StudyTitle
Study Director

Test Facility

Sponsor

Internal distribution Study No. FINAL REPORT
Determination ofthe boiling point of accordingto OECD Guideline No. 103 (principle accordingto 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 numberof pages : 12 Page 2/12 Page



### 1 2 

### 3 4 

### 5 6 7 

### 8 

### 9 9 9 10 

### 11 12Study 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 forthe Environment, Forests and Landscape 

# p

March 31 -Apri11, 2005 

# lilntercantonal Office forthe Control of Medicines

was inspected by the Swiss Agency for the Environment, Forests and Landscape with respectto the compliance with the Swiss legislation on Good Laboratory Practice. Test Facility Areas ofexpertise

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 itwas inspected.

Bern, June 2005 Swiss Agency forthe Environment, Forests and Landscape
Philippe Roch

### Study No. - Final report Page 5/12
STATEMENT OF COMPLIANCE WITH GOOD LABORATORY PRACTICE: 

### Study No. Testsubstance 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. Testsubstance 

### 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

DateStudy 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 ofthe 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 MolecularWeight 

### 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. GENERALTEST 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 (101.325 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 awindowforthe observation ofthe 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 

### I5.0 

### I 10.0 

### I20.0 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 leavingthe 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: Firstdetermination: 122.3°C to 122.4

# oc 122.4°Cto 122.6

# oc Second determination: 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 underthe atmospheric pressure of 95.89 kPa. A correction of the temperature to normalised pressure (101.325 kPa) was made. The determination of this correction factor was made using the Sidney Young equation, as recommended in OECD guideline 103. Tn = 

### 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 Tn

## =normal boiling point With this correction made, it can be concluded thatthe 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 thatthe standard boiling point of is:
> 675.7 K (402.6 oc)