Study Title 

Study Director 

Test Facility 

Sponsor 

Internal distribution 

Study No. 

FINAL REPORT 

Determination of the boiling point of 

according to OECD Guideline No. 103 (principle 

according to Siwoloboff) 

Archives 

Author. 
Study No. - Final report 

CONTENTS: 

Title page 

Contents 

Signatures 

Statement of GLP compliance (Swiss GLP monitoring authorities) 

Statement of GLP compliance (Study Director) 

Quality Assurance Unit 

Summary 

1. General information 

2. Information on the test substance 

2.1 . Identity 

3. 

4. 

5. 

2.2. Physical-chemical and analytical data 

General test method 

Results 

Conclusion 

Total number of pages : 12 

Page 2/12 

Page 

1 

2 

3 

4 

5 

6 

7 

8 

9 

9 

9 

10 

11 

12 
Study No. - Final report Page 3/12 

Signatures: 

Study director 

Date: 

Test Facility Management: 

Date: 
Study No. - Final report Page 4/12 

The Swiss GLP Monitoring Authorities 

Swiss Federal 

Office of 

Public Health 

m 

It is hereby confirmed that 

during the period of 

the following Test Facility of 

t 

Swiss Agency for the 

Environment, Forests 

and Landscape 

p 

March 31 -Apri11, 2005 

li 

lntercantonal Office 

for the Control of 

Medicines 

was inspected by the Swiss Agency for the Environment, Forests and Landscape with 

respect to the compliance with the Swiss legislation on Good Laboratory Practice. 

Test Facility Areas of expertise 

The inspection was performed in agreement with the OECD Guidelines for National GLP 

Inspections and Audits. It was found that the aforementioned test facility was operating in 

compliance with the Swiss Ordinance on Good Laboratory Practice [SR 813.016.5] at the 

time it was inspected. 

Bern, June 2005 

Swiss Agency for the Environment, 

Forests and Landscape 

Philippe Roch 
Study No. - Final report Page 5/12 

STATEMENT OF COMPLIANCE WITH GOOD LABORATORY PRACTICE: 

Study No. 

Test substance 

Title Determination of the boiling point of according 

to OECD Guideline No. 103 (principle according to 

Siwoloboff) 

This study has been performed in compliance with the Swiss Ordinance relating to 

Good Laboratory Practice, adopted May 18th, 2005 [RS 813.112.1 ]. This ordinance is 

based on the OECD Principles of Good Laboratory Practice, as revised in 1997 and 

adopted November 26th, 1997 by decision of the OECD Council [C(97)186/Final]. 

The undersigned declares that this study was carried out according to the procedures 

herein described and this report represents a true and accurate record of the results 

obtained. 

Study director 

Date: 
Study No. - Final report Page 6/12 

QUALITY ASSURANCE UNIT 

STATEMENT 

Study No. 

Test substance 

Title Determination of the boiling point of according 

to OECD Guideline No. 103 (principle according to 

Siwoloboff) 

Test facilities are periodically inspected and the results are reported to the responsible 

persons and the management. 

Experimental procedures were periodically inspected. The study plan and this final 

report were audited by the Quality Assurance Unit. The dates are given below: 

Dates of Reports to 

Dates and Types of QAU inspections the Study Director and 

to the Management 

April 04, 2008 Study plan April 04, 2008 

April 07, 2008 Observation of the boiling point April 07, 2008 

April 15, 2008 Final report April 15, 2008 

The methods and procedures as used in the reference study are accurately described 

in this document and reported results reflect accurately the raw data of the study. 

Manager, Quality Assurance Unit 

Date 
Study No. - Final report Page 7/12 

SUMMARY 

The boiling point of was measured according to OECD Guideline No. 103 

(principle according to Siwoloboff). The result can be expressed as follows: 

The boiling point of > 675.7 K (402.6 oc) 
Study No. - Final report Page 8/12 

1. GENERAL INFORMATION 

Study No. 

Purpose Determination of the boiling point of according 

to OECD Guideline No. 1 03 (principle according to 

Siwoloboff), using an electronically controlled heating device. 

Guidelines 

Study Director 

Laboratory 

Technician 

Schedule: 

OECD Guideline for the Testing of Chemicals No. 103, Paris, 

1995 

Study initiation date March 31, 2008 

Start of experiments : April 07, 2008 

End of experiments : April 07, 2008 

Study completion date: April 15, 2008 

Archives The study plan, all data generated and recorded during the 

study and the final report will be stored in the Archives of the 

for at 

least ten years after issue of the final report. 
Study No. - Final report Page 9/12 

2. INFORMATION ON THE TEST SUBSTANCE 

2.1 . Identity 

Commercial name 

Code No. 

Chemical nature 

Empirical formula 

Molecular Weight 

CAS No. 

2.2. Physical-chemical and analytical data 

-General 

Aspect 

- Sample tested 

Lot No. 

Purity 

Expiration date October 18, 2008. 
Study No. - Final report Page 10112 

3. GENERAL TEST METHOD 

3.1. Introduction 

For the determination of the boiling point of the method of the capillary 

tube was used. A small amount of the test item was heated in the electronically 

temperature controlled sample block, the sample was observed visually for any possible 

changes in appearance, consistency and colour. 

The phase transition from liquid to vapour is deduced by the continuous formation of 

steam bubbles leaving the inserted boiling capillary. 

3.2 Definitions and units 

The standard boiling point is the temperature at which the vapour pressure of a liquid is 

the same as the standard pressure (1 01.325 kPa). 

Conversion of units t [°C] = T [K] - 273.15 

Where: 

t = Celsius temperature [°C] 

T = Thermodynamic temperature Kelvin [K] 

3.3 Equipment 

The boiling point was determined using a Buchi 8540 boiling point device (Buchi, Flawil, 

Switzerland). The device consists of an electrically heated and electronically controlled 

heating block for the capillary, and a window for the observation of the capillary. 

The technical data are: 

- temperature range: room temperature to 400°C 

- temperature programming: 0.1 I 0.2 I 0.5 I 1.0 I 2.0 I 3.0 I 5.0 I 10.0 I 20.0 oclmin 

- accuracy of the electronic thermometer: 

• 0 ....... 1 00 oc: ±0.3°C 

• 100 .... 250 oc: ±0.5°C 

• 250 ... .400 oc: ±0.8°C 

- dimensions of the capillary tube: 

• internal diameter: 2 mm 

• length : 80 mm 

• closed at one end. 

3.4 Preliminary test 

In a preliminary test no boiling was observed up to 400 oc (not corrected for pressure). 

Observation: Melting point at - 150.3 oc. 
Study No. - Final report Page 11/12 

3.5 Boiling point determination 

A capillary tube filled with the test substance to a height of 5 mm was placed in the 

instrument. The substance was molten and the boiling capillary was inserted. The 

sample was heated to 1 ooc below the approximate boiling point, then at rate 

0.5°C/minute. The sample was visually observed for the formation of steam bubbles 

leaving the inserted boiling capillary. This determination was done in duplicate. 

4. RESULTS 

4.1. Accuracy checking 

The accuracy of the instrument was checked by determining the melting point of a 

certified sample of benzoic acid (certified boiling point: 122.2°C). The results was: 

First determination: 122.3°C to 122.4 oc 

Second determination: 122.4°C to 122.6 oc 

4.2. Boiling point determination 

First determination 

Second determination 

: no boiling observed up to 400 oc 

: no boiling observed up to 400 ac 

4.3 Correction to normalized pressure 

No boiling was observed up to a temperature of 400 oc under the atmospheric pressure 

of 95.89 kPa. A correction of the temperature to normalised pressure (1 01.325 kPa) 

was made. The determination of this correction factor was made using the Sidney 

Young equation, as recommended in OECD guideline 103. 

T n = T + ( h · flp) 

Where: flp = 101.325 kPa- p 

p = pressure in kPa ; the pressure was obtained from the Swiss 

meteorological service for the time of the experiment; 

fT = rate of change of boiling temperature with pressure in KlkPa, here a 

value of 0.47 KlkPa, as published in DIN 53171, was used. 

T = temperature in K 

T n = normal boiling point 

With this correction made, it can be concluded that the standard boiling point of 

is: 

> 675.7 K (402.6 oc) 
Study No. - Final report Page 12/12 

5. CONCLUSION 

From the tests described above, it can be concluded that the standard boiling point of 

is: 

> 675.7 K (402.6 oc)