REPORT 

Study Title: 

DETERMINATION OF THE SURFACE TENSION OF AN AQUEOUS 

SOLUTION OF DEAl Acid anhydride reaction product 

Data Requirement I Test Guidelines: 

OECD Guideline No. 115 

EEC Directive 92/69, A.5 

Study Director: 

Mrs. Alessandra Tognucci 

Study Completion Date: 

September 23, 2003 

Test Facility: 

RCC Ltd 

Environmental Chemistry & Pharmanalytics 

CH-4452 ltingen/Switzerland 

Sponsor: 

Rockwoollnternational AJS 

Hovedgaden 584 

DK-2640 Hedehusene 

Denmark 

RCC Study Number: 

848618 

Page1of15 
RCC Study Number 848618 

DEA/Acid anhydride reaction product 

GLP CERTIFICATE 

REPORT 

The Swiss GLP Monitoring Authorities 

Swiss Federal 

Office of 

Public Health 

Swiss Agency for the 

Environment. Forests 

and Landscape 

./ Swlssmedic 

~ d" SwissAgencyfor SWlssme JC TherapouucProducts 

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 for 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. 

Bem, March 2003 

Federal Office of Public Health 

The Director 

Prof. Th. Zeltner 

• TOX =Toxicology ; ACC = Analytical and Clinical Chemlst:y ; ECT = Environmental toxicity on aquatic and terrestrtal organisms: ENF =Behaviour In water, soli and air. BioaccumulaUon; EMN ::Studies on effects on mesocosms and natural ecosystems: MUT =Mutagenicity; PCT = Physical-chemlc:a.J testing; RES= Residue studies: OTH = Oth~r, to be spedfied. 

Page 2 
RCC 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 of the Surface Tension 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 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 

261

", 1997 by decision of the OECD Council [C(97)186/Final]. 

Study Director: Mrs. Alessandra Tognucci 
RCC Study Number 848618 REPORT Page 4 DEN Acid anhydride reaction product 

SIGNATURES 

Study Director: 

Management: Dr. Jorn SchreitmOIIer 

... !giJ~~:mr... ....................................... . Dbj~: ~k J-3, ,JCOJ 
RCC Study Number 848618 

DEA/Acid anhydride reaction product 

REPORT 

QUALITY ASSURANCE 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. Alessandra Tognucci 

Page 5 

Title: Determination of the Surface Tension 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 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 OAU Inspections Dates of Reports to the Study 

Director and to the Management 

June 06, 2003 Study Plan June 06, 2003 

July 16, 2003 Sample preparation July 16, 2003 

September 11 , 2003 Final report September 11 , 2003 

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

Quality Assurance: fc. Mrs. Diana Burgin 

Date: 
RCC Study Number 848618 REPORT Page6 

DEN Acid anhydride reaction product 

CONTENTS 

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 MATERIALS AND METHODS ................................................................................ 9 

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

2.2 VALIDATION OF THE TENSIOMETER ........................................................ 9 

2.3 PERFORMANCE OF THE TEST ................................................................ 10 

2.3.1 Principle ........................................................................................ 10 

2.3.2 Test System .................................................................................. 10 

2.3.3 Cleaning ........................................................................................ 10 

2.3.4 Calibration of the Tensiometer ...................................................... 10 

2.3.5 Preparation of the Test Solution .................................................... 10 

2.3.6 Test Procedure .............................................................................. 11 

2.4 DATA HANDLING ....................................................................................... 12 

3 RESULTS ............................................................................................................ 13 

Table 1: Determination of the Calibration Factor Using Water. ...................................... 14 

Table 2: Determination of Surface Tension for the Test Item Solution .......................... 15 
RCC Study Number 848618 

DEA/Acid anhydride reaction product 

PREFACE 

GENERAL 

Title: 

Sponsor: 

Monitoring Scientist: 

Test Facility: 

RESPONSIBILITIES 

Study Director: 

Deputy Study Director: 

Technical Coordinator: 

Head of RCC Quality Assurance: 

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 I ntemational A/S 

Hovedgaden 584 

DK-2640 Hedehusene 

Denmark 

Mr. Flemming A. Simonsen 

Danish Toxicology Centre 

KogleAIIe 2 

Dk-2970 H0RSHOLM 

Denmark 

RCC Ltd 

Environmental Chemistry & Pharmanalytics 

Zelgliweg 1 

CH-4452 ltingen/Switzerland 

Mrs. Alessandra Tognucci 

Mr. Michael Lindemann 

Mrs. B. Flukiger 

Mrs. Iris Wuthrich 

August18, 2003 

August 19, 2003 

September 23, 2003 I WIH 

RCC Ltd, CH-4452 ltingen/Switzerland 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 discarded without the sponsor's consent. 
RCC Study Number 848618 REPORT PageS DEN 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.5 "Surface tension", EEC Publication No. L383, December 1992. 

OECD Guideline for Testing of Chemicals No. 115, "Surface Tension of Aqueous 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 of the 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 of 9.545 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 a flame. 

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 of the Tensiometer 

The apparatus was calibrated using double distilled water from 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 

cr0 = the surface tension of water at the test temperature. 

cr9 = measurement value of the surface tension of the water 

at the test temperature. 

2.3.5 Preparation of the 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 of double 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'flaY from 

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 of the test item solution. 
RCC Study Number 848618 REPORT Page 12 DEAl Acid anhydride reaction product 

2.4 DATA HANDLING 

The surface tension is given in mN/m (SI sub-unit). 

In order to calculate the surface tension, the values read on the apparatus were multiplied by 

the calibration factor <Pb. This yields a value which is only approximate and requires addiiional 

correction. The additional correction was made using the factor for 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 Factor for Experimental Corrected Factor for 

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 Number 848618 

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 of Aqueous 

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 for the surface tension of the aqueous test item 

solution. From these, the mean and the corrected value for the 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 Number 848618 

DEA/Acid anhydride reaction product 

REPORT 

Table 1: Determination of the Calibration Factor Using Water 

Surface tension 

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 of water at the test temperature. 

measurement value of the surface tension of water 

at the test temperature. 

Page 14 
RCC Study Number 848618 REPORT Page 15 DEN Acid anhydride reaction product 

Table 2: Determination of Surface Tension for the Test Item Solution 

Time expired Temperature Surface tension 

[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) 

First sample 

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 = factor for correction ace. to Harkins-Jordan 

= 0.983 for 57.31 mN/m and 0.985 for 58.63 mN/m.