. 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This report contains the unpublished results cf research sponsored by Akzo 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 

QSee_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 -4Pa. 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 

—41= /

! 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 

•