# REPORT
StudyTitle: 

### DETERMINATION OFTHE SURFACETENSION OFAN AQUEOUS SOLUTION OF DEAl Acid anhydride reaction product
Data RequirementITest Guidelines: OECD Guideline No. 115 EEC Directive 92/69, A.5 Study Director: Mrs. AlessandraTognucci StudyCompletion Date: September23, 2003 Test Facility: RCC Ltd Environmental Chemistry & Pharmanalytics CH-4452 ltingen/Switzerland Sponsor: RockwoollnternationalAJS Hovedgaden 584 DK-2640 Hedehusene Denmark RCC StudyNumber: 848618 Page1of15RCC Study Number848618 DEA/Acid anhydride reaction product 

# GLP CERTIFICATE REPORT

The Swiss GLP Monitoring Authorities
Swiss Federal Office of Public Health SwissAgencyforthe Environment. Forests and Landscape ./ Swlssmedic

**~** 

## d" SwissAgencyfor 

### SWlssme JC TherapouucProducts 

# Statement of GLP Compliance

It is hereby confirmed that during the period of thefollowingTest 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 forthe 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 timethey were inspected.

Bem, March 2003 Federal Office of Public Health The Director

Prof. Th. Zeltner

•TOX =Toxicology ;ACC

### = Analyticaland Clinical Chemlst:y ;ECT

### = Environmental toxicityon aquatic and terrestrtal organisms: ENF=BehaviourInwater, soli and air. BioaccumulaUon; EMN ::Studies on effects onmesocosms and natural ecosystems: MUT=Mutagenicity; PCT

### = Physical-chemlc:a.J testing; RES=Residue studies: OTH=

**Oth~r,**tobe spedfied. Page 2RCC Study Number 848618 DEA/Acid anhydride reaction product 

### GOOD LABORATORY PRACTICE REPORT Page3



# STATEMENT OF COMPLIANCE

RCC Study Number: Test Item: Study Director: Title: 848618 DEA/Acid anhydride reaction product Mrs. Alessandra Tognucci Determination ofthe SurfaceTension of an Aqueous Solution of DEA/Acid anhydride reaction product This study was conducted in compliance with the Swiss Ordinance relating to Good Laboratory Practice, adopted February2nd, 2000 [RS 813.016.5]. This Ordinance is based on the OECD Principles of Good Laboratory Practice, as revised in 1997and adopted November 261", 

### 1997 bydecision ofthe OECD Council [C(97)186/Final].

Study Director: Mrs. Alessandra TognucciRCC Study Number848618 REPORT Page 4 DEN Acid anhydride reaction product 

# SIGNATURES

Study Director:

Management: Dr. 

### Jorn SchreitmOIIer



# ...
**!giJ~~:mr...**

# ........................................

**Dbj~: ~k**  

# J-3, ,JCOJRCC Study Number848618 DEA/Acid anhydride reaction product REPORT 

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

### I Switzerland STATEMENT RCC Study Number: 848618 Test Item: DEAl Acid anhydride reaction product Study Director: Mrs. AlessandraTognucci Page 5

Title: Determination ofthe SurfaceTension of an Aqueous Solution of DEAl Acid anhydride reaction product The general facilities and activities are inspected periodically and the results are reported to the responsible person andthe management. Study procedures were periodically inspected. The study plan and this reportwere audited by the QualityAssurance Unit. The dates are given below: · Dates and Types of OAU Inspections Dates of Reports to the Study Director and to the Management June 06, 2003 Study Plan June06, 2003 July 16, 2003 Sample preparation July 16, 2003 September 11 ,2003 Final report September 11 , 2003 This statement also confirms thatthisfinal report reflects the raw data. QualityAssurance: 

# fc. Mrs. Diana Burgin

Date:RCC Study Number 848618 REPORT Page6 DEN Acid anhydride reaction product 

# CONTENTS

GLP CERTIFICATE ........................................................................................................2 STATEMENTOF COMPLIANCE....................................................................................3. SIGNATURES.................................................................................................................4 QUALITYASSURANCE UNIT ........................................................................................5 CONTENTS ....................................................................................................................6 PREFACE.......................................................................................................................7 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 VALIDATION OF THETENSIOMETER........................................................9 2.3 PERFORMANCE OF THETEST................................................................ 10 2.3.1 Principle ........................................................................................10 2.3.2 Test System ..................................................................................10 2.3.3 Cleaning ........................................................................................ 10 2.3.4 Calibration ofthe Tensiometer ...................................................... 10 2.3.5 Preparation ofthe Test Solution.................................................... 10 2.3.6 Test Procedure.............................................................................. 11 2.4 DATA HANDLING....................................................................................... 12 3 RESULTS ............................................................................................................13 Table 1: Determination ofthe Calibration Factor Using Water....................................... 14 Table 2: Determination ofSurface Tension forthe Test Item Solution .......................... 15RCC Study Number848618 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: Study completion date:
ARCHIVING REPORT Page 7

Determination of the Surface Tension of an Aqueous Solution of DEA/Acid anhydride reaction product Rockwool Intemational A/S Hovedgaden 584 DK-2640 Hedehusene Denmark
Mr. FlemmingA. Simonsen Danish Toxicology Centre KogleAIIe 2 Dk-2970 H0RSHOLM Denmark RCC Ltd Environmental Chemistry& Pharmanalytics Zelgliweg 1 CH-4452 ltingen/Switzerland

Mrs. AlessandraTognucci Mr. Michael Lindemann Mrs. B. Flukiger Mrs. Iris Wuthrich

August18, 2003 August 19, 2003 September23, 2003

### IWIH

RCC Ltd, CH-4452 ltingen/Switzerland will retain the study plan, raw data, a sample of test item andthefinal report ofthe present studyforat leastten years. No datawill be discarded withoutthe sponsor's consent.RCC Study Number 848618 REPORT PageS DEN Acid anhydride reaction product 

# DATA REQUIREMENT 

# ITEST 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.5 "Surface tension", EEC Publication No. L383, December 1992. OECD Guideline for Testing of Chemicals No. 115, "Surface Tension ofAqueous Solutions", adopted July 27, 1995.


# SUMMARY OF STUDY PLAN AMENDMENTS

There were no amendments to the study plan.RCC Study Number 848618 DEA/Acid anhydride reaction product REPORT 

# 2.3 PERFORMANCEOFTHETEST 2.3.1 Principle Page 10



### The determination of the surface tension was accomplished by means of a tensiometer, using the ring method. The force which was required to withdraw a horizontally suspended ring from the surface ofthe solution is measured. 

### 2.3.2 Test System The experiment was performed using a tensiometer Model K8, KROSS GmbH, Hamburg, Germany. The measuring body was a platinum-iridium ring with a wire radius of 0.185 mm and a ring radius of9.545 mm. All measurements were made at 20oc with a maximum deviation of±0.5°C. 

### 2.3.3 Cleaning The measurement vessel was washed with chromo-sulphuric acid and subsequently with syrupy phosphoric acid. Thereafter, the vessel was thoroughly washed with water and with acetone. Finally, the vessel was briefly heated above aflame. The measuring ring was rinsed thoroughly with double distilled water, briefly immersed in chromo-sulphuric acid, washed with water and acetone and finally briefly heated above a flame. 

### 2.3.4 Calibration ofthe Tensiometer The apparatus was calibrated using double distilled waterfrom RCC supply. Th.ese data are part of RCC's instrument files. The calibration factor <Pb, 

### by which all the instrument readings were multiplied, was determined in accordance with the equation:
where cr

0 = 

### the surface tension ofwater at the testtemperature. cr9 = 

### measurement value ofthe surface tension ofthe water atthe testtemperature. 

### 2.3.5 Preparation ofthe Test Solution An aqueous solution of the test item was prepared by weighing 201.7 mg of test item in a 200 ml flask and filled up to the mark with double distilled water from RCC supply. This mixture was submitted to ultrasonification for 5 minutes and then stirred for about 18 hours. After filtration, the solution was diluted with 1 part ofdouble distilled water per 9 parts (v/v) of saturated test item solution.RCC Study Number 848618 DENAcid anhydride reaction product 

### 2.3.6 Test Procedure REPORT Page 11



### The cleaned measurement vessel was filled with the test solution and placed onto the mobile sample table. The table was raised until the ring was immersed below the surface of the solution. Subsequently, the table was lowered until the ring was attached to the liquid surface. After additional lowering of the table, the ring exerted a torque on the force measuring system. Lowering of the table and subsequent compensation of the resulting torque were continued in small increments until the lamina was broken. This occurred when upward force completely overcame the surface tension force and the ring was torn 

### a'flaYfrom the surface. The surface tension was then recorded. Afterwards, the ring was immersed below the surface again and the measurement was repeated. Since the surface tension of a solution in the measurement vessel alters over a period of time, several measurements were made until a constant value was obtained. The time expired, from when the solution was transferred to the measurement vessel, was recorded for each determination. The measurement was done in duplicate using a second aliquot ofthe test item solution.RCC Study Number848618 REPORT Page 12 DEAlAcid anhydride reaction product 

## 2.4 DATA HANDLING The surface tension is given in mN/m (SI sub-unit). In orderto calculate the surface tension, the values read on the apparatus were multiplied by the calibration factor 

### <Pb. This yields avalue which is only approximate and requires addiiional correction. The additional correction was made using the factorfor correction 

### Fe derived from the table below compiled on the basis of Harkins-Jordan correction (W. D. Harkins, H. F. Jordan, J. Amer. Chern. Soc. 52, 1751, 1930). '

* Experimental Corrected Factorfor Experimental Corrected Factorfor Value Value Correction* Value Value Correction* [mN/m] (Water Calibration) [mN/m] (Water Calibration) [mN/m] 

### Fe [mN/m] 

### Fe 20 18.1 0.905 50 48.6 0.972 22 20.1 0.914 52 50.7 0.975 24 22.1 0.921 54 52.8 0.978 26 24.1 0.927 56 54.9 0.980 28 26.1 0.932 58 57.0 0.983 30 28.1 0.937 60 59.1 0.985 32 30.1 0.941 62 61.3 0.989 34 32.1 0.944 64 63.4 0.991 36 34.1 0.947 66 65.5 0.992 38 36.1 0.950 68 67.7 0.996 40 38.2 0.955 70 69.9 0.999 42 40.3 0.960 72 72.0 1.000 44 42.3 0.961 74


## - 46 44.4 0.965 76


## - 48 46.5 0.969 78


## - with 

### Fe = Corrected Value 

### I Experimental Value, calculated from the data given in the OECD Guideline 115 (as given in the columns 1 and 2 and 4 and 5, respectively).
According to the criteria as mentioned in the directive, substances showing a surface tension lower than 60 mN/m under the conditions of this method, should be regarded as being surface active material.RCC Study Number848618 DEA/Acid anhydride reaction product 

# 3 RESULTS REPORT Page 13



### The determination of the surface tension of an aqueous solution of DENAcid anhydride reaction product was based on the OECD Guideline No. 115: "Surface Tension ofAqueous Solutions" (1995) and on the EEC Directive 92/69, Part A, Methods for the determination of physico-chemical properties, A.5 "Surface tension", EEC Publication No. L383, December 1992. The calibration factor <l>b 

### was determined to be 1.0240 for double distilled water (Table 1 ). The data are part of RCC's instruments' files and a copy is presented in the raw data of the present study. Table 2 shows the individual measurements forthe surface tension ofthe aqueous test item solution. From these, the mean and the corrected value forthe given solution were calculated and shown in the same table. The tabulated values represent rounded results obtained from calculation using the exact raw data. In conclusion, the surface tension of DENAcid anhydride reaction product in water (90 % 

### of saturation concentration) was determined to be 58.0 mN/m 

### at 20.1

# oc ± 0.1

# oc. Based on the criteria as outlined in the EEC Guideline, DEA/Acid anhydride reaction product is a surface active substance.RCC Study Number848618 DEA/Acid anhydride reaction product REPORT
Table 1: Determination ofthe Calibration Factor Using Water
Surfacetension Time expired Temperature [mN/m] mean value (hours:min] 

### ('C] measured calculated from the bold

values cr9 00:28 20.3 71.1 00:30 20.3 71.1 00:31 20.3 71.0 70.98 00:32 20.4 71.0 00:34 20.5 70.9 00:35 20.5 70.8
with
O"o 

### = 72.69 mN/m at 20.4'C <l>b 

### = <l>b 

### = 72.69 

### I 70.98 = 1.0240 where

= calibration factor Calibration factor

<l>b

1.0240

= 

### = the surface tension ofwaterat the testtemperature. measurementvalue ofthe surfacetension ofwater at the testtemperature. Page 14RCC Study Number848618 REPORT Page 15 DEN Acid anhydride reaction product Table 2: Determination ofSurface Tension forthe Test Item Solution
Time expired Temperature Surfacetension

[hours:min] 

### [OC] [mN/m]
mean value mean value cr1

**correct~d** for calculated from corrected for Harkins-Jordan measured the bold values calibration (cr*) (cr,) (cr) Firstsample 00:29 19.8 57.5 00:31 20.0 56.8 00:32 20.0 56.8 56.92 58.29 57.31 00:33 20.0 56.8 00:34 20.0 56.8 00:36 20.0 56.8

Second sample 00:31 20.2 58.4 00.33 20.2 58.3 00.34 20.2 58.3 58.15 59.55 58.63 00.35 20.2 58.1 00.36 20.2 57.9 00.38 20.2 57.9

Mean value from both samples: cr 

### = 58.0 mN/m with cr* · <l>b 

### = cr1 <l>b 

### = calibration factor 

### = 1.0240 and
cr1 · 

### Fe= cr 

### Fe = factorforcorrection ace. to Harkins-Jordan = 0.983 for57.31 mN/m and 0.985 for58.63 mN/m.