REPORT

DETERMINATION OF THE SURFACE TENSION OF AN AQUEOUS

SOLUTION OF TKA 40278 (CGI 827)

Data Requirement I Test Guidelines:

OECD Guideline No. 115

EEC Directive 92/69, A.5

Study Director:

Mrs. Alessandra Tognucci

Stud Corn letlon Date:

April 16, 2003

Test Facility:

RCC Ltd

Environmental Chemistry & Pharmanalytics

CH-4452 Itingen/Switzerland

CIBA SPECIALTY CHEMICALS INC.

CH - 4002 Basel/Switzerland

RCC Study Number:

845421

Page 1 of 16

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RCC Study Number 845421 REPORT Page 3

TKA 40278 (CG1827)

GOOD LABORATORY PRACTICE

STATEMENT OF COMPLIANCE

RCC Study Number:

Test Item:

Study Director:

Title:

845421

TKA 40278 (CGI 827)

Mrs. Alessandra Tognucci

Determination of the Surface Tension of an Aqueous

Solution of TKA 40278 (CGI 827)

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

26t~, 1997 by decision of the OECD Council [C(97)186/Final].

The purity of the test item is excluded from the statement of compliance (purity available in

Analytical Certificate No. 14026512-1; Ciba Specialty Chemicals Inc.).

Study Director: Mrs. Alessandra Tognucci

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RCO Study Number 845421 REPORT Page 4

TKA 40278 (CGt 827)

SIGNATURES

Study Director: nucci

Management: ,~Dr. JSrn Schreitmeller

Date:

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RCC Study Number 845421 REPORT Page 5

TKA 40278 (CG1827)

QUALITY ASSURANCE UNIT

RCC Ltd, Environmental Chemistry & Pharmanalytics, CH-4452 Itingen / Switzerland

STATEMENT

RCC Study Number:

Test Item:

Study Director:

Title:

845421

TKA 40278 (CGI 827)

Mrs. Alesssndra Tognucci

Determination of the Surface Tension of an Aqueous

Solution of TKA 40278 (CGI 827)

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

September 16, 2002 Study Plan September 16, 2002

November 19, 2002 Process based (Measurement) November 22, 2002

April 03, + 09, 2003 Final report April 09, 2003

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

Quality Assurance: Ut~ Mrs. M. Richter-Auer

Date:

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RCC Study Number 845421 REPORT Page 6

TKA 40278 (CG1827)

CERTIFICATION OF GLP

AND VERIFICATION OF THE REPORT

The statement of Compliance with Good Laboratory Practice found in this reporL and signed

by the Study Director is truthful and accurate, and this repor~ as provided by the testing

facility is complete and unaltered.

Signature of the Sponsor:

Date:

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RCC Study Number 845421 REPORT Page 7

TKA 40278 (CG1827)

CONTENTS

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

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

SIGNATURi=S ................................................................................................................ 4

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

CERTIFICATION OF GLP AND VERIFICATION OF THE REPORT .............................. 6

CONTENTS .................................................................................................................... 7

PREFACE ................................................................................................................... ~... 8

DATA REQUIREMENT I TEST GUIDELINES ................................................................ 9

SUMMARY OF STUDY PLAN AMENDMENTS .............................................................. 9

1 PURPOSE ........................................................................................................... 10

2 MATERIALS AND METHODS ............................................................................. 10

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

10

2.2 VALIDATION OF THE TENSIOMETER ......................... ~ ............................10

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

11

2.3.1 Principle ........................................................................................ 11

2.3.2 Test System .................................................................................. 11

2.3.3 Cleaning ........................................................................................ 11

2.3.4 Calibration of the Tensiometer ...................................................... 11

2.3.5 Preparation of the Test Solution .................................................... 11

2.3,6 Test Procedure .............................................................................

12

2.4 DATA HANDLING ...................................................................................... 13

3 RESULTS ............................................................................................................

14

Table 1: Determination of the Calibration Factor Using Water .................................. 15

Table 2: Determination of the Surface Tension of the Test Item Solution ................. 16

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RCC Study Number 845421 REPORT Page 8

TKA 40278 (CG1827)

PREFACE

GENERAL

Title:

Sponsor:

Monitoring Scientist:

Test Facility:

Determination of the Surface Tension of an Aqueous

Solution of TKA 40278 (CGI 827)

CIBA SPECIALTY CHEMICALS INC.

CH-4002 Basel/Switzerland

Dr. Moung Sook Lee

RCC Ltd

Environmental Chemistry & Pharmanalytics

Zeigliweg 1

CH-4452 Itingen/Switzerland

RESPONSIBILITIES

Study Director:

Deputy Study Director:

Technical Coordinator:

Head of RCC Quality Assurance:

Mrs. Alessandra Tognucci

Dr. Ute Schmiedel

Mrs. Katalin Kiss

Mrs. Iris Wethrich

SCHEDULE

Experimental starting date:

Experimental completion date:

Study completion date:

November 20, 2002

November 21, 2002

April 16, 2003/waj

ARCHIVING

RCC Ltd, CH-4452 Itingen/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.

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RCC Study Number 845421 REPORT Page 9

TKA 40278 (CG1827)

DATA REQUIREMENT / 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 !992.

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.

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RCC Study Number 845421 REPORT Page 10

TKA 40278 (OG1827)

1 PURPOSE

The purpose of the study was to evaluate the surface tension of TKA 40278 (CGI 827) in an

aqueous solution by means of a ring tensiometer.

The reduction in surface tension of water, by dissolving a substance in it, indicates whether

the substance is surface-active or not. Knowledge of this property is useful to assess the

environmental impact of a substance.

2 MATERIALS AND METHODS

2.1 TEST ITEM

Data as provided by the sponsor..

Identity:

Product Name:

Batch:

Purity:

Appearance:

Expiration date:

Storage:

TKA 40278

CGI 827

KL 01/02

See Analytical Certificate, Study No. 14026512-1

Ciba Specialty Chemicals Inc.

Solid, slightly yellow

August 30, 2004

At room temperature at about 20 °C.

The test item is light sensitive.

2.2 VALIDATION OF THE TENSlOMETER

The measurement as described below is validated twice every year:

The surface tension of n-hexane was determined using the identical test procedure and

conditions as for the aqueous solution of the test item. These data are part of RCC’s

instrument files. The last validation was performed on October 23, 2002. The results found

were in accordance with the criteria in the directive and therefore, the test method was

accepted.

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RCC Study Number 845421

TKA 40278 (CGI 827)

REPORT Page 11

2.3 PERFORMANCE OF THE TEST

2.3.1 Principle

The determination of the surface tension was accomplished by means of a tensiometer,

using the ring method. 1he 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.

o

" a All measurements were made at 20.3 C w~th maximum deviation of :1:0.1 °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 water, briefly immersed in chromo-sulphuric

acid, washed with double distilled 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. These data are

part of RCC’s instrument files. The calibration factor ~b, by which all the instrument readings

were multiplied, was determined in accordance with the equation:

where

the surface tension of water at the test temperature.

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 208.4 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 15 minutes and then stirred for 23 hours. After

filtration, the solution was diluted with 1 part of double distilled water per 9 parts (v/v) of

saturated test item solution.

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RCC Study Number 845421 REPORT Page 12

TKA 40278 (CG1827)

2.3.6 Test Procedure

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 away 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.

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TKA 40278 (CG1827)

2.4 DATA HANDLING

The surface tension is given in mN/m ($1 sub-unit).

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

the calibration factor ~b. This yields a value which is only approximate and requires additional

correction. The additional correction was made using the factor for correction Fc derived from

the table below compiled on the basis of Harkins-Jordan correction (W. D. Harkins, H. F.

Jordan, J. Amer. Chem. 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

IroN/m] Fc [mN/m] Fc

2O 18.1 0.905 5O 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

3O 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 O.95O 68 67.7 0.996

4O 38.2 0.955 70 69.9 0,999

42 40.3 0.960 72 72.0 1.000

42.3 0.961 74

46 44.4 0,965 76

48 46.5 0,969 78

* with F¢ = Corrected Value / 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.

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TKA 40278 (CG1827)

3 RESULTS

The determination of the surface tension of an aqueous solution of TKA 40278 (CGI 827)

was based on the OECD Guideline No. 115: "Surface Tension of Aqueous Solutions" (1995)

and on the EEC Directive 92169, Part A, Methods for the determination of physico-chemical

properties, A.5 "Surface tension", EEC Publication No. L383, December 1992.

The calibration factor ~b was determined to be 1.0033 for double distilled water (Table 1). The

data are part of RCC’s instruments’ files and a copy is given 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 given in the same table. The tabulated values represent rounded results obtained from

calculation using the exact raw data.

In conclusion, the surface tension of TKA 40278 (CGI 827) in water (90 % of saturation

concentration) was determined to be

67.3 mN/m at 20.3 °C "*- 0.1 °C.

Based on the criteria as outlined in the EEC Guideline, TKA 40278 (CGI 827) is not a surface

active substance.

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TKA 40278 (CG1827)

Table 1: Determination of the Calibration Factor Using Water

Time expired Temperature Surface tension Calibration

[hours:mini [°C] [mN/m] factor

measured mean value

calculated from

the bold values

00:01 20.2 72.5

00:02 20.3 72.5

00:03 20.3 72.5

00:04 20.3 72.5 72.5 1.0033

with

~o = 72.7406mN/mat 20.3 °C

Cb = 72.7406 / 72.5 = 1.0033

where

~b = calibration factor

(~o = the surface tension of water at the test temperature.

% = measurement value of the surface tension of the water

at the test temperature.

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RCC Study Number 845421 REPORT Page 16 TKA 40278 (CG1827)

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

Time expired Temperature Surface tension

[hours:min] [°C] [mN/m]

measured mean value corrected for

calculated from calibration and

the bold values for HarkinsJordan

First sample

00:3"i 20.2 67.0

00:32 20.2 67.’1

00:33 20.3 67.3

00:34 20.3 67.3

00:35 20.3 67.3

Second sample

00:36 20.3 67,6

00:37 20.4 67.6

00:38 20.4 67.5

00:39 20.4 67.4

00:40 20.4 67.6 67.34 67.29

with

G* ’~b" = ~ (67.34  ̄ 1.0033=67.56)

~b = calibration factor = 1.0033

and

m’ Fc = ~ (67.56 . 0.996=67.29)

Fc = factor for correction acc. to Harkins-Jordan = 0.996 for 68 mN/m

181