are up to 2%. So a value of 20 Pa (i.e. 6.6 %) is a reasonable value for the uncertainty in the final result. 

## • Conclusion,

The value of the vapour pressure of 1,1,3,3-TETRAMETHYLBUTYL PEROXYPIVALATE at 20°C was found to be: 

## 0 p(20°C) = 300 ± 20 Pa = 2.25 t 0.15 mm Hg.

n ~ Page 10

r , u

## ♦ r -,-.



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

# ~
APPENDIX

## ♦ Tabte of the vapour pressures, calculated from the raw data. p/Pa ln(p/Pa) Nr p/Pa 1n(p/Pa) Nr p/Pa In(p/Pa) 2 432 6.07 * 16 464.0 6.14 * 24 579.6 6.36

## ♦ 5 415 6.03 * 17 468.8 6.15 25 586 6.37 * 7 398.7 5.99 * 18 467.6 6.15 26 597 6.39 * 9 395.3 5.98 * 19 476.9 6.17 28 615 6.42 * 10 386.4 5.96 20 477.7 6.17 30 624 6.44 * 11 385.6 5.95 21 478.2 6.17 12 382.5 5.95 22 476.8 6.17 35 837 6.73 * + 13 379.3 5.94 40 909 6.81 '

14 378.4 5.94 45 954 6.86 * 50 979 6.89 ' [7 

### * Not used for calculations.

Note: The calculations were performed using not rounded values. 

# n
11
0

E
0
❑ Page il 

# C

## 1,1,3,3-TETRAMETHYL8U7YL PEROXYPIVALATE NOTOX Project 

# ~
! 

### CERTIFICATE OF ANALYSIS

— 

# 4 1 / = ! 

## AK7A NOBEL 

# Certificate ofAnalysis

IOS-33f 

### ! Piodu¢tname :1,1,3,3,-tetrameEhylbutylperoaypivalate Trada'name Trigbr 

# ~ o7c425 ~ 8atchnumbor 

### !

n

...
7 AnatyfIcal documenta8o 

# ~ ~ Ffle code 

# ! Authorizad 6

~ ' — Natue 

### FuncHon Data ` 

### Slgnafv 

### !

!


### ! Page 12 

# •