Document EqjK61O7b3MQ2KBEEQoBYvb2n

RECEIVED A fu a - /s Telomer Research Program 1200 South Hayes Street Arlington, Virginia 22202-5050 Tet (703)413-1100 45264 Fac (703)4136111 Clariant February 14, 2003 Mary F. Dominiak U.S. Environmental Protection Agency EPA East (Mail Code 7405M) 1200 Pennsylvania Avenue NW Washington, DC 20460 E-mail: dominiak.mary@epa.gov Dear Mary: yo o cn ro The Telomer Research Program (TRP) and its member companies, Asahi Glass, Clariant, Daikin, and DuPont, are providing to U.S. EPA Docket# AR226 final reports on the acute hazard of 8-2 Telomer B Alcohol (3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluorodecan-1-ol; CAS No. 678-39-7) when tested with standard freshwater aquatic test species. These reports present the results of the acute aquatic toxicity testing conducted by an independent laboratory at the request of the TRP. These studies were conducted according to existing OECD test guidelines and in accordance with the provisions of the appropriate Good Laboratory Practices (GLP) regulations. The physical-chemical characteristics of the test substance indicate that the test substance is a "difficult" substance, as indicated in OECD Monograph 23 (Guidance Document on Aquatic Toxicity Testing of Difficult Substances and Mixtures, OECD 2000), and the experimental designs selected for the acute aquatic toxicity testing were reflective of this observation. Common practices for testing these types of materials, and for evaluating the results from tests of these types of materials, were used during the conduct of the studies and the preparation of the study reports. The TRP and its member companies believe that the data gathered from these studies are consistent with the hypothesis that the 8-2 Telomer B Alcohol is of low to medium concern in terms of its potential for causing acute effects on aquatic species. If there are questions concerning the technical aspects of the studies submitted, please contact me so that I may direct your questions to the appropriate TRP member company personnel. Sincerely, Katie D. Smythe TRP Administrator This docum ent does not contain TSC A CBI. 000003 Dr.U.Noack-Laboratorium fr Angewandte Biologie 1-Decanoi, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro- Acute Immobilisation Test (48 h) to Daphnia magna STRAUS, Limit Test with the Saturated Solution acc. to OECD-Guideline 202 I for Testing of Chemicals (adopted April 04, 1984) Sponsor Telomer Research Project Asahi Glass Atofina Clariant Daikin Industries Ltd Dupont Author Martina Noack Test Facility D r .U.No a c k -Laborato rium FR ANGEWANDTE BIOLOGIE Kthe-Paulus-Str. 1 D-31157 Sarstedt Laboratory Project ID Project-No. Study-No. 020109CK DAI84111 Study Completed On August 07, 2002 Page 1 of 31 Original 7 of 7 000004 Dr.U.Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 2 of 31 Project-No. 020109CK Study-No. DAI84111 Statement of GLP Compliance Title Guideline Test Item Test Facility Deviations from GLP Principles 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS, Limit test with the Saturated Solution OECD 202 I for testing of chemicals (adopted April 04,1984) 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro(Batch No: P00/001) D r .U.No a c k -Lab o r a t o r iu m f r a n g e w a n d t e B iologie Kthe-Paulus-Str.1, D-31157 Sarstedt Phone: (+49) 050 66/706 70, Fax: (+49) 05066/706 789 E-mail: lnfo@ noack-lab.de None We declare that this study was conducted and reported in compliance with the actual OECD principles of Good Laboratory Practice and the national GLP regulations as specified In the law in force, except deviations mentioned above. August 07, 2002 M l . fu.ot<JUv (Martina Noack, Study Director) August 07, 2002 (Thomas Geffke, Scientist) August 07, 2002 (Dr. Udo Noack, Head of Testing Facility) ooooos Dr.U.Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8.8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 3 of 31 Project-No. 020109CK Study-No. DAI84111 Statement of the Quality Assurance Unit Title Guideline Test Item Study Director 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS, Limit test with the Saturated Solution OECD 202 I for testing of chemicals (adopted April 04,1984) 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro(Batch No: P00/001) Martina Noack The study was verified as follows: inspection study plan process based report dates 2002-03-12 2002-04-03 2002-04-05 2002-04-09 2002-04-10 2002-04-11 2002-04-12 2002-08-07 date of report 2002-03-12 2002-04-03 2002-04-05 2002-04-09 2002-04-10 2002-04-11 2002-04-12 2002-08-07 The reported results accurately and completely reflect the raw data of the study. Also methods, procedures, and observations are accurately and completely described in the report. The accordance of the study with its study plan and the principles of Good Laboratory Practice is guaranteed. August 07, 2002 000006 Dr.U.Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 4 of 31 Project-No. 020109CK Study-No. DAI84111 Personnel Involved Study Director: Scientist: (Analytical part) Martina Noack (Biologist) Thomas Geffke (Chemical Engineer) Technical Staff: Anke Gehlert Gwendolin Kraetzig Quality Assurance Unit: Director of the Test Facility: Gudrun Mohrmann-Kalabokidis (Biologist) Susanne Becker (Biologist) Dr. Udo Noack (Biologist) 000007 Dr.u .Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 5 of 31 Project-No. 020109CK Study-No. DAI84111 Table of Content Title Page Statement of GLP Compliance Statement of Quality Assurance Unit Personnel Involved Table of Content List of Tables 1 2 3 4 4.1 4.2 4.3 4.4 5 6 7 8 8.1 8.2 8.2.1 8.2.2 8.2.3 8.2.4 8.2.5 8.3 8.4 8.5 9 10 Summary Characterisation Data of the Test Item Method Results Solubility of the test item Results of the definitive test Results of the reference item Water parameters Validity criteria Literature / References Physicochemical data: pH-values, dissolved oxygen GC - Analysis of 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9, 10,10,10heptadecafluoroMethod Method Validation Linearity Quantification Limit and Detection Limit Precision (Repeatability) Peak Symmetry Accuracy Results Calibration Curves Chromatograms Certificate of 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10heptadecafluoro- Analysis GLP-Certificate of Dr .u .Noack-Laboratorium Page 1 2 3 4 5 5 7 8 9 15 15 15 15 15 16 16 17 18 18 20 20 20 21 21 22 23 24 27 30 31 000008 Dr.U.Noack-Laboratorium for Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 6 of 31 Project-No. 020109CK Study-No. DAI84111 List of Tables Tables Page Table 1: Percentage number of daphnids incapable of swimming after 24 and 48 h of exposure 7 Table 2: W ater parameters at the beginning of the test 17 Table 3; W ater parameters at the end of test (48 h) 17 Table 4: W ater parameters of the dilution water 17 Table 5: Repeatability of Injections of Test Item 21 Table 6: Mean Recovery Rate of Fortified Samples 22 Table 7: Concentrations of the Active Ingredient 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10, 10,10-heptadecafluoro 23 List of Figures Figures Fig. 1: Fig. 2. Fig. 3: Fig. 4: Fig. 5: Fig. 6: Calibration Curve of Standard - concentration range 0.01 - 0.06 mg/L Calibration Curve of Standard - concentration range 0 .1 -1 0 mg/L Calibration Curve of Standard - concentration range 0.1 - 0.6 mg/L Chromatogram of Standard Chromatogram of Test Item Chromatogram of Control 24 25 25 27 28 29 000009 Dr.U.Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 7 of 31 Project-No. 020109CK Study-No. DAI84111 1 Summary In the acute immobilisation test with Daphnia magna (STRAUS) the effect of the saturated solution as limit concentration of the test item 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro- (Batch number P00/001), was determined according to OECD Guideline 202 I. The limit test was conducted from 2002-04-03 to 2002-04-05 at D r .U .N o a c k -La b o r a t o r iu m f r a n g e w a n d t e B io lo g ie D-31157 Sarstedt. A coating period of 14 days was carried out. The preparation method was chosen with regard to the test item properties and in accordance with the relevant guidance documents (OECD 2000, BAUA 2001). The study was conducted under static conditions over a duration of 48 hours. 20 test organisms were exposed to the saturation concentration and control. The saturation concentration was analytically verified by GC-analysis (for details see part 8). The mean measured concentration of the saturation concentration was 0.16 mg/L. In the tested saturation concentration of 0.16 mg/L (mean measured concentration) no biologically significant effect was determined. Table 1: Percentage number of daphnids incapable of swimming after 24 and 48 h of exposure (n = 20) Saturation concentration [mg/L] 0.16 Control 1. 0 0 IMMOBILISATION [%] 24 h Replicates 2. 3. 4. MV 1. 000 00 000 00 MV Mean value 48 h Replicates 2. 3. 4. 000 000 MV 0 0 A reference test is carried out once per month with potassium dichromate as reference item and the reference toxicity determined. The ECso-value of the reference item at 2.1 mg/L after 24 h was within the prescribed concentration range of 1.0 to 2.5 mg/L according to AQS, DIN Guideline 38412 L 30. Water quality parameters of pH-value and dissolved oxygen concentration measured at 0 and 48 h were determined to be within the acceptable limits. The validity criteria of the test guideline were fulfilled. * Saturation concentration: The maximum dissolved concentration of the test item that can be achieved under the test conditions in the test medium, acc. to O EC D Series, No. 23 (2000)6. OOOOIO Dr.U.Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro- Acute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 8 of 31 Project-No. 020109CK Study-No. DAI84111 2 Characterisation Data of the Test Item TEST ITEM 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10heptadecafluoro- Batch Number P00/001 CAS RN 678-39-7 Chemical characterization Purity Appearance Water solubility 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluorodecane-1-ol (EINECS) C8-perfluoroalkylethanol: 99.3 % (a/a), sum perftuoroalkylethanol 99.9 % (a/a) Yellowish solid wax 134 pg/L at 12 degree C, Std 29 pg/L, n=8 (DuPont, 2002) 137 pg/L at 25 degree C, Std 53 pg/L, n=17 (DuPont, 2002) Stability in water Stable at test conditions Density Ca. 1.7 g/cm3 Expiry date Recommended storage Storage at testing facility Retention Identification parameter at testing facility Unlimited if stored under the recommended conditions. Room temperature (20 C), protected from moisture. Room temperature, protected from moisture and light. At least 1 g has been retained. Name, batch number and colour. The test item and the information concerning the test item were provided by the sponsor. O O O O ll Dr.U.Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 9 of 31 Project-No. 020109CK Study-No. DAI84111 3 Method GUIDELINE TYPE AND PURPOSE TEST SYSTEM Reason for the selection of test system Origin Breeder Culture Culture medium Feeding OECD-Guideline for Testing of Chemicals No. 202 1 "Acute Immobilisation Test of Daphnia magna STRAUS" adopted April 04,1984. Determination of the acute toxicity of 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroto Daphnia magna STRAUS in a limit test with the saturated solution. Daphnia magna STRAUS (Clone 5) Daphnia magna STRAUS belongs, in accordance with the study guideline, to the suitable Daphnia types and are bred in the test facility. Institut fr Wasser-, Boden- und Lufthygiene des Bundes gesundheitsamtes, Corrensplatz, 14195 Berlin, FRG D r .U .N o a c k -La b o r a t o r iu m , 31157 Sarstedt, FRG ln 2-3 L glass vessels with approximatively 1.8 L culture medium (Elendt M4), at 21 C (temperatures of 20-25 "C are tolerated), in an incubator, 16 h illumination, illumination strength max. 20 uE/m2/s (corresponding to 1200 lux). Brood daphnids were maintained in 100 % dilution water at the test temperature for at least 48 h prior to the test. Elendt M4, according to Elendt (1990), modified to a total hardness of 160 to 180 mg CaCCVL. 5x weekly ad libitum with a mix of Scenedesmus subspicatus and Chlorella vulgaris, with an algae cell density of > 108 cells/mL. 000012 __________________ Dr. .Noack-Laboratorium fr Angewandte Biologie__________________ Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafIuoro- Acute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 10 of 31 Project-No. 020109CK Study-No. DAI84111 TEST ITEM Pretreatment of 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroThe test item was heated to 50 C before weighing for homogenisation. TEST CONDITIONS Coating of the Test vessels Preparation A coating phase of 14 days was carried out. 200 mg 1-Decanol, 3,3,4,4,5,5,6,6,7l7,8,8l9,9,10,10,10-heptadecafluoro-/L (total volume 2 L) were shaken in a rotating shaker with 20 rpm for 96 h at 20 C. 2 L -brown glass flasks were used. After phase separation 20 mL per test replicate were transferred from the clear liquid phase to each replicate and covered with glass tops. Dilution water was used for the preparation of the coating solution. Coating period The readily filled and covered beakers were stored at nominally 1 8 -2 2 C, 1 C constant for 14 days. At the end of the coating period the beakers were emptied and used for the test. Preparation of the test medium (saturated solution) 200 mg 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro- /L (total volume 2 L) were shaken in a rotating shaker with 20 rpm for 96 h at 20 "C. 2 L -brown glass flasks were used. After phase separation the suspension was centrifuged for 20 min at 3000 rpm. 20 mL per test replicate of the clear saturated solution were transferred to each replicate. The preparation method had been chosen with regard to the test item properties and in accordance with the relevant guidance documents (OECD 2000, BAUA 2001). CONTROL Dilution water without test item tested under same conditions as the test group. 000013 Dr.u .Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 11 of 31 Project-No. 020109CK Study-No. DAI84111 REFERENCE ITEM CAS No. Item purity Batch No. Stability under storage conditions Test concentrations Range of validity Test duration Potassium dichromate p.a. (Merck) 7778 - 50 - 9 100% K 28974764 2006-02-28 0 .5 8 -1 .0 -1 .8 -3 .2 -5 .8 mg/L 1.0 mg/L < EC (24 h) < 2.5 mg/L 2002-03-27 to 2002-003-28 TEST METHOD Test duration Test vessels Volume of the study medium Dilution water Static 48 h, 2002-04-03 to 2002-04-05 Glass beakers (5 cm ID x 8 cm H), 50 mL volume were used. 20 mL Dilution water according to EEC 92/69 L383A C.2. Annex 2 was used: Component CaCI2 2 H20 MgS04-7 H 20 NaHC03 KCI pH-value Concentration [mg/L] 294.0 123.25 64.75 5.75 7.8 0.2 Number of study organisms per concentration and control Number of animals per test vessel 20 animals, divided into 4 (2*) parallel samples, each with 5 (10*) animals 5(10*) 000014 Dr.U.Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 12 of 31 Project-No. 020109CK Study-No. DAI84111 Number of parallel samples per concentration Age of test organisms Test temperature Illumination Photo period 4(2*) 2 - 24 h old 18 - 22 C, 1 C constant Diffuse light, illumination range max 20 uE/m2/s (corresponding to 1200 lx) 16/8 h light/dark cycle COURSE OF THE STUDY TYPE AND FREQUENCY OF MEASUREMENTS AND OBSERVATIONS The definitive study was performed as limit test with the saturated solution to enable the determination of immobilization after 24 and 48 hours. 2 to 24 h old daphnids were used for the definitive study. They were obtained by removing the mother animals twice within 22 h. Brood daphnids were maintained in 100 % dilution water at the test temperature for at least 48 hours prior to the test. 20 daphnids divided into 4 (2*) groups with 5 (10*) animals per test vessel were used. Control replicates without test item were tested under the same conditions as the test groups. All test beakers were placed in an incubator (light/dark cycle 16/8 for 48 h at 20 1 C). The immobilisation of the daphnids was observed after 24 and 48 hours of exposure. The reference item was tested in five concentrations within the concentration range 0.58 to 5.8 mg/L. Observations, measurements and evaluation were carried out as described below. Prior to test start the water parameters of the dilution water (pH-value, dissolved oxygen concentration, temperature, conductivity and total hardness) were measured. At the beginning of the test the water parameters (pH-value, dissolved oxygen concentration) were measured in one additional replicate per concentration and control. After 48 h the water parameters were measured in all replicates per concentration and control. *) The information in brackets refer to the test of the reference item 000015 Dr.u .Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7 ,7,818,9,9,1 0,10,1O-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 13 of 31 Project-No. 020109CK Study-No. DAI84111 Equipment The temperature was recorded throughout the test with a thermohygrograph. The percentage immobility was determined in all test and control groups after 24 h and 48 h. Oxygen : Oximeter, Oxi 530 (WTW) pH value : pH-Meter InoLab pH Level 1 (WTW) Temperature : Hygro-thermograph (Lu f f t ) Water hardness : Spectrophotometer, Cadas 100 LPG 158 (Dr. Lange) Fluorescence of algae : Chlorophyll-Fluorometer (Kleinfeld) Dispersion treatment: Rotating Shaker 3040, GFL Centrifuge: ZK 364, ZlRBUS STATISTICAL METHODS EVALUATION EC-values and statistical analyses SOFTWARE The effects of the limit concentration as immobilisation in percent were determined directly from the test results. ECso-value was only calculated for the reference item. ECso-value was calculated via probit analysis. Probits according to W eber (1986). Calculation of the confidence intervals was carried out using standard procedures according to B reitig & TOm p lin g (1982). SigmaPlot rel. 2000 (2000), Spss Corporation VALIDITY CRITERIA The test is unacceptable if more than 10 percent of the control organisms are immobilised during the 48 h test period. The control daphnids should not be trapped on the surface of the water. The EC50 after 24 h of the reference substance should be in the range from 1.0-2.5 mg/L. The dissolved 0 2 concentration at the end should be > 5.21 mg/L (60 % of the air saturation value at the temperature used). The deviation of the pH-value from the initial value should not be more than 1 unit. 000016 Dr.U.Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 14 of 31 Project-No. 020109CK Study-No. DAI84111 DETERMINATION OF THE TEST ITEM DEVIATIONS FROM THE GUIDELINE DEVIATIONS FROM THE STUDY PLAN REPORTING ARCHIVING The test concentration level and control was analytically verified by gas chromatography with mass spectrometric detection (m/z = 463 and 395) at test start and test end. Additional replicates were set up for the analytical work. None Purity was C8-perfluoroalkylethanol 99.3 % (ala). LOD and LOQ were 0.009 and 0.027 mg/L, respectively. These deviations had no impact on the quality and integrity of the study. The final report is issued as paper copy (6 originals) and an electronic record (1 original). The following was retained in the archive of the test facility for the period as specified in the operative national GLP regulations: all raw data Study plan (Original 1 of 2) final report paper copy (Original 1 of 6) all records performed by the quality assurance programme including master schedules sample of test item Microfilms will be retained in a safe-deposit by Volksbank Sarstedt, D-31157 Sarstedt. 000017 Dr.U.Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 15 of 31 Project-No. 020109CK Study-No. DAI84111 4 Results 4.1 Solubility of the test item The test item was clearly dissolved throughout exposure. 4.2 Results of the definitive test The percentage immobility was determined in the tested limit concentration and the control after 24 h and 48 h. The immobilisation rates in % after 24 h and 48 h of exposure are given in Table 1. There is no biologically significant effect (10 %) neither in the tested limit concentration nor in control group. 4.3 Results of the reference item The percentage immobility for the reference item was determined after 24 h. The EC10o value was determined directly from the test results. The EC10 and EC with 95 % confidence interval (Cl) were determined by probit analysis according to standard procedures. EC- values after 24 h of the reference item in mg/L were as follows: ECTM : 1.5 ECso : 2.1 (Cl 1 .8 -2 .3 ) EC100 : 5.8 The EC50 - value of reference item potassium dichromate after 24 h is within the prescribed concentration range of 1.0 - 2.5 mg/L of validity criteria according to AQS: DIN Guideline 38412 L 30. 4.4 Water parameters The water parameters (dissolved oxygen concentration, pH-value) of test and control groups at the beginning of the test in one replicate per concentration and control and in all replicates after 48 h are listed in Tables 2 - 3 . pH-value, oxygen concentration, temperature, conductivity and total hardness of the dilution water were measured prior to test start. The results are listed in Table 4. During the test the temperature was in the range of 20 1 C. Dr.U.Noack-Laboratorium fr Angewandte Biologie Report 1-Oecanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro- Acute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 16 of 31 Project-No. 020109CK Study-No. DAI84111 5 Validity criteria The study was performed according to OECD Guideline 202 l/EEC Directive 92/69/EEC Method C.2. The validity criteria were fulfilled: In the control group no Daphnia were immobilised or trapped on the surface of the water. The ECso -value after 24 h of the reference item was in the range of 1.0 to 2.5 mg/L. The dissolved 0 2concentration was > 5.21 mg/L (60 % of the air saturation value at the temperature used). The pH-value did not vary by more than 1 unit. 6 Literature / References BAUA, Bundesanstalt fr Arbeitsschutz und Arbeitsmedizin (2001): Leitfaden fr Anmeldungen neuer Stoffe nach dem Chemikaliengesetz. 3. berarbeitete Auflage B reitig G. & T m p lin g W. (1982): Methoden der Wasseruntersuchungen Bd.II, VEB Gustav Fischer Verlag, Jena. DuPont, Determination of physico-chemical parameters of Perfluorooctylethanol, CAS No. 678-39-7, Unpublished results, Update Feb. 15, 2002 E l e n d t B. P. (1990): Selenium Deficiency in Crustacea, Protoplasma 154, 25 - 30 OECD-guideline 202-I for testing of chemicals. Acute Immobilisation Test of Daphnia magna STRAUS. Adopted April 04, 1984 OECD (2000): Guidance document on aquatic toxicity testing of difficult substances and mixtures. OECD series on testing and assessment no. 23 Weber E.(1986): Grundriss der biologischen Statistik, 9. Auflage Dr.U.Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro- Acute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 17 of 31 Project-No. 020109CK Study-No. DAI84111 7 Physicochemical data: pH-values, dissolved oxygen Table 2: Water parameters at the beginning of the test (measured in one replicate per concentration and control) Saturation Concentration [mg/L] 0.16 Control pH-value 7.79 7.72 0 2-conc. [mg/L] 7.72 7.80 Table 3: Water parameters at the end of test (48 h) (measured in all replicates) Saturation concentration [mg/L] 0.16 Control 1 7.53 7.65 pH-values no. of replicate 23 7.60 7.62 7.63 7.67 4 7.63 7.58 1 7.66 7.53 0 2-cone. [mg/L] no. of replicate 23 7.72 7.73 7.57 7.64 4 7.71 7.35 Table 4: Water parameters of the dilution water Dilution water pH-value 0 2-conc. Temp. Conduct. dated: [mg/L] [C] [pS/cmJ 2002-04-03 7.72 7.80 21.0 672 Total Hardness CaC03 [mg/L] 258 Q00020 __________________ dr.U.Noack-laboratorium fr Angewandte Biologie__________________ Report 1-Oecanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 18 of 31 Project-No. 020109CK Study-No. DAI84111 8 GC - Analysis of 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10heptadecafiuoro- 8.1 Method METHOD OF DETERMINATION Equipment Analyses of various concentrations of 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro-were carried out via gas chromatography on a Fused Silica CP-SIL 8 capillary column using external standards. Detection was performed with a mass selective detector (MS). Gas chromatograph Autosampler Detector Software CP-3800, V a r a n CTC Combi P A L , CTC A n a l y t ic s MS, Saturn 2000, Varan Saturn GC/MS Workstation 5.51, V a r a n Reagents fert.-butyl methyl ether 99.8 %, Batch 423370/1 31101, Fluka CONDITIONS OF ANALYSIS Column Injector Injector temperature Injection volume Temperature programme Chrompack CP-SIL 8 (V a r a n ), 30 m, i.d.: 0.25 mm, LOW BLEED / MS, Film thickness: 0.25 pm Splitless (30 psi pressure puls) for 1 min 250 C 1 pL Heating rate rc/m in] -- 10 30 Temperature PC] 40 90 220 Holding time (min] 0.0 1.0 5.0 Carrier gas Detector Ionisation mode Run time Retention time Helium 1 mL / min column flow MS Electron ionisation (El) 15.33 min approx. 4.9 min OOOl dr.U.Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 19 of 31 Project-No. 020109CK Study-No. DAI84111 STANDARD PREPARATION OF STANDARDS PREPARATION OF SAMPLES Test item was used as standard. Two stock solutions of the standard of 200 mg/L were prepared in terf.-butyl methyl ether, diluted (9 concentrations each) and used for calibration. For calibration range see part 8.2.1. 40 mL of the sample were extracted with 4.0 mL ferf.-butyl methyl ether. After phase separation the extract was injected directly into the GC/MS. METHOD VALIDATION Peak symmetry Repeatability Accuracy Quantification of the test item was calculated by peak area of the masses 69 + 395 + 463 (m/z) based on the external standards. The calibration procedure and the principle for the determination of detection and quantitation limits were adapted from DIN 32645. The method was validated as described below: Peak symmetries were calculated from chromatograms of analytical standards and test item according to the following equation: T = Wo.os / (2-f) T = Peak symmetry W0.05 = Peak width at 5 % of peak height [mm] f = first sector of peak width ( divided by the perpendicular line from the peak maximum ) [mm] 5 sub-samples of the highest and lowest concentration prepared from a single homogenous sample were analysed. Mean values, standard deviations and variations of coefficients were calculated. 5 samples with 40 mL water were spiked with an amount of 8 pg 1Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro- (80 pL of 100 mg/L) to give a final concentration of 200 pg/L. Afterwards samples were extracted as described above. __________________ Dr.U.Noack-Laboratorium fr Angewandte Biologie__________________ Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 20 of 31 Project-No. 020109CK Study-No. DAI84111 8.2 Method Validation The method was validated and tested with satisfactory results with respect to linearity precision (repeatability) peak symmetry accuracy determination limit and detection limit. 8.2.1 Linearity The analytical system gave linear response in the range of 0.1 -1 0 mg/L of 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro-. The calibration curve and chromatograms obtained for standard and test item are given in Fig. 1 - Fig. 6. For limits of determination and quantification see part 8.3. 8.2.2 Quantification Limit and Detection Limit The lim it of quantification (LOQ) and limit of detection (LOD) were calculated using the blind value method described in DIN 32645 "Nachweis- und Bestimmungsgrenze". The LOD was determined to be 0.009 mg/L and therefore the LOQ was 0.027 mg/L (threefold the LOD), see part 8.3. 000023 Dr.U.Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 21 of 31 Project-No. 020109CK Study-No. DAI84111 8.2.3 Precision (Repeatability) The results of the repeatability tests are provided in the table below. Tab. 5: Repeatability of Injections of Test Item Peak area (pV*sj Serial No 1 2 3 4 5 Mean SD C V [%j 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10- heptadecafluoro(m/z = 69+395+463) 0.1 mg/L 0.6 mg/L 2098 2098 1978 1958 2341 2094.61152.5 12141 13563 13291 13597 13500 13218.41613.9 7.3 4.6 8.2.4 Peak Symmetry The peak symmetry of the test item 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10heptadecafluoro- was 1.8. 000024 Dr.U.Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 22 of 31 Project-No. 020109CK Study-No. DAI84111 8.2.5 Accuracy Tab. 6: Mean Recovery Rate of Fortified Samples Fortified concentration of test item 0.1986 [mg/L] Replicate 1 Replicate 2 Replicate 3 Replicate 4 Replicate 5 Mean SD (N-1) CV% LOQ [mg/L] LOD [mg/L] Linearity correlation coefficient ( r2 ) 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10 -heptadecafluoro- calc. cone. RR (mg/L] [%1 0.22 111 0.24 121 0.23 116 0.21 106 0.21 106 0.21 106 0.22 111 0.21 106 0.21 106 0.21 106 110 5.3 0.027 0.009 4.8 0.9906 calc. cone. RR LOQ LOD SD (N-1) CV calculated concentration, accumulation factor taken into account Recovery rate related to the nominal concentration of the test Item Limit of quantification Limit of detection standard deviation coefficient of variation ,,G002S d r .U.Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 23 of 31 Project-No. 020109CK Study-No. DAI84111 8.3 Results Tab. 7: Concentrations of the Active Ingredient 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10, 10,10-heptadecafluoro- Sampling Date Start of Analysis Test Item Replicate No. Saturated solution 1 2 Control LOQ [mg/L] LOD [mg/LJ linearity ( r2 ) 2002-04-03 Test Start 2002-04-05 2002-04-05 Test End 2002-04-05 1.n a ra n n l 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10heptadecafluoro- Calc. Conc. [mg/L] Calc. Conc. [mg/L] 0.12 0.14 0.10 0.15 0.13 0.23 0.13 < LOQ < LOQ 0.28 0.027 0.009 0.9996 0.0071) <LOQ Mean [mg/L] 0.16 calc. conc. LOQ LOD 1) = calculated concentration, accumulation factor taken into account = Limit of quantitation = Limit of detection = single incident was not included in calculations (peak area of accumulated sample was > LOQ) 000026 Dr.U.Noack-Laboratorium for Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 24 of 31 Project-No. 020109CK Study-No. DAI84111 8.4 Calibration Curves The calibration curves shown were established for different concentration ranges and at different times. Calibration Curve of Fluowet (2002-04-04) Fig. 1: Calibration Curve of Standard - concentration range 0.01 - 0.06 mg/L (dated 2002-04-04) 000027 Dr.U.Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 25 of 31 Project-No. 020109CK Study-No. DAI84111 Calibration Curve of Fluowet (2002*04-10) 500000 450000 400000 ^ 350000 300000 -- 250000 200000 < 150000 100000 50000 0 0 2 4 6 8 10 Conc. [mg/L] Fig. 2: Calibration Curve of Standard - concentration range 0.1 - 1 0 mg/L (dated 2002-04-10) Calibration Curve of Fluowet (2002-06-19) Fig. 3: Calibration Curve of Standard - concentration range 0.1 - 0.6 mg/L (dated 2002-06-19) 000028 __________________ Dr.U.Noack-Laboratorium fr Angewandte Biologie__________________ Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 26 of 31 Project-No. 020109CK Study-No. DAI84111 The first calibration curve was established 2002-04-04 but the concentration range (0.01 - 0.06 mg/L) was broad enough to be used for all tests running. Therefore the second curve (2002-04-10) which covers a much wider range ( 0 . 1 - 1 0 mg/L) was used for the calculations in this test. The concentration calculations using the two different curves do not differ more than 10 % from each other. The calibration curve from 2002-06-19 with a concentration range of 0.1 - 0.6 mg/L shows that the GC/MS system has a good stability over a long period of time. 000029 Dr.U.Noack-Laboratorium fr Angewandte Biologie Report 1'Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro- Acute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 27 of 31 Project-No. 020109CK Study-No. DAI84111 8.5 Chromatograms T e g a Compound R ap ai h r #1 (mm 84110.1 |_1-SM8 Sampia ID: tnstrvfnent D: Measurement Type: Acquidtion Dale: Calculation Data: Sample Typo: Inj. Sampia Notes: Oivlsor: 8411 0 .1 1 Area 10.04.02 13:21 11.04.02 08:08 Calibration 1,000000 Operator. La stC riib ra tio n : Celibraon Type: Data Fila: Method: 11.04.02 06:08 Extamai Standard c \... 84110.1 i 1.m c\...\8411_fep2.m th M ultiplier: 1,000000 Parameter Compound Number Retention Time RT Offset Peek Name CAS Number Status Quan lone Area Height Amount (RF) Fit Calibration Equation Baseline Code Specification 4,918 +/- 0,200 69+3954463 > -1 0 >700 Linear, Include, Nona Actual 1 4,911 min. A0,00678 min. Ffcowet 876-39-7 4368 2263 44124,941 971 y +4,4125e+4x *0,0 BB Slatoa P a is Peas Pass Segnane 2 T im <n*i* 3,485-16,318 Scans: 210-1828 fentzatan: E lA tio P r^am tlcn: Nona Q w n f e : 1 Fig. 4: Chromatogram of Standard 0.1 mg/L (dated 2002-04-10) 000030 Dr.U.Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 28 of 31 Project-No. 020109CK Study-No. DAI84111 TteDM Cm nwuxIRtocrl t o il from DM04111 EO LU -SM S Sample IO: (natrumant D : Measurement Type: Acquisition Date: Calculation Date: Sample Type: Inj. Sample Notes: Divisor: DAI34111 E O LI Area 05.04.02 18:51 09.04.0208:39 Analysis 1,000000 Pacaoutac Compound Number Retention Time RT Offset Peek Name CAS Number Status Quart Iona Area Haight Amount Fit Calibration Equation Baseline Coda Spcification 4,925 4/. 0,200 69+395*463 >*10 > * 0,000 >*700 Linear, Ignore, Nona O ps raion LastCahbratkm; Calibration Typs: Osta Ft: Method: 05.04.02 13:48 External Standerd c\...dal84111 a g l c\...\8411_rap2.m th M ultiplier 1,000000 Actual 4,927 min. 0,00185 min. Fluowet 678-39-7 XC 61538 24045 3003 997 y * +2,028Se+4x+830,0136 68 StaHa Paw Error Pass Paw Paw 5 m n m 2 TOrtomm* 3.400.W .312 S c a n t 210-1012 bnfralon; Et M as P -fa m O m N w . C h in a te : 1 Fig. 5: Chromatogram of Teat Item Saturated solution at the test end (dated 2002-04-05) 000031 Dr.U.Noack-Laboratorium for Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 29 of 31 Project-No. 020109CK Study-No. DAI84111 TargetComprend R *x rt for ( fnm DA1M111J t E Wr L2.SM8 Sample ID: Instrument ID: Measurement Type: Acquisition Date: Calculation Data: Sample Type: Inj. Sample Notes: Divisor: DAt8411t_2 E K trl Area 05.04.02 18:30 08.04.02 08:39 Analysis 1,000000________ Parameter Compound Number Retention Time RT Offset Peak Name CAS Number Status Quan tone Area Haight Amount F it Calibration Equation BasaNna Code Specification 4,925 H - 0,200 69+395+463 10 0,000 >*700 Linear, latore, Nona O perator Last Calibration: Celtoration Type: Date File: M ethod 05.04.02 13:46 External Standard <x\...<M 64111_2ekt c\...\8411_repZm th M ultiplier.___________1,000000 Actua| 1 4,923 min. A0,00184 min. Fluowet 878-39-7 X 'C 335 176 N/A 627 y +2,0285a+4x+630,0136 BB Statoe Peas Error Pare Fail Pam Staue end Erare: * : No iw uS cw he c a lttie le l; c h e ti catertew awve. C : ResuS ad of Tdereiee er GtebnOon R ap*- Fig. 6: Chromatogram of Control at test end (dated 2002-04-05) 000032 Dr. .Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoro- Acute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 30 of 31 Project-No. 020109CK Study-No. DAI84111 9 Certificate of 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10heptadecafluoro- Analysis CUriaai Gm bH, Warft Gtnderf CQ C / QuattumMtcm*M D>8*30* Btirfkirehaa Fi: +-*9 5679 l 267 C la r ia n t Inspection certificate a cco rd in g to EN102Q4-3.1B D ate: 13.11.2001 Page: 1 / 1 Our c on sign ! Material M ar.erial-r.o a d '.- .l N o . 1-Oecanol, 3 ,3 ,4 ,4 ,5 ,5 ,6 ,6 ,7 ,7 ,8 ,8 ,9 ,9 ,1 0 ,1 0 , 1G -h e p t a d e o a fl u o r o 10*1705 ?00/0i Os en e - . a t e n , o f w n i . - - r.iio . ' o n a i q n i p e n t i s a p a r e , t h e C o l l o w m q ' r a l u e s p f ,- . o r ; R ir .e ru . ' . . a y c o n t u x T . r;iv r .q e e e d p r o d u c t s p e c i f i c a t i o n . r .n sc a c t t tr. r .a r a i r. r. l j / -me t h ocia pec o. i c a c i o r . R e su lt T3-Ter i *uo:2 iky-loth a n d J3D H i : ! V .iw um P e r i l u o r o a l k y l e t h a n o l C a p il l a r y CC Sum P e c r l ' - o c i U y i b u t a n o i CaciU ary j C Sum ? e t f 1c a r s < y i s c h e n e C a p i l l a r y CC tfater content K a rl r ia c h e r OIN 31777 S-X eth yipyrroliicr.e content C a p i l l a r y CC CM 00 11 VV > - 97,5 > - 98,0 < -1 ,0 <-G , 2 9 9 , J% J a / a ) 99 ,9 % [a /a ] < 0,1% [a /a} < 0, 1% (a / a ) c 0 , 1% <0,1% The aoeva p a r t i c u l a r s c o not r e l e a s e th e cu sto m e r from th e o b l i g a t i o n c a r r y out an in sp e ctio n o f goods received . to Ms. s aumgac tn ar - W crk sin sp e cto r 000033 Dr.U.Noack-Laboratorium fr Angewandte Biologie Report 1-Decanol, 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluoroAcute Immobilisation Test (48 h) to Daphnia magna STRAUS Limit-Test with the Saturated Solution, acc. OECD 202 I Page 31 of 31 Project-No. 020109CK Study-No. DAI84111 10 GLP-Certificate of Dr.U.Noack-Laboratorium F) N M tr s Ic h ilB C h M Um w U m W U rtu w Gut Laborpraxls/Good Laboratory Practice GLP-Boschelnlgung/Statement of GLP Compliance (gem/aocording to 19 b Abe.1 ChsmBcallanp-- tz) Eine GLP-Inapektion zur berwachung der ElnhaHung der GLP-GrundsAtze gemflQ Chemikaliengesetz bzw. Richtlinie B8/320/EG wurde durchgefhrt In: Assessment of conformity with QLP according to Chemlkailengesetz and Otewcttve 88/320/EEC at: X Prfeinrichtung / Test facJNty Profetandoli ! Teet alta D r. U. NOACK LABORATORIUM fr angewandte Biologie Kfithe-Paulua-Str. 1 D -31157 Sarstedt Or. U. NOACK LABORATO RY of applied biology Kflthe-Pautua-Str. 1 D -31157 Sarstedt (i 0 -- Sehnung und Adf-- MAJneguhooal name and addraaa) Prfungen nach Kategortan/Areas of Expertise (gsm M/aaaafdlne ChanAtoV-GLP Nr. 5 .V 0 6C D guktanca) 1 - Prfungen zur Bestimmung der phyalkailech-chemlachen Eigenscharften und GehaKsbestimrmingen 3 - Prfungen zur Bestimmung dar srbgutverandemden E igarschatten (In vitro und in vivo) 4 - Umwelttoxlkologlsche Prfungen zu Auswirkungen auf aquatlscha und terrestrische Organismen 5 - Prfungen zum Verhalten im Boden, Im W asser und In dar Luft, Prfungen zur Bioakkumulation und zur Metabollslarung 6 - Prfungen zur Bestimmung von Rckstnden 7 - Prfungen zur Bestimmung der Auswirkungen auf Mesokosmen und natrliche kosysteme Datum dar Inspektion / Date of inspection (TsO'McmeLJahr/ dsy.monei.yssr) 25. - 27. Juni 2001 / June 2 5 * - 2 7 *. 2001 29. A ugust und 21. Septem ber 2001 / A ugust 2 9 * and Septem ber 2 1 **, 2001 D ia genann te PrO fainrtchlunp/P ar genannte P rtSatoM art b efindet sfch im nationalen G LP Q berw aehungeverfehren und w ird regelm ig a u f Einhaltung d e r G LP -G rundsS tze berw acht. A u f d e r G rundlage des InapekMonabertchtee w ird hierm it besttigt, daes in d iee a r PrQtelnrtchiung/dleesiw PrQfatandort die oben genannten Prfungen unter Einhaltung d e r O LP -G runds itz e durohgeflOhrt w erden knnen. Niederechslsches Umwattministart! Referat 33 Archivstrae 2 30169 Hannover T he above m entioned te e t feclM y / te at alts Is included In the national G LP C om piane# Program m e and is Inspec ted on a regular beala. Baaed on the inspection report It can b e confirm ed, th at this te s t fa d tty / la s t a lte (a a b le to conduct the aforem entioned studies in com pliance w ith th e Principles of GLP. 11. Mftrz 2002 Im Auftrge ,- Or. Braedt 0001