Study Title 

Study Director 

Test Facility 

Sponsor 

Internal distribution 

Study No. 

FINAL REPORT 

Determination of the melting point of 

according to OECD Guideline No. 102 (method of 

the capillary tube 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 

Office of 

Public Health 

It is hereby confirmed that 

during the period of 

the following Test Facility of 

Swiss Agency for the 

Environment, Forests 

and Landscape 

March 31 - April 1 , 2005 

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 813.016.51 at the 

time it was inspected. 

Bern, June 2005 

Swiss Agency for the Environment, 

Forests and Landscape 

Philippe Roch 
Study No. Final report Page 4/10 

STATEMENT OF COMPLIANCE WITH GOOD LABORATORY PRACTICE: 

Study No. 

Test substance 

Title Determination of the melting point of according 

to OECD Guideline No. 1 02 (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 of the results 

obtained. 

Study director 

Date: I 

Test Facility Management: 

Date: 
Study No. - Final report Page 5/10 

QUALITY ASSURANCE UNIT 

STATEMENT 

Study No. 

Test substance 

Study title Determination of the melting point of 

according to OECD Guideline No. 102 (method of the 

capillary tube in a liquid bath). 

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 and Types of QAU inspections 

January 9, 2007 

March 28, 2007 

Study plan 

Observation of the 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 accurately the raw data of the study. 

Manager, Quality Assurance Unit 

Date 
Study 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 for the Testing of Chemicals No. 102, Paris, 

1995 

92/69/EEC, method A.1. 

January 2nd, 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 

least ten years after issue of the 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 

Molecular Weight 

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 of the 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 holder with 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: ±1 0% 

- 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 Preliminary test 

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

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

First determination: 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 that the melting range of 

is: 

420.2 K to 424.5 K (147.0°C to 151.3°C)