REPORT 

Study Title: 

DETERMINATION OF THE FREEZING POINT I FREEZING RANGE 

AND OF THE BOILING POINT I BOILING RANGE OF DEA/Acid 

anhydride reaction product 

Data Requirement I Test Guidelines: 

OECD No. 1 02, 1 03 

EEC Directive 92/69, A.1 and A.2 

Study Director: 

Mrs. Alessandra Tognucci 

Study Completion Date: 

December 17, 2003 

Test Facility: 

RCC Ltd 

Environmental Chemistry & Pharmanalytics 

CH-4452 ltingen/Switzerland 

Sponsor: 

Rockwoollnternational A/S 

Hovedgaden 584 

DK-2640 Hedehusene 

Denmark 

RCC Study Number: 

848616 

Page 1 of 15 
RCC Study Number 848616 

DEA/Acid anhydride reaction product 

GLP CERTIFICATE 

REPORT 

The Swiss GLP Monitoring Authorities 

Swiss Federal 

Offioe of 

Public Health 

Swiss Agency for the 

Environment. Forests 

and Landscape 

~ Swissmedic 

r . Swiss Agency for SW1ssmed1c TherapeutlcProducts 

Statement of GLP Compliance 

It is hereby confirmed that 

during the period of 

the following Test Facilities of 

November 18 - 22, 2002 

RCC Ltd 

4452 ltingen 

Switzerland 

were inspected by the Federal Office of Public Health, the Swiss Agency for Therapeutic 

Products and the Swiss Agency fo'r the Environment, Forests and Landscape with respect to 

the compliance with the Swiss legislation on Good Laboratory Practice. 

Test Facilities 

-Toxicology 

-Environmental Chemistry and 

Pharmanalytics 

Areas of expertise * 

TOX, ACC, MUT, 

OTH (Safety Pharmacology) 

ACC, ECT, ENF, EMN, PCT, 

RES, OTH (Animal metabolism) 

The inspections were performed in agreement with the OECD Guidelines for National GLP 

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

compliance with the Swiss Ordinance relating to Good Laboratory Practice [RS 813.016.5] at 

the time they were inspected. 

Bern, March 2003 

Federal Office of Public Health 

The Director 

Prof. Th. Zeltner 

• TOX:: Toxicology : ACC =Analytical and Clinical Chemlstty : ECT = Environmental toxicity on aquatic and terrestrial 

organisms : ENF = Behaviour In water. soli and air. Bioaccumulation ; EMN =Studies on effects on mesocosms and natural 

ecosystems: MUT • Mutagenicity; PCT =Physical-chemical testing: RES= Residue studies: OTH:: Other, to be specified. 

Page2 
RCC Study Number 848616 

DEA/Acid anhydride reaction product 

GOOD LABORATORY PRACTICE 

REPORT Page 3 

STATEMENT OF COMPLIANCE 

RCC Study Number: 

Test Item: 

Study Director: 

Title: 

848616 

DEA/Acid anhydride reaction product 

Mrs. Alessandra Tognucci 

Determination of the Freezing Point I Freezing 

Range and of the Boiling Point I Boiling Range of 

DEAl Acid anhydride reaction product 

This study was conducted in compliance with the Swiss Ordinance relating to Good 

Laboratory Practice, adopted February 2nd, 2000 [RS 813.016.5]. This Ordinance is based on 

the OECD Principles of Good Laboratory Practice, as revised in 1 997 and adopted November 

26th, 1997 by decision of the OECD Council [C(97)1861Final] . 

. Study Director: 
RCC Study Number 848616 REPORT Page4 

DEAl Acid anhydride reaction product 

SIGNATURES 

Study Director: 

Management: Dr. Jorn Schreitmuller 

.... aJJ.~ ................................... . /1~~ 1t r ckJo3 
RCC Study Number 848616 

DENAcid anhydride reaction product 

REPORT 

QUALITY ASSURANCE UNIT 

RCC Ltd, Environmental Chemistry & Pharmanalytics, CH-4452 ltingen I Switzerland 

STATEMENT 

RCC Study Number: 848616 

Test Item: DEA/Acid anhydride reaction product 

Study Director: Mrs. Alessandra Tognucci 

Page 5 

Title: Determination of the Freezing Point I Freezing Range 

and of the Boiling Point I Boiling Range of DEA/Acid 

anhydride reaction product 

The general facilities and activities are inspected periodically and the results are reported to 

the responsible person and the management. 

Study procedures were periodically inspected. The study plan and this report were audited by 

the Quality Assurance Unit. The dates are given below: 

Dates and Types of QAU Inspections Dates of Reports to the Study 

Director and to the Management 

June 06, 2003 Study Plan June 06, 2003 

September 23, 2003 Process based September 23, 2003 

December 02 I 03, 2003 Final report December 03, 2003 

This statement also confirms that this final report reflects the raw data. 

Quality Assurance: J Margot Richter-Auer 
RCC Study Number 848616 

DEA/Acid anhydride reaction product 

CONTENTS 

REPORT Page 6 

GLP CERTIFICATE ........................................................................................................ 2 

STATEMENT OF COMPLIANCE .................................................................................... 3 

SIGNATURES ................................................................................................................ 4 

QUALITY ASSURANCE UNIT ........................................................................................ 5 

CONTENTS .................................................................................................................... 6 

PREFACE ....................................................................................................................... 7 

DATA REQUIREMENT I TEST GUIDELINES ................................................................ 8 

SUMMARY OF STUDY PLAN AMENDMENTS .............................................................. 8 

1 PURPOSE ............................................................................................................. 9 

2 MATERIAL AND METHODS .................................................................................. 9 

2.1 TEST ITEM ................................................................................................... 9 

3 FREEZING POINT I FREEZING RANGE ............................................................ 10 

3.1 PRINCIPLE OF THE TEST ........................................................................ 10 

3.2 PERFORMANCE OF THE TEST ................................................................ 10 

3.2.1 Preliminary Test ............................................................................ 10 

3.2.2 Main Test ...................................................................................... 10 

. 4 BOILING POINT I BOILING RANGE ................................................................... 11 

4.1 PRINCIPLE OF THE TEST ........................................................................ 11 

4.2 PERFORMANCE OF THE TEST ................................................................ 11 

4.2.1 Test System .................................................................................. 11 

4.2.2 Preliminary Test ............................................................................ 11 

4.2.3 Main Study .................................................................................... 11 

5 DATA HANDLING ................................................................................................ 12 

5.1 FREEZING POINT I FREEZING RANGE ................................................... 12 

5.2 BOILING POINT I BOILING RANGE .......................................................... 12 

6 RESULTS ............................................................................................................ 13 

6.1 FREEZING POINT I FREEZING RANGE ................................................... 13 

6.2 BOILING POINT I BOILING RANGE .......................................................... 13 

6.3 CONCLUSION ............................................................................................ 14 

Figure 1: DSC-curve for the determination of the boiling of DEA/Acid anhydride 

reaction product (preliminary test) .............................................................. 15 
RCC Study Number 848616 

DEA/Acid anhydride reaction product 

PREFACE 

GENERAL 

Title: 

Sponsor: 

Study Monitor: 

Test Facility: 

RESPONSIBILITIES 

Study Director: 

Deputy Study Director: 

Technical Coordinator: 

Reporting: 

Head of RCC Quality Assurance: 

SCHEDULE 

Experimental starting date: 

Experimental completion date: 

Study completion date: 

ARCHIVING 

REPORT Page 7 

Determination of the Freezing Point I Freezing Range 

and of the Boiling Point I Boiling Range of DEAl Acid 

anhydride reaction product 

Rockwool International A/S 

Hovedgaden 584 

DK-2640 Hedehusene 

Denmark 

Mr. Flemming A. Simonsen 

Danish Toxicology Centre 

Kogle Aile 2 

Dk-2970 H0RSHOLM 

Denmark 

RCC Ltd 

Environmental Chemistry & Pharmanalytics 

Zelgliweg 1 

CH-4452 ltingeniSwitzerland 

Mrs. Alessandra Tognucci 

Mr. Michael Lindemann 

Mrs. Barbara FIOkiger and Mr. Christoph Wild 

Dr. HansjOrg Widmer 

Mrs. Iris Wuthrich 

October 16, 2003 

October 30, 2003 

December 17, 2003 I wih 

RCC Ltd, CH-4452 ltingeniSwitzerland will retain the study plan, raw data, a sample of test 

item and the final report of the present study for at least ten years. 

No data will be disca~ded without the sponsor's consent. 
RCC Study Number 848616 REPORT PageS 

DEAl Acid anhydride reaction product 

DATA REQUIREMENT I TEST GUIDELINES 

This study followed the procedures indicated by the following internationally accepted 

guidelines and recommendations: 

EEC Directive 92/69, Part A, Methods for the determination of physico-chemical properties, 

A.1 "Melting/Freezing temperature", EEC Publication No. L383, December 1992. 

EEC Directive 92/69, Part A, Methods for the determination of physico-chemical properties, 

A.2 "Boiling temperature", EEC Publication No. L383, December 1992. 

OECD Guideline for Testing of Chemicals No. 102, "Melting Point I Melting Range", adopted 

July 27, 1995. 

OECD Guideline for Testing of Chemicals No. 103, "Boiling Point", adopted July 27, 1995. 

SUMMARY OF STUDY PLAN AMENDMENTS 

First Amendment to Study Plan: 

1) Concerning: Study Title 

Alteration: Melting Point I Melting Range replaced by 

Freezing Point I Freezing Range 

Reason for Alteration: Physical state of test item at room temperature is liquid 

2) Concerning: Schedule 

Alteration: Anticipated experimental starting date 

Anticipated experimental completion date 

Anticipated date of draft report 

Reason for Alteration: Test item batch delivered later 

3) Concerning: Test Item 

Alteration: New batch used for study 

New expiration date 

Reason for Alteration: New batch to be used by request of sponsor 

RCC Study Number 848616 REPORT Page 10 

DEAl Acid anhydride reaction product 

3 FREEZING POINT I FREEZING RANGE 

3.1 PRINCIPLE OF THE TEST 

The above mentioned guidelines contain several different methods for the determination of 

the freezing point I freezing range. These are, between others, thermal analysis using a 

calorimeter and visual test (e.g. capillary method), where the melting or freezing temperature, 

respectively, is measured. In the present study a combination of both methods was applied. 

The test item was cooled down slowly in a glass tube immersed into a cooling bath, while the 

consistency of the sample was judged visually. Thermocouples were inserted into the sample 

with the aim to utilise the heat effect of a phase transformation for the detection of the 

freezing point. 

3.2 PERFORMANCE OF THE TEST 

3.2.1 Preliminary Test 

1 ml of the test item was filled into a vial and stored in a freezer for 27 hours at about- 21 oc. 

After storage, the sample was assessed visually. 

3.2.2 Main Test 

In a first test, about 15 ml of the test item were filled in a test tube and cooled down using 

acetone and dry ice. The probe of a thermocouple was placed in the centre of the sample. 

· The temperature was measured with an appropriate thermocouple. A second and third test 

was carried out with about 20 ml of test item. The temperature/time curves were recorded 

during the cooling of the test item. Additionally, the physical state was observed visually. 
RCC Study Number 848616 REPORT Page 11 

DEAl Acid anhydride reaction product 

4 BOILING POINT./ BOILING RANGE 

4.1 PRINCIPLE OF THE TEST 

The above mentioned guidelines contain several different methods for the determination of 

the boiling point I boiling range. These methods include thermal analysis using a calorimeter 

and visual tests (e.g. capillary tester), where the boiling temperature is measured. In the 

present study the thermal analysis was used for the preliminary and main test . 

A phase transformation, e.g. melting or evaporation, or a reaction, e.g. dissociation, usually is 

associated with a heat effect. 

In the calorimeter, two identical aluminium sample containers, one filled with the test then 

and the other empty (used as a reference), are heated at a constant rate. During the 

experiment, the heat effect, i.e. the difference in heat flow, between the sample container and 

the reference container is registered. 

4.2 PERFORMANCE OF THE TEST 

4.2.1 Test System 

Thermal Analysis (Preliminary and Main Test) 

Instrument: 

Sample cups: 

Test conditions: 

Reference cup: 

4.2.2 Preliminary Test 

Differential Scanning Calorimeter 

DSC 821, Mettler Toledo 

Aluminium cups with a normed pinhole. 

The test was performed in an air atmosphere. 

Empty aluminium cup. 

A test item amount of 8.24 mg was heated up from 25°C to 400°C at a rate of 20 K/min. The 

quantities of heat absorbed or released were measured and recorded. Before and after the 

test, the weight and the appearance of the sample were determined. 

4.2.3 Main Study 

A test item amount of 8.31 mg was heated up from 25°C to 400°C at a rate of 10 K/min. The 

quantities of heat absorbed or released were measured and recorded. Before and after the 

test, the weight and the appearance of the sample were determined. 
RCC Study Number 848616 REPORT Page 12 

DEN Acid anhydride reaction product 

5 DATA HANDLING 

5.1 FREEZING POINT I FREEZING RANGE 

The freezing point is defined as the temperature at which phase transition from liquid to solid 

state at normal atmospheric pressure takes place. This temperature ideally corresponds to 

the temperature at the melting point. As the phase transition of many substances takes place 

over a large temperature range, it is often described as . the freezing respectively melting 

range. 

Results will be given in degrees Centigrade and in Kelvin. 

5.2 BOILING POINT I BOILING RANGE 

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

liquid is the same as the standard pressure (1 01.325 KPa). The measured boiling point 

depends on the atmospheric pressure. 

Thermal Analysis 

As the phase transition from liquid to vapour of many substances takes place over a large 

temperature range, it is often described as the boiling range. If the difference between the 

temperature at the beginning and at the final stage of boiling is within 1 K, the temperature at 

the beginning of boiling is taken as the boiling point, otherwise the two temperatures will be 

reported. 

A correction to normalized pressure can be made. Because the correction factor for the 

· boiling point is a specific parameter for each test item, the correction factor had to be 

determined. The determination of this correction factor by the used method is not applicable, 

therefore no correction will be applied to the boiling point observed. 

Conversion of units (K to °C): 

t = T- 273.2 

with 

t = Celsius temperature, degrees Centigrade [°C] 

T = Thermodynamic temperature, Kelvin [K] 
RCC Study Number 848616 

DENAcid anhydride reaction product 

6 RESULTS 

REPORT 

6.1 FREEZING POINT I FREEZING RANGE 

Page 13 

The determination of the freezing point I freezing range of. the test item was performed 

according to the EEC Directive 92/69, A.1 "Melting/Freezing temperature .. , December 1992 

and to the OECD Guideline No. 1 02: .. Melting point I melting range .. , adopted July 27, 1995. 

A preliminary test was performed to check if the test item becomes solid if stored in a freezer 

at about - 21 oc. About 1 ml of the test item was placed in a small vial and stored for 27 hours 

at about - 21 oc. After storage the sample was judged visually and was found to be at the 

physical change from highly viscous to solid. Based on this observation the freezing point I 

range was around - 21 oc. 

During the main tests, 15 ml and twice 20 ml of the test item DEAl Acid anhydride reaction 

product were placed in a test tube and cooled down from room temperature to about - 53°C 

(first test), - 32°C (second test) and - 25°C (third test) using a dry ice and acetone mixture. 

From the recorded temperature curves, no freezing point or range could be deduced. 

By visual observation during the first test, the test item began to solidify at - 16. 7°C and was 

solid at- 29.6°C. During the second test, the test item was very viscous at- 19.8°C and was 

completely solid at - 20.9°C. During the third test, the test item turned very viscous in the 

temperature range from - 21.1 to - 22.6°C and was completely solid at - 22.9°C. The first test 

was not used for the result evaluation, as something inhibited the freezing of DEA/Acid 

anhydride reaction product. 

In conclusion, the freezing range for DEA/Acid anhydride reaction product was determined 

to be at 

which is equal to 

- 20.9°C to - 22.9°C 

250.3 K to 252.3 K. 

6.2 BOILING POINT I BOILING RANGE 

The determination of the boiling point I boiling range of the test item was performed 

according to the EEC Directive 92/69, A.2 "Boiling temperature .. , December 1992 and to the 

OECD Guideline No. 103: .. Boiling point .. , adopted July 27, 1995. 

The DSC-curve of the preliminary test (heating rate of 20 Klmin from 25°C to 400°C) is 

shown in Figure 1 . Endothermic heat effects were observed between about 1 oooc and about 

260°C. After the experiment, the sample had lost 55.7 °/o of its mass and black foam had 

formed around the pinhole of the aluminium cup. The colour of the sample residue in the cup 

had changed to black. 

The DSC-curve of the main test (heating rate of 1 0 Kim in from 25°C to 400°C) showed 

endothermic heat effects in the temperature range from about 1 oooc to about 260°C. After 

the experiment the sample had lost 62.3 o/o of its mass and black foam had formed around 

the pinhole of the aluminium cup. The colour of the sample residue in the cup had changed to 

black. 
RCC Study Number 848616 

DEA/Acid anhydride reaction product 

REPORT Page 14 

The test item DEA/Acid anhydride reaction product is a complex mixture of monomers, 

dimers, trimers and polymers that also contains water. Therefore, the endothermic effects 

observed cannot be deduced to boiling only but are combined effects of boiling and 

polymerisation. 

In conclusion boiling and polymerisation of DEA/Acid anhydride reaction product was 

observed between 

which is equal to 

6.3 CONCLUSION 

1 oooc and 260°C 

373 K and 533 K. 

The freezing range of DEAl Acid anhydride reaction product was observed between 

Boiling and polymerisation of DEAl Acid anhydride reaction product was observed 

between 1 oooc and 260°C. 
Aexo 

mw 

0 

-30 

-40 

Experiment: 848616/DEA/boil_pt1/16.10.2003/wic, 16.10.2003 10:18:48 

Methodenname: PreTest 25-400/20°C/min/Air 

Methode: PreTest 25-400/20°C/min/Air 

25.0-400.0°C 20.00°C/min 

50 100 150 

&848616/DEA/boil_pt1/16.10.2003/wic 

848616/DEA/boil_pt1/16.10.2003/wic, 8.

200 250 300 

RCC Ltd: PhysChem METTLER TOLEDO