Study Title
Study Director
Test Facility

Sponsor

Internal distribution Study No. FINAL REPORT Determination ofthe melting point of accordingto OECD Guideline No. 102(method of the capillarytube in a liquid bath).

Archives Author.Study No. - Final report
CONTENTS:

Title page Contents Statement of GLP compliance (Swiss GLP monitoring authorities) Statement of GLP compliance (Study Director) and signatures 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 : 10 Page 2/10 Page

1 2 

### 3 4 5 

### 6 7 8 8 

### 8 9-10 10 10

### Study 

### No. - 

### Final report Page 3/10

The Swiss GLP Monitoring Authorities Swiss Federal Officeof Public Health

It is hereby confirmed that during the period of the following Test Facility of SwissAgencyforthe Environment, Forests and Landscape

March 31 - April 1 , 2005 lntercantonal Office forthe Controlof 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 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 813.016.51 at the time it was inspected.

Bern, June 2005 Swiss Agencyforthe Environment, Forests and Landscape
Philippe RochStudy No. Final report Page 4/10
STATEMENT OF COMPLIANCE WITH GOOD LABORATORY PRACTICE: Study No. Testsubstance Title Determination ofthe melting point of according to OECD Guideline No. 102 (method of the capillary tube in a liquid bath). 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 declare that this study was carried out according to the procedures herein described and this report represents a true and accurate record ofthe results obtained. Study director

Date: I

Test Facility Management:

Date:Study No. - Final report Page 5/10
QUALITYASSURANCE UNIT STATEMENT Study No. Testsubstance Studytitle Determination of the melting point of according to OECD Guideline No. 102 (method ofthe capillary tube in a liquid bath). Testfacilities 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 reportwere audited by the Quality Assurance Unit. The dates are given below: Dates and Types of QAU inspections January 9, 2007 March 28, 2007 Study plan Observation ofthe melting range Final report Dates of Reports to the Study Director and

to the Management January 9, 2007 March 28, 2007

The methods and procedures as used in the reference study are accurately described in this document and reported results reflect accuratelythe raw data ofthe study. Manager, QualityAssurance Unit

DateStudy No. - Final report Page 6/10
SUMMARY

The melting point of was measured according to the OECD guideline No. 102 (method of the capillary tube in a liquid bath). The result can be expressed as follows: Melting range of 420.2 K to 424.5 K (147°C to 151.3°C)Study No. - Final report Page 7/10


### 1. GENERAL INFORMATION Study No. Purpose Guidelines
Study Director Laboratory Technician Schedule: Study initiation date Start of experiments : End of experiments : Study completion date: Archives Determining the melting point of using the method known as the capillary tube in a liquid bath method. OECD Guideline forthe Testing of Chemicals No. 102, Paris, 1995 92/69/EEC, method A.1.

January2nd, 2007 March 27, 2007 March 29, 2007

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 leastten years after issue ofthe final report.Study No. - Final report Page 8/10


### 2. INFORMATION ON THE TEST SUBSTANCE 2.1. Identity Commercial name Code No. Chemical nature Empirical formula MolecularWeight CAS No. N/A



### 2.2. Physical-chemical and analytical data -General Aspect

- Sample tested Lot No. Purity (GC) Expiration date May 14, 2007.

### Study No. Final report Page 9/10


### 3. GENERAL TEST METHOD 

### 3.1. Introduction is a solid at room temperature. The method of the capillary tube in a liquid bath is applicable. 3.2 Definitions and units The melting point is the temperature at which the transition from solid to liquid state takes place at atmospheric pressure. Sl unit is Kelvin (K). Frequently the transition from solid to liquid phase takes place over a temperature range. Therefore, the term "melting range" is often used and, in practice, the temperatures ofthe initial and final stages are determined. 3.3 Equipment Melting point apparatus (type 535, Buchi, Flawil, Switzerland) comprising:

- a stirred, electrically heated, programmable-temperature silicone oil bath

- an electronic thermometer (Pt 1 00)

- a capillary tube holderwith lighting and magnifying glass The technical data are:

- temperature range: room temperature to 280°C

- temperature programming: 0.5; 1; 2; or 3°C/minute

- precision of the temperature programming: ±10%

- accuracy of the electronic thermometer: 

# • o .......2oooc: ±O.rc • 200....280°C: ±1

# oc

- dimensions of the capillary tube: • internal diameter: 1 mm • length : 80 mm • closed at one end. 3.4 Preliminarytest No preliminary test was made, since the estimated melting point was already known from another experiment (safety test 2005-269, Differential Scanning Calorimetry). 3.5 Melting point determination A capillary tube filled with the test substance to a height of 2 mm was placed in the instrument and heating was started, at first at 3°C/minute to 1 

# ooc below the approximate melting point, then at 0.5°C/minute. The sample was observed and the temperatures corresponding to the beginning and the final stages of melting were recorded.Study No. - Final report Page 10/10
These determinations were done in duplicate. 

### 4. RESULTS 4.1. Accuracy checking The accuracy ofthe instrumentwas checked by determining the melting point of a certified sample of benzoic acid (certified melting point: 122.2°C). The results was: Firstdetermination: 121.4°C to 123.7

# oc Second determination: 121.6°C to 123.7°C 

### 4.2. Melting point determination First determination: beginning : 147.0°C final : 151 .3°C Second determination: beginning : 147.0°C final : 151 .3°C 

### 5. CONCLUSION From the above-described tests, it can be concluded thatthe melting range of is: 420.2 Kto 424.5 K (147.0°C to 151.3°C)