# REPORT
StudyTitle: 

### DETERMINATION OFTHE RELATIVE DENSITY OF DEAl Acid anhydride reaction product
Data RequirementITestGuidelines: OECD No. 109 EEC Directive 92/69, A.3 Study Director: Mrs. AlessandraTognucci StudyCompletion Date: December 10, 2003 Test Facility: RCC Ltd Environmental Chemistry&Pharmanalytics CH-4452 ltingen/Switzerland Sponsor: Rockwool International A/S Hovedgaden 584 DK-2640 Hedehusene Denmark RCC Study Number: 848617 Page 1 of 13RCC Study Number848617 REPORT DEAl Acid anhydride reaction product 

# GLP CERTIFICATE
The Swiss GLP Monitoring Authorities
Swiss Federal Officeof Publlc Health SwissAgencyforthe Environment. Forests and Landscape Swissmedic / • SwissAgencyfor SWlSSm

## ed1C Therapeutic Products 

# Statement of GLP Compliance

Itis herebyconfirmed that during the period of thefollowingTest FaciiHies 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 Agencyforthe 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 ofexpertise* 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. Itwas 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 theywere inspected.

Bern, March 2003 Federal Office ofPublic Health The Director

Prof. Th. Zeltner

•TOX =Toxicology :ACC =Analyticaland Clinical Chemistly : ECT = Environmental toxicityon aquatic and terrestrial organisms : ENF= BehaviourIn water, soil and air. Bioaccumulation : EMN =Studieson effects on mesocosms and natural ecosystems: MUT • Mutagenicity; PCT • Physicak:hemlcal testing :RES

## = Residue stud)es ;OTH •

**~·** to bespecified. Page 2RCC Study Number848617 DEA/Acid anhydride reaction product 

### GOOD LABORATORY PRACTICE REPORT



# STATEMENT OF COMPLIANCE

RCC Study Number: 848617 Test Item: DEAl Acid anhydride reaction product Study Director: Mrs. Alessandra Tognucci Title: Determination of the Density of DEAl Acid anhydride reaction product Page 3

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

Study Director: 

# lv

**Date:~**RCC Study Number848617 REPORT Page4 DEAl Acid anhydride reaction product 

# SIGNATURES

Study Director: Tognucci

Management: Dr. Jorn SchreitmOIIer



# ~-1~~~~~·····~···················RCC Study Number848617 DEAl Acid anhydride reaction product REPORT Page 5 

# QUALITY ASSURANCE UNIT
RCC Ltd, Environmental Chemistry & Pharmanalytics, CH-4452 ltingen 

### I Switzerland STATEMENT RCC Study Number: 848617 Test Item: DEAl Acid anhydride reaction product Study Director: Mrs. Alessandra Tognucci Title: Determination of the Density of DEAl 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 October 17, 2003 Measurements October 17, 2003 December 02 

### I 03, 2003 Final report December 03,2003 This statement also confirms thatthis final report reflects the raw data. Quality Assurance: Margot Richter-Auer



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# 3RCC Study Number848617 REPORT Page 6 DEAl Acid anhydride reaction product 

# CONTENTS
GLP CERTIFICATE ........................................................................................................2 STATEMENT OF COMPLIANCE .....................................................................................3 SIGNATURES
....

**~**............................................................................................................4 QUALITY ASSURANCE UNIT ........................................................................................5 CONTENTS ....................................................................................................................6 PREFACE .......................................................................................................................? DATA REQUIREMENT 

### ITEST GUIDELINES.................................................................8 SUMMARY OF STUDY PLAN AMENDMENTS...............................................................8 1 PURPOSE .............................................................................................................9 2 MATERIALS AND METHODS................................................................................9 2.1 TEST ITEM...................................................................................................9 2.2 PRINCIPLE OF THE TEST...........................................................................9 2.3 PERFORMANCE OFTHE TEST................................................................ 10 2.3.1 Apparatus......................................................................................10 2.3.2 Calibration ofthe Densitometer..................................................... 10 2.3.3 General Test Procedure ................................................................10 2.3.4 Repeatability .................................................................................10 2.4 DATA HANDLING.......................................................................................11 2.4.1 Definitions .....................................................................................11 2.4.2 Calculation ....................................................................................11 3 RESULTS ............................................................................................................12 Table 1: Results ofthe Calibration Using Air and Water........................................... 13 Table 2: Determination ofthe Density of DEAl Acid anhydride reaction product
........ 13RCC Study Number848617 DEA/Acid anhydride reaction product 

# PREFACE GENERAL Title: Sponsor:
Monitoring Scientist:

Test Facility:

RESPONSIBILITIES Study Director: Deputy Study Director:

.Technical Coordinator:

Head of RCC QualityAssurance:
SCHEDULE Experimental starting date: Experimental completion date: Studycompletion date:
ARCHIVING REPORT

Determination ofthe Densityof 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 ltingen/Switzerland

Mrs. Alessandra Tognucci Dr. Ute Schmiedel Mrs. Katalin Kiss Mrs. Iris Wuthrich

October 17, 2003 October31 , 2003 December 10, 2003

### I wih Page 7

RCC Ltd, CH-4452 ltingen/Switzerland will retain the study plan, raw data, a sample of test item andthe final report ofthe presentstudyfor at leastten years. No datawill be discarded withoutthe sponsor's consent.RCC Study Number848617 REPORT Page 8 DEAl Acid anhydride reaction product 

# DATA REQUIREMENT

# f.TEST GUIDELINES

This study followed the procedures indicated by the following internationally accepted guidelines and recommendations: EEC Directive 92/69, Methods for the determination of physico-chemical properties, A.3 "Relative density'', EEC Publication No. L383, December 1992. OECD Guideline for Testing of Chemicals, No. 109, "Density of Liquids and Solids", adopted July27, 1995.


# SUMMARY OF STUDY PLAN AMENDMENTS
First Amendment to Study Plan: 1) Concerning: Schedule Alteration: Anticipated experimental starting date Anticipated experimental completion date Anticipated date of draft report Reason for Alteration: Test item batch delivered later 2) Concerning: Test Item Alteration: New batch used for study New expiration date Reason for Alteration: New batch to be used by request of sponsorRCC Study Number848617 REPORT Page 10 DEAl Acid anhydride reaction product 

## 2.3 PERFORMANCE OF THE TEST 2.3.1 Apparatus Instrument: Oscillating densitometer, PAAR DMA-48. Conditions: The test was performed at 20°C

## ±0.1

# oc. 2.3.2 Calibration ofthe Densitometer The apparatus must be calibrated before use in case the last calibration was performed more than one week ago. This is done by determination of the resonance frequency (period time) of the tube when filled with water and with air, respectively. The calibration will normally be performed at 20.0°C ± 0.1

# oc. On the days of the present experiments, the calibration was checked by the measurement of air and water, resulting in the expected value for air of 0.001204 gtcm3 and for water of 0.9982 g/cms at 20.0°C. The accepted range is 0.9982 ± 0.0003 g/cm
. The print out is given in the raw data and details are later given in this report. 

### 2.3.3 General Test Procedure The test item was then injected into the U-tube by means of a disposable plastic syringe, avoiding air bubbles. The test item for the first test was filled in at 20°C. For better prevention of air bubble formation, the sample for the second test was filled in at about 30°C. The sample was then thermostated to 20.0°C in the apparatus. The density was read from the display after a constant oscillating frequency (constant period time) was reached. 

### 2.3.4 Repeatability Two tests with two measurements each were performed. The measurements did not vary by more than 0.0003 g/cm3 and were therefore accepted to be valid.RCC Study Number848617 REPORT Page 11 DEAl Acid anhydride reaction product 

## 2.4 DATA HANDLING 2.4.1 Definitions The density (p) of a substance is the quotient of the mass (m) and the volume (V) of that substance at a specific temperature. m 

### P=- V 

### Sl unit is in [kg/m3]. 

### 1 g/cm3 

### corresponds with 1000 kg/m3• (1)



### The relative density 

### Di 0 

### of solids or liquids is the ratio between the mass of a volume of substance to be examined, determined at 20°C, and the mass of the same volume of water, determined at 4°C. The relative density has no dimension. The mass of water, determined at 4°C, is 0.99997 g/cm3 (as published by the Physikalisch-Technische Bundesanstalt in Braunschweig, Germany, PTB-Mitt. 81 (1971), p. 412-415)


### Di 0 

# = pI0.99997 (2)


### 2.4.2 Calculation During this study the density (g/cm3) 

### was determined at 20.0°C. To calculate the relative density (no dimension), the factor 0.99997 of equation (2) was applied. As result, the relative densityDi0 

### is given.RCC Study Number 848617 DEA/Acid anhydride reaction product 

# 3 RESULTS REPORT Page 12

The determination of the density of the test item was performed in accordance with the EEC directive 92/69, Methods for the determination of physico-chemical properties, A.3 "Relative density'', EEC Publication No. L383, December 1992 and the OECD Guideline for Testing of Chemicals, No. 109, "Density of Liquids and Solids" using an oscillating densitometer. As the density of the test item was determined at 20.0°C, the relative density is stated. First, the apparatus was tested by determination of the density of air and water at 20.0°C. The results for water are given in Table 1. The measured values are in the accepted range of 0.9982 

### ±0.0003 g/cm3. Table 2 shows the individual measurements for the density of DEA/Acid anhydride reaction product. From these, the mean and the corrected values were calculated and given in the same table. The tabulated values represent rounded results obtained from calculation using the exact raw data. In conclusion, the relative density of the DEA/Acid anhydride reaction product was determined to be 

# Di 0

# = 1.2907RCC Study Number848617 REPORT Page 13 DEAl Acid anhydride reaction product Table 1: Results of the Calibration Using Air and Water The density of air was measured to be 0.001204 g/cm3•
Test No. Temperature Density [oC) [g/cm3] measured mean value theoretical value 1 20.0 0.9982 2 20.0 0.9982 0.9982 0.9982

Table 2: Determination of the Density of DEA/Acid anhydride reaction product

Test No. Temperature Density [oC] [g/cm3 ] measured mean value corrected (standard for relative deviation) density 1 20.0 1.2908 1 20.0 1.2906 1.2907 1.2907 2 20.0 1.2905 (0.0001) 2 20.0 1.2907

Calculation ofthe relative density 

### Di 0 

# =1.2907

### I 0.99997

# =1.2907