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AR226-3340 o2 \ % E.l. DUPONT DE NEMOUKb & COMPANY INC. REPORT NO: /__GL-2001-42 j ____________ C0PY NO' 5 TITLE: Anuatic Toxicity andjolubilitv off i j j B ^ F liio r o te .lo m e r Intermediate 1 AUTHOR: \ Roland C. Hall, Jr. J L_ ^ ^__ > CONTRIBUTORS: /Thomas V. Robertson, Olver Laboratoriesj DISTRIBUTION: ABSTRACT ONLY ! Company Sanitized. Does not contain TSCA CBi GL-2001-42 J 1 Report Num ber. C TL-2001-42_j Issued. December 5, 2001 Technical Report Aquatic Toxicity and Solubility of. )nrnfpinmer Intermediate Report Written By Period Covered Research Notebooks Work Supervised By n Roland C Hall, Jr December 2000 to May 2001 NA F KmecT^ ' Abstract , , , Hn-nphv Olver Labatones to determine the the aquatic This report,d TM toxicity and solubility or 0Tie, study was conducted in "component of the spin agent to be used f the new spin agent in " " ^ p l a n r w a s subsequently eancded. however, f t e l l S n m this report was forwarded to the Lme 3 organ,satton to asstst m meeting their environmental requirements ^ ^ Olver Laboratones determined that the solubility S r a p p e a r e d ,0 be the order T^eir screening tests also indicated no acute toxicity at comentr maximum solubility of 5 mg/L nressure ^ Company Sanitized. Does not contain TSCA CBI Th* report contains confident!, rif th, '.rhnipiil Manager. may be reproduced withou, the approve, TABLE OF CONTENTS Introduction Objectives Summary and Conclusions i Patent Situation Program Publication Status Acknowledgement Signature(s) Appendixes 1 1 1 2 ~i 2 *> 3 4 Company Sanitized. Does not contain TSCA CB! G L - 2 0 0 1-42 INTRODUCTION In late 2000 addkeeccii,ssiioo. nn. wwaass made U ct~nomevnaalup.anttetothbeespteisnteadgewnat.tob_e______ , in t h e 0 A llOt Plant Th, P ! ^ n ich lo ro elh v len e Tn order to obtain FluorSornenntermedi ate and tran J ^ M ^ f c d o t plant, information w a s ^ -- environmental approval to run t e t e s J' 1 ..g e iu ^ ^ r e w a s noputtisRea^afa available n eed ed on the a q u a d c t o j g j y ^ therefore a study was on aquatic toxicity coZ.ss.oned ft ofterUboratonesto rhe solubility m water and the ho,,ever. fte ~ aquaticto^toit)|fhe test in the pilo P ^ organization to assist m meeting T ^ S m S i ^ d i i s report was forwarded to the Line i orca their environmental requirements OBJECTIVE The purpose of this ot the study was to deterame Fluorotelomer Intermediate at a maximum cone Cenodaphnia and fathead minnows (Pimephales promel ) SUMMARY AND CONCLUSIONS t0 near the conducted ustng an expanded test solulion sen a P o u r e d j S ! l s tndtcated that small amounts of methanol to .crease solubrl ty T he m a m ,,a s not acutely toxic to Cenodaphnia and fa head mmno ^ ha,K ^ 48. hour at concentrations approaching met ano ai , than 500 msA . The no LCso values for Cenodaphnia observed effect concentration (NOEC) tor th Fathead Minnow Reproduction chrome test was 100 m g ^ w htkthe NOECM b r f t e T C 5 ^ ^ S u m val and Growth chronic test w a s / " Z S Z e n c e ^ R n the maximum be no direct acute or chronic toxicity due to the presence o t ^ ^ T armarent solubility m water of 6 mg/L PATENT SITUATION At the present time we have no plans to tile for a patent Company Sanitized. Does not contain TSCA CBI GL-2001-42 PROGRAM No additional testing is planned at this time PUBLICATION STATUS At the present tinte e have no plans to pnbltsh the data conta,ned ,n th.s report acknow ledgm ents Thanks to Tom Robertson and Olver Labortones. Incorporated for then conmbonons ,0 this study and report. 1 SIGNATURE(S) Sanitized. Does not contain TSCACBl Company GL-2001-42 (> APPENDIX Appendix A Memo from R Lawrence Hoffman, V ic^ 'residenl, Olver Laboratories to (Thomas V. Robertsonjdated May 4, 2001 subject p p P P Kr'o~l'u"b,~i'l,i`t"y and' Toxicity Determination Program, Job Number 60175 ' Appendix B "Determination of solubility and aquatic toxicity of DuPont Product fi^^jpBFIuorotelomer Intermediate for E E DuPont De Nemours and Company by R j^rwrcnce Hoffman dated May 3, 2001 Company Sanitized. Does not contain TSCA CB OLVER Consulting Engineers Environmental Laboratories LABORATORIES 1116 South Mam Street Blacksburg, Virginia 24060 May 4, 2001 Mr Thomas V. Robertson) Development Associate Environmental Affairs E.l du Pont de Nemours and Company, Inc P O Box 27001 Richmond, VA 23261 J ^ 0 R S o Iu b ility and Toxicity "Determination Program, Job Dear Tom Enclosed for your review and use are three (3jcopies of the report which describes the performance and results of th e g B B ^ o lu b ility and Toxicity Determination program performed by Olver Laboratories Incorporated for E I du on de Nemours and Company, Incorporated. This program was performed to support evaluations of the potential for the use of this product by examining its potential effects on wastewater toxicity The program, as described in our December 14, 2000 proposa , consisted of an initial determination of solubility in water and subsequent determinations of acute and chronic toxicity to two common freshwater test organisms As for the standard compliance monitoring performed by Olver Laboratories for DuPon , the toxicity testing component of this program is reported in a GLP format As indicated on the Material Safety Data Sheet provided with the sample, the material appeared to be only slightly soluble in water As described in thajeport, the solubility of the material in water appeared to be in the order of 6 mg/L at standard temperature and pressure. The solubility in water appeared to in c re a ^^^je v e ls o 500 mg/L to 1000 mg/L by adding a small amount of methanol to t h e | l^ ^ | 3Jrninor itnto ,, addition to water For the reasons referenced in the report, the analysis of th msolutions provided inconsistent results and could not be used to confirm the concentrations used in the toxicity evaluation component of this program. Blacksburg, VA (540) 552-6974 Company Sanitized. Does not contain TSCA CBI Mr Thomas V. Robertson "May 4, 2001 - Page 2 The initial screening tests indicated no acute toxicity at concentration!near the apparent maximum solubility of 6 mg/L. In an effort to determine th e p B g p n c e n tra tions that results in acute and chronic toxicity, acute anachronic testing was conducte using an expanded test solution series prepared u s in g M p m e n d e d with smal amounts of methanol to increase solubility. The results of tfiese tests indicated that M L a s not acutely toxic to Ceriodaphma and fathead minnows (Pimephales J ^ rm la s ) at concentrations approaching methanol-aided solubility limits. The 48-hour l_r values for Ceriodaphnia and fathead minnows was greater than 500 mg/L. Tlne no observed effect concentration (NOEC) for the Three-Brood Ceriodaphnia Survival and Reproduction chronic test was 100 mg/L while the NOEC for the 7-Day Fathead Minnow Survival and Growth chronic test was 500 mg/L These results suggest tha there should be no direct acute or chronic toxicty due to the presence o f g p ^ a t the maximum apparent solubility in water of 6 mg/L ' I look forward to the opportunity to discuss this with you in more detail and to answer any questions that you may have As always, please do not hesitate to contact me or David Griffiths Sincerely, R Lawrence Hoffman Vice President RLH/egl Enclosures cc: David W Griffiths, Ph.D.. President, Olver Laboratories Incorporated Company Sanitized Do* not contain TSCA CBf STUDY TITLE DETERMINATION DFSOLUBIUTY AND AQUATIC TOXICITY OF DuPONT PRODUCT m fjK f^LU O R O T E LO M E R INTERMEDIATE FOR F I DU PONT DE NEMOURS AND COMPANY DATA REQUIREMENTS DuPONT CONTRACT ORDER NUMBEf AUTHOR R. LAWRENCE HOFFMAN STUDY COMPLETED ON May 3, 2001 PERFORMING LABORATORY OLVER LABORATORIES INCORPORATED ENVIRONMENTAL LABORATORIES AND CONSULTANTS 1116 SOUTH MAIN STREET BLACKSBURG, VIRGINIA 24060 for ' OLVER LABORATORIES INCORPORATED JOB NUMBER 60175 Comnww f*AAA AAl A*A<A!n QgJ OLVER LABORATORIES TABLE OF CONTENTS REPORT APPROVAL RECORD QUALITY ASSURANCE STATEMENT GENERAL INFORMATION . . . . PROJECT P E R S O N N E L................. SUMMARY . . INTRODUCTION METHODS AND MATERIALS 1-41 0 SOLUBILITY DETERMINATION........... 2 0 QUAT1C TOXICITY DETERMINATION 2.1 TEST ORGANISMS . .................................... 2.2 TEST SUBSTANCE . . . : ........................................ 2.3 DILUTION WATER ................................................. 2.4 TOXICITY TEST PROCEDURES.............................. 2.4.1 GENERAL PROCEDURES.............................. 2.4.2 TOXICITY RANGE-FINDING T E S T S ............. 2.4.3 ACUTE TOXICITY TESTING ....................... 2 4.4 CHRONIC TOXICITY T E S T IN G ..................... 2.5 STATISTICAL ANALYSIS.......................................... RESULTS . . 1.0 SOLUBILITY DETERMINATION 2 0 M S h TOXICITY DETERMINATION . . 2.1 TOXICITY RANGE-FINDING . . 2 2 ACUTE TOXICITY TESTING . . . . 2.3 CHRONIC TOXICITY TESTING . Page Number h 1 2 3 4 4 4 4 .4 .5 .6 6 .6 8 8 9 10 11 11 12 12 12 14 Company Sanitized. Does not contain TSCA CBI OLVER LABORATORIES Table 1 Table 2 Table 3 LIST OF TABLES Toxicity Range-Finding Data Summary Acute Toxicity Data Summary . . . . ................. - 13 15 Chronic Toxicity Data Summary - Companson to Standard Controls . . . ................................................ . 16 Table 4 Chronic Toxicity Data Summary - Comparison to Methanol- Spiked Controls ............. ................................................ 17 APPENDICES Appendix 1 Material Safety Data Sheet . . . ........................... 18 Appendix 2 P j ^ ^ o l u b i l i t y Determination - Test P r o t o c o l................. i Appendix 3 ^ J J ^ o lu b ilit y Determination - Analytical D a ta ..................... . 25 27 Appendix 4 Toxicity Range-Finding Test Data . . . - - . 32 Appendix 5 Acute Toxicity Test Data . . . ....................................... . . 39 Appendix 6 Chronic Toxicity Test Data - Pimephales promelas . . . . . 45 Appendix 7 Chronic Toxicity Test Data - Cenodaphnia dubia . . . . 67 Appendix 8 Acute Reference Toxicity Test D a t a ........................ . 93 Appendix 9 Chronic Reference Toxicity Test D a t a ................................... . 101 Appendix 10 Dilution W ater Quality Analyses D a ta ..................................... 113 Appendix 11 Chemical Analyses of Brine Shrimp and YCT Food Mixtures 122 Company Sanitized, Does not contain TSCA CEI OLVER LABORATORIES Report Prepared by: Susan Mirlohi Date Bioassay Laboratory Manager Reviewed and Approved for Issue by R Lawrence Hoffman Vice President and Study Director 5~j 3 Date Company Sanitized. Does not contain TSCA CBi OLVER LABORATORIES n i 1AI ITY ASSURANCE STATEMENT Quality Assurance Statement for final report entitled "Determination of Solubility and Aquatic Toxicity of DuPont P r o d u c t^ |^ B B ^ F lu o r o te lo m e r Intermediate for E I du Pont de Nemours and Company Audits for the study were conducted on the dates listed below: Items Audited Sample Receipt Range-Finding Test Initiation Range-Finding Test Termination Acute Test Initiation Acute Test Termination Chronic Test Initiation Chhomc Test Renewal Chronic Test Termination Audit Dates 1/ 11/01 1/25/01; 2/01/01 1/27/01; 2/03/01 2/14/01 2/16/01 2/13/01; 2/20/01 2/14/01; 2/21/01 2/20/01; 2/27/01 Date findings reported to management and study director -- 2/27/01-- . The information provided within this report was generated in accordance with Good Laboratory Practice Regulations and Protocols. A final review of all data and records indicate the report submitted is an accurate reflection of the study conducted: Reported by: Prian d. Bjoltinghouse Date (Duality Assurance Auditor, Olver Laboratories ii 1Company Sanitized. D*s contain TSCA CB OLVER l a b o r a t o r ie s Material Tested: CFNFRAL INFORMATION Olver Sample Designation: Study Initiated; Completed: Experimental Start; End: . Location of Onginal Raw Data and Final Report: 1/12/01; 5/03/01 . 1/25/01,2/27/01 Olver Laboratones Incorporated 1116 South Main Street Blacksburg, Virginia 24060 Page 1 60175 Company Sanitized. Does not contain TSCA CBI OLVER LABORATORIES PROJECT PERSONNEL The study director of itus project for E. 1, du Pont de Nemours and Company was ^ R . Lawrence Hoffman.J The following Olver Laboratories personnel assisted with the various phases of the aquatic toxicity determination study NAME TITLE lNIT!ALS Susan Mirlohi Stacey Boyles Sheryl Newton Laura Dunham Fran Boltinghouse Bioassay Laboratory Manager Biological Technician Biological Technician Biological Technician Quality Assurance Officer S.Q1- 5 PW Lml? i Page 2 60175 Company Sanitized. Does not contain TSCA CBI OLVER LABORATORIES PRODUCT DETERMINATION OF SOLUBILITY IMP AQUATIC TOXICITY OF DuPONT P R u OROTELOMER INTERMEDIATE SUMMARY Solubilityandaguatic toxicity determination studies were performed for the DuPont product, facilitate projections and assessments of the potential for toxicity in wastewater that'may contain this material. The solubility determination was performed using a procedure developed by Olver Laboratories based on the substai^^tfprm ation contained on the Matenal Safety Data Sheet (MSDS) provided by DuPont. Jp P jpo iu bility in water wag estimated by establishing a calibration curve for GC/MS analysis. The solubility of B a f f in water was determined to be on the order of 6 mg/L. However, when introduced as a methanolic solution, it proved possible to produce wha^mpeared to be homogenous aqueous solutions containing as much as 1,000 mg/L o f ^ is believed that these are not true solutions, but rather dispersions or micellar solutions The aiute and chronic toxicity of B H I to Cenodaphnia dubia and fathead minnows (Pimephales promelas) was assessed utilizing EPA/600/4-90/027F and EPA/600/4-91/002 methods ^ Toj^city testing consisted of initial range-finding tests which included a wide range o f B B p ncen^rat|ons to establish a general level of toxicity for acute and chronic testing using Cenodaphnia dubia and fathead minnows. Toxicity range-finding tests were followed by 48-hour static acute Cenodaphnia and fathead minnow tests, a three-brood chronic Cenodaphnia dubia test, and a 7-'day chronic static renewal fathead minnow test The concentration series used in the toxicity ram e^nding tests ranged from 0.01 to 1,000 mg/L o f F o r acute toxicity testing,ppjfconcentrations ranged from 5 to 200 mg/L, while chronic testing included concentrations which ranged from 5 to 500 mg/L Estimated toxicity endpoints (LC5Dand NOEC values) were found to be as follows. Toxicity Test Type Toxicity End-points Cenodaphnia Acute Test Fathead Minnow Acute Test Cenodaphnia Chronic Test - Survival Cenodaphnia Chronic Test - Reproduction Fathead Minnow Chronic Test - Survival Fathead Minnow Chronic Test - Growth LC^ >500 mg/L (100% survival at 500 mg/L) LCjq>500 mg/L (100% survival at 500 mg/L) NOEC = 100 mg/L NOEC = 100 mg/L NOEC = 500 mg/L NOEC = 500 mg/L Page 3 60175 Company Sanitized. Does not contain TSCA CBt INTRODUCTION Solubility determination and aquatic toxicity testing for the DuPont p ro d u c t------- ere ngrfnrmpd hv Qlver Laboratones Incorporated for the E.l. du Pont de [Nemours and C o m p a n y W B i l i B i r o m January 12*2001 to February 27, 2001. The5 pyuuirppuoosec of this study w is to detergiiml the solubility o f p m | n water and to determine thiee acute anI d chronic toxicity o f M p o representative freshwater organisms. The toxicity oc f^f lH n v ras assessed through determination of median lethal concentration (LC50) valueess'for acut te testing and no observed effect concentration (NOEC) values for chronic testing, using Ceriodaphnia and fathead minnows. METHODS AND MATERIALS 1.0 olubiiity Determination All testing was performed using a sample contained in a 3.63 kg/8 lb can bearing t h e T a b e f : | | ^ H H H H H H I ^ ^ H H j l P Solubility tests were performed according to the test protocol that is provided in Appendix 2. M2.0 Aquatic Toxicity Determination The toxicity tests were conducted according to "Methods for Measunng the Acute Toxicity of Effluents to Freshwater and Marine Organisms", EPA/600/4-90/027F and Short-Term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms", EPA/600/4-91/002 The toxicity testing component of this study was conducted following Good Laboratory Practice general testing and reporting guidelines and the final report was reviewed by the , Olver Laboratories Quality Assurance Unit. Copies of the report and original raw data will be maintained by Olver Laboratories. The original signed report and raw data will be archived at Olver Laboratories Incorporated. 2.1 Test Organisms Ceriodaphnia dubia and fathead minnows, originally obtained from the U.S. EPA and subsequently cultured at Olver Laboratories, were used for acute and chronic testing. Fathead minnow and Ceriodaphnia cultures were maintained in EPA moderately hard water and the culturing records indicated that the test organisms were in satisfactory health at test initiation. Ceriodaphnia cultures were fed a YCT (yeast-cerophyll-trout chow) and algae (Selanastrum capncomutum) food mixture prepared at Olver Laboratories. Fathead minnow cultures were fed brine shnmp nauplii (Artemia sp. eggs obtaineckfrom Ocean Page 4 60175 Company Sanitized. Does not contain TSCA CBI Star International Inc.", Snowville, VT, Lot No. 4400). Test organisms were fed for at least two hours prior to use in testing. Larval fathead minnows used in the chronic testing (Olver Culture No. 1810) were 1-24 hours old at test initiation and the control organisms had an average dry weight of 0 429 mg at test completion. The biological loading factor in the controls was 0.02 g . Test organisms were fed 0.1 mL of a concentrated suspension of newly hatched (less than 24 hours old) bnne shrimp nauplii (approximately 700 to 1000 nauplii) 2-3 times daily during testing Larval fathead minnows used in the acute testing (Olver Culture No 180 ) were 3 days old at test initiation. The biological loading factor in the controls was 0 05 g/L with an average weight (not dried) of 2.4 mg at test completion. The Ceriodaphnia dubia used in the chronic test were obtained from Olver Laboratories cultures produced from EPA-supplied stock. Cenodaphnia used in the chronic testing (Olver Culture Nos. 1-30) were less than 24 hours old, and all within 8 hours of the same age, at test initiation, and the control organisms had an average reproduction of 25.9 (per surviving female) at test completion. Test organisms were fed 0.1 mL of YCT and 0 1 mL of a cobcentrated suspension of algae (approximately 3.1 x 107 cells) once daily at test solution renewal time. Cenodaphnia used in acute toxicity testing were less than 24 hours old at test initiation and they were not fed dunng testing. The brine shrimp and YCT used in feeding were tested to show that concentrations of metals, pesticides, and PCBs remained within acceptable limits No chemicals were present in the bnne shrimp that made them unsuitable for use as a food source in aquatic toxicity tests. Data for these analyses are included in Appendix 11 Monthly reference tests (Appendices 8 and 9) were performed to ensure that test organism sensitivities and health were within acceptable limits. A sodium chloride reference toxicant (EM Science; CAS #7647-14-5) was used and the results showed fathead minnow and Ceriodaphnia sensitivities to be comparable to ranges previously established at Olver Laboratories. 2.2 Test Substance A concentrated sample f jjjH p ^ o n ta in e d in aon^gallonsealeqynetal container was provided to Olver LaboratonesTy the D u P o n t [ jH B H H 0 ^ ^ | a c il i t y The MSDS provided with the sample identified the material a ^ U ^ u o r o t e io m e r Intermediate with the following composition: Page 5 60175 'Company Sanitized. Does not contain TSCA CB1 Based on the results of th e (B (|s o lu b ility determination, various concentrations of were prepared for use in acute and chronic toxicity testing. The solubility l e v ^ ^ in water was estimated at 6 mg/L, therefore, the theoretical concentrations o f jp P u s e d in initial range-finding toxicity tests were selected at and below the 5 i n s o lu b i l i t y level Since no toxicity was observed at this level, higher concentrations of B d f v e r e prepared for use in the acute and chrome toxicity testing. These rangedfrom 5 to 500 mg/L To enhance the solubility o f p jj^ p in preparing test s o lu tio n s , ((^ v a s initially dissolved in methanol (Burdick & Jackson, High Purity Methanol, CAS #67-56-1) prior to being mixed in dilution water Test solution preparation for the range-finding, acute and chronic t ^ n u i is described in Section 2.4 2 through 2.4.4. In all cases, preparations of the H P standards and test solutions was performed in a manner to minimize loss by volatization to the xtent practical. 2.3 Dilution W ater The dilution water used for culturing, toxicity testing, and f l t f e s t solution preparation was moderately-hard synthetic freshwater prepared using EPA guidelines (EPA/600/490/027F and EPA 600/4-91/002) This dilution water was aerated prior to testing with oilfree compressed air. pH ranged from 7.7 to 8.0, conductivity ranged from 300 336 /mhos/cm, alkalinity ranged from 60 to 64 mg/L, and hardness ranged from 84 to 100 mg/L. Annual dilution water quality analyses data are provided in Appendix 10. 2.4 Toxicity Test Procedures 2.4 1 General Procedures The acute and chronic toxicity tests were performed at 25C 1C by placing the test chambers in a constant temperature water bath. Test organisms were exposed to ambient laboratory light (50-100 foot candles, measured at water surface) for a 16-hour day/8-hour night photoperiod. Transitional lighting (30 minutes, 30-40 foot candles) was included at the beginning and end of the 16-hour light period For the Cenodaphnia dubia acute toxicity tests, plastic beakers filled with 25 mL of test solution were used. For the fathead minnow acute toxicity tests, 600^ mL glass beakers filled with 500 mL of test solution were used. Beaker positions were randomized in the water bath using random numbers. Test organisms were pooled Page 6 60175 Company Sanitized. Does not contain TSCA CB1 and placed (five at a time) into each test solution in a random order. Test organisms were less than 24 hours old for the Ceriodaphnta acute tests and within 1 to 14 days old and within 24 hours of age for the fathead minnow acute tests. Routine chemical analyses were cond^ted. Alkalinity and hardness were measured in the control and h ig h e s tU B p te s t concentrations at test initiation. Conductivity, was measured in all test concentrations at test initiation and termination. Dissolved oxygen, pH, and temperature were measured daily in one replicate per effluent concentration. All chemical analyses were conducted as per the EPA document "Methods for Chemical Analysis of Water and Wastes (EPA 600/4-79-020) or APHA, "Standard Methods for the Examination of Water and Wastewater", 18th Edition. Dissolved oxygen was determined by electrode EPA Method 360.1. PARAMETER ` PH Temperature Dissolved Oxygen Conductivity Alkalinity Hardness TEST METHOD EPA 1501 EPA 170 1 EPA 360 1 EPA 120 1 EPA 310 1 EPA 130 2 TEST SOLUTIONS ANALYZED FREQUENCY All Daily All Daily All Daily All . Beginning/End Control and Highest Concentration Beginning Control and Highest Concentration Beginning For the Ceriodaphnia chronic test, 30 mL plastic beakers filled with 15 mL of test solution were used. Beaker positions were randomized in a holding tray using random numbers. One Ceriodaphnia neonate (20-24 hours old) was placed in each of ten replicate test chambers per test solution using the assigned positions All test chambers, contained in their holding trays, were placed in the water bath. The number of surviving Cenodaphnia in each test concentration was determined prior to test solution renewal. Dead Cenodaphnia were discarded. Test solutions were renewed daily by transferring each of the original Cenodaphnia into freshly, prepared t Q d ^ t e s t solutions. The number of Ceriodaphnia neonates, reproduced by the adult female Ceriodaphnia in each replicate test chamber, was counted and recorded at each daily test solution renewal time In the chronic test, Cenodaphnia were fed 0.1 mL of a concentrated suspension (approximately 3.1 x 107cells) of algae and 0.1 mLofYCT food mixturg daily, attest solution renewal time. Cenodaphnia were exposed to ambient laboratory light (50- Page 7 60175 Company Sanitized. Does not contain TSCA CBi 100 foot candles, measured at water surface) for a 16-hour day/8` h ^ photoperiod with transitional lighting Transitional lighting (30 minutes, 30-40 foot candles) was Included at the beginning and end of the 16-hour hght pe^no _ Temperature was maintained at 25C 1C by placing the tes c constant temperature water bath. For the fathead minnow chronic test, beakers (glass; 600 m L )filled ^ 2| ^ ,f test solution were used. Ten fathead minnow larvae, 1-20 hours old, placed in each of four replicate test chambers per test solution using random test chambers were positioned in the water bath using randomization techrnques The number of surviving larvae in each chamber was determined p n o jo test solution renewal. Dead larvae were discarded. Test solutions were renewed daily by siphoning approximately 80% of the test solution out o f t t e chamber lhe original test volume was restored by adding freshly p re p a re d ^ !s o lu tio n s to tne test chambers. 2.4.2 Toxicity Ranae-Findina Tests th e initial phase of testing consisjed o j a series of 48-hour range-finding tests to determine the general toxicity of f i ^ v e r a wide range of te s tc ^ e n tra tio n s Targeted test solutions ranged from 0.01 mg/L to 1,000 mg/L o f^ ^ H p the results of t h e f jjf t o lu b ilit y determination, an initial concentration se oe^/as selected to perform the toxicity range-finding tests. Since the solubility water was estimated at 6 mg/L, the initial toxicity range-finding tests were performed using a dilution series consisting of control, 0.01 mg/L, 0.1 mg/L, 1 mg , an 5 mg/L of f M B Since no evidence of toxicity was observed at these levelM he dilution senes was expanded to include targetoilO O mg/L^^TPOO mg/ | concentrations. To enhance the solubility o f { 0 p f n water, p a u s e d to prepare test concentrations greater than 6 mg/L was initially mixed with 500 A. ot reagen grade methanol; this mixture was then added to moderately hard water to prepare the test solutions. 2.4.3 Acute Toxicity Testing The second phase of testing involved the performance of 48-hour static acute Cenodaphnia dubia and fathead minnow tests. Based on the results of the toxicity range-finding tests, a concentration serjgs consisting of control, 200 mg/U 300 mg/L, 400 mg/L, and 500 mg/L o 0 t N a s used. The highest t a r a e t e d f ^ ^ concentration used in testing was at 500rng/L since, above 500 m g /L ,^ |^ p ii no appear to remain in solution. At concentrations greater than 500 mg/L sma droplets o fJ M fc v e re observed adhenng to the glassware used to prepare the test solutions. Ar^dditional control solution consisting of 500 A. methanol/L of dilution water was included in testing to identify any potential toxicity associated with the presence of methanol in solution. Based on the available toxicity data on met ano Page 8 60175 Company Sanitized. Does not contain TSCA CB! (EPA documents: EPA-600/6-91/005 and EPA/600/6-91/003), the concentration of methanol in the test solutions (0 05%) was well below the expected toxic levels (i.e., 2% to 5% for acute toxicity and 0 3% to 0 5% for chronic toxicity) B test solutions were prepared by first dissolving the pre-measured volume of concentrate in 500 u Lj A m&thanol pnor to mixing in the dilution water The measured concentrations o iQ ^ P jn test solutions were based on a specific gravity of 1.4 as noted on the m atenal^gM ^ data sheet provided with the sample The acute test dilution series and 9 N v est solution preparations are summarized below. Test Solution (m g /lfp l Control Control with Methanol 200 300 400 500 Volume o | J J /1 0 0 0 mL DilutSnWater None None 142 A213 L 284 fiL 355 A 2.4.4 Chronic Toxicity Testing The third phase of testing involved the performance of the static renewal Ceriodaphnia dubia and fathead minnow tests. Based on the results of the acute toxicity tests, a dilution senes consisting o fc o n to l, 5 mg/L, 10 mg/L, 25 mg/L, 50 mg/L, 100 mg/L, and 500 mg/L of targeted5 ^P concen*:ra^Gns were used for the chronic testing An additional control solution consisting of 500 A- of methanol/L of dilution water was included in testing to serve as a second control for determinations of potential toxicity associated with the p re s e n c ^f methanol in test solutions Methanol was used as a solvent medium fo n B iB p n o r to mixing of S l V w i t h dilution water and preparation o f test solutions. Test solutions were prepared at test initiation and daily chronic test solution renewals. A 100 mg/L stock usedto prepare the 5 mg/L, 10 mg/L, 25 mg/L, and 50 m g / L ^ U ^ e s t solutions, j p ^ f t t o c k solutions were measured volumetrically, dissolved in 500 fA. of pure methanol, and added to premeasured volumes of dilution water. The solutions were gently mixed in a separatory funnel prior to use. Page 9 60175 Company Sanitized. Does not contain TSCA CBI Test Concentration Control Control with Methanol 5 10 25 50 100 500 Volume o fl^ R lO O O mL dilution water None None 5 mL of 100 m g /U fc ^ o lu tio n 10 mL of 100 m gAJB B P solution 25 mL of 100 m g /L |s o lu tio n * 50 mL of 100 m g / L ^ d solution 71 p L 355 p L 2.5 Statistical Analysis In light of the analytical difficulties p r e s e n te ^ D ^ B jJ I all statistical analyses of acute and chronic test data were based on ta rg e te d (U p te s t concentrations. Insufficient mortalities occurred in the acute toxicity tests to calculate an LCX. Mortality per test concentration was reported, and the LC ^ values were approximated based on the highest test solution used. Statistical analysis procedures described in EPA/600/4-91/002 were used with Toxstat Version 3.5 to perform statistical analyses for the Ceriodaphnia and fathead minnow chronic tests. For the Cenodaphnia chronic test, survival was analyzed first using Fisher's Exact Test. Normality of distnbution and homogeneity of vanance for the reproduction data were next checked with the Shapiro Wilk's or Chi-Square Tests and Bartlett's Test, respectively. ANOVA and Dunnett's Test or Steel's Many-One Rank Test were used to evaluate reproduction. Any Cenodaphnia test replicates identified as males were excluded from the reproduction data analyses as per EPA guidelines. For the fathead minnow chronic test, data were transformed using the arc sine [square root (y)] transformation. Survival was analyzed first. Normality of distnbution and homogeneity of variance were next checked with Shapiro-Wilks and Bartlett's Test, respectively ANOVA and Dunnett's Test or Steel's Many-One Rank Test were used to evaluate mortality and growth. If any test concentrations showed statistically significant mortalities, they were excluded from the growth data analyses For statistical analyses of growth data, average growth of the organisms was based on the onginai number of larvae, as per EPA method guidelines. s- Page 10 60175 Company Sanitized. Does not contain TSCA CBl Two sets of data analyses were perform e^or the chronic toxicity tests. Test organism survival and reproduction or growth in th e M ((p e s t solutions were statistically compared to both the standard control group (with no added methanol) and the methanol control group. RESULTS Attempts to determine the water solubility o approach given in the test protocol that is included in Appendix 2. In t as received from DuPont - was equilibrated with deionized water in a separato^^anel. After phase separation, an aliquot of the aqueous phase was analyzed for B P ^ c o n te n t by purge and trap gas chromatographic/mass spectrometric (GC/MS) techniques. The analytical system used for all determinations consisted of a Tekmar Model 3000 purge and trap concentrator interfaced to a Hewlett Packard Model 58^^G C , and a VG Trio I mass spectrometer Calibration ^ n d a rd s consisted of samples o f B H p in Moratory pure deionised water c o n ta in in g iB ^ concentrations of 80, 40, 20, 8.474 2, and 2.1 g/L. The standards were prepared by cauefullv adding to 25.0 mL of water appropriate quantities of a stock^solujjpn c o n ta in m g p B j^ t a concentration of 40 g/mL in methanol. To minimize loss o n p B R y evaporation, the standards were prepared in purge and trap test tubes which were secured to the Tekmar purge and trap unit immediately after preparation. Based on the chromatographic results obtained during calibration, H a p p e a re d to consist of a mixture of three poorly resolved constituents eluting witivci retention time of between 4.0 and 4.1 minutes. Mass spectra for each o f the constituents were virtually identical in that they exhibited prominent peaks, in decreasing order of intensity, at mass to charge ratios of 77 (100% intensity), 51 (26% intensity), and 69 (14% intensity) Raw data illustrating a typical chromatogram and mass spectrum are included in Appendix 3 Also included in Appendix 3 is the derived calibration curve, which proved to be linear with a coefficient of determination of 0.991. Samples of^ B J ^ a t u rated water were analyzed fo r^ P B ^ io n te n t on 11 separate occasions, over the course of three separate days. Eaclymn was preceded by the analysis of a mid-point calibration standard containing ( f l B at a concentration of 0.040 mg/L. Recoveries of the standard ranged from a low of 0.037 mg/L to a high of 0.052 mg/L, and averaged 0.046 mg/L (115% of theory). For reason that are not immediately obvious, the results for thp^pBPsaturated water solutions proved to be poorly reproducible, ranging from a minimum value of 1.15 mg/L to a maximum of 16.7 mg/L. For the entire set of 11 determinations, the average was found to be 6.14 mg/L, with a standard deviation of 5.33 mg/L. Page 11 50175 Company Sanitized. Does not contain TSCACBi It is equally puzzling to note that the chromatogram obtained for th d jP js a iu ra te d water solutions was different from that obtained during the analysis of theTalibration standards Whereas th e J fc e a k had onginally appeared as a poorly resolved triplet the peak for the saturated water solutions took on the appearance of a well-resolved doublet, with one peak eluting at a retention time of approximately 3 6 minutes, and the second with a retention time of 4 1 minutes. Again, mass spectra for the peaks were virtually identical Although it amounts to little more than speculation, possible explanations for the observed behav'ior of in water .in...c..l.u..d..e...t..h..e...f.o..l.lowing: 1. f l B r l a y possess sufficient surface activity to form micellar solutions If so,___ _ m a ^e n d to form monomolecular layers at the air/water interface and/or at the water/glass interface, making it difficult to withdraw representative samples from the bulk "solutions" for analysis. 2. _ nay be sufficiently reactive to undergo degradation (or polymenzation) in the Feafed inlet of the gas chromatograph. If this were the case, it would not be surprising to see multiple peaks of vanable intensity. 3 ' Focusing finally on the different peak patterns, and noting that the standards (which appeared as triplets) were analyzed immediately after preparation, whereas the 4B M 0saturated water samples (which appeared as well-res^/^Ldoublets) had ^ 2cTfor up to several days prior to analysis, it may be t h a t m ^ i s undergoing some unspecified sort of time dependent chemical transformation when allowed to equilibrate with water. Despite the unusual properties exhibited b y H p n water, it can be concluded with a high degree of certainty that its solubility is extremely low, most likely on the order of 10 mg/L or less., 2.0 i^ ^ ^ P 'o x ic ity Determination 2.1 Toxicity Range-Finding All data generated for the toxicity range-finding tests are included in Appendix 4. The results indicated no acute toxicity to fathead minnows and Cenodaphnia at targeted concentrations ranging from 10 mg/L to 1,000 mg/L ( ^ L ^ ^ concentration may be less than 1,000 mg/L due to apparent accumulation on glassware) Toxicity data for these tests are summarized in Table 1 2.2 Acute Toxicity Testing All data generated for the acute toxicity tests are included in Appendix 5 The results indicated no acute toxicity to fathead minnows and Cenodaphnia a1| Page 12 S0175 Company Sanitized. Does not contain TSCA CBI TABLE 1 TOXICITY RANGE-FINDING DATA SUMMARY Test Concentration*1' (m g /L ^ H Control*2' 0 01 0.1 10 ........ 5 0 100 1,000*3> Toxicity End-Point*'1' Percent Survival Cenodaphnia 24-Hour 48-Hour 100 100 100 100 100 100 100 100 100 100 Fathead Minnow 24-Hour 48-Hour 100 100 100 TOO 100 100 100 100 100 100 100 100 100 100 100 100 100 100 LCkj >1,000 mg/L LCso >1,000 mg/L Notes 1 Targeted test concentrations. 2. Control consisted of EPA m oderately hard water and contained n o p | j | 3 Actual^BBPconcentration may be less than 1,000 mg/L based on appearance of f-esidual on glassware used to prepare test solution. . 4. LC50 values estim ated based on test organism response in highest targeted test solution. Job Number 60175 April 20, 2001 Company Sanitized. Does not contain TSCA CBi 13 Q j r p> laboratories concentrations ranging from 200 mg/L to 500 mg/L. The sur/ival of Cenodaphnta in the methanoi co n tro ^'0% survival) was reduced relative to the standard control (100% survival) ^ndp^QJ^test solutions (90% - 100% survival). No reason for this reduction in survival was identified. The results are summarized in T a b le ^ ^ ^ ^ _ depicted, the LCH values for both tests were estimated based on the h i g h e s t f ^ ^ test solution used and are reported as greater than (>) 500 mg/L. 2.3 Chronic Toxicity Testing ^ All data generated for the chronic toxicity tests are included in Appendices 6 and 7 and the test results are summarized in Tables 3 and 4. Statisticall^^^^iead minnow survival and growth were not significantly reduced by exposure to ^ ^ B te s t concentrations ranging from 5 to 500 mg/L. This was consistent for comparisons to standard laboratory water (no methanol) controls as well as comparisons to control water spiked with 500 iA. methanol. The no observed effect concentration (NOEC) value for this test Was based on the highest test concentration used and is reported as NOEC = 500 mg/L. No unusual behavior was observed by control larvae in the dilution water controls and dilution water with methanol controls. i jn t h ^Ceriodaphnia chronic test, survival was significantly reduced in the 500 mg/L J jjB s o n c e n tra tio n (40% survival) Ceriodaphnia survival and reproduction data were statistically analyzed by comparing the survival and reproduction in each test concentration to the standard control group (with no methanol added) (Table 3) and to the methanol control group (Table 4)^A^tetistically significant reduction in reproduction was observed at the 25 mg/LJ ^ J p e s t concentration when the data were compared to the standard control group, resulting in a non-continuous dosedependent toxicity response In accordance with standard EPA chronic test data evaluationprocedures, the NOEC value for this test may be defined as 10 mg/L, the h ig h e s ^jH c o n c e n tra tio n under the lowest statistically significant concentration (25 mg/L). Alternatively, test organism reproduction at the 25 mg/L concentration may be considered aberrant and the NOEC may be defined as 100 mg/L, based on improved reproduction (relative to the 25 mg/L concentration) in the 50 mg/L and 100 mg/L test concentrations The reproduction data analyses s t a j ^ n o statistically significant reduction in reproduction in the 100 mg/L and low ei^B JP est concentrations when the data were compared to the methanol-spiked control group (Table 4). The NOEC value for the test when compared to the methanol-spiked control was 100 mg/L. In light of test organism reproduction reproduction in the 5 mg/L, 10 mg/L, 50 mg/L, and 100 mg/L test concentrations, the NOEC for Ceriodaphnia is believed to be 100 mg/L. Page 14 6D175 Company Sanitized. Does not contain TSCA CBI TABLE 2 ACUTE TOXICITY DATA SUMMARY Test Concentrati^1 Control121 Control wtth MethanolP) 200 300 400 ______ __L------ ----- 5,00 Toxicity End- Point*41 Percent Survival Cenodaphma 24-Hour 48-Hour 100 100 100 70 Fathead Minnow 24-Hour 48-Hour 95 95 100 100 100 100 100 100 LCjo >500 mg/L 95 100 90 95 LCm >500 mg/L 100 100 100 100 LC50 >500 mg/L 100 100 100 . 100 LC-*, >500 mg/L Notes. 1. Targeted test concentrations. 2. Control consisted of EPA moderately hard water and contained n o p j j | 3. Control consisted of EPA moderately hard water and contained 500 (A. methanol/L and 4. LCsqvalues estimated based on test organism response in highest targeted test solution. Job Number 60175 May 3. 2001 15 Company Sanitized. Does not contain TSCA CBI OLVER la b o r a to r ie s TABLE 3 Test C o n c e n ta to ^ 1' (m g /L ^9 Control*2' 5 10 . 25 50 100 i 500 Toxicity End Points CHRONIC TOXICITY DATA SUMMARY COMPARISON TO STANDARD CONTROLS Toxicity Test Results Cenodaphma Fathead Minnow Percent Survival 100 Average Reproduction 18 0 Percent Survival 98 Average Growth (mg) 0 420 100 16 6 98 0 468 90 17 1 95 0 416 90 13.9-P) 95 0.430 70 . 152 100 0.442 70 172 100 0.399- 40*ct NAW 98 0.422 NOEC - Survival = 100 mg/L NOEC - Reproduction = 100 mg/L*5) IC2S- Reproduction >500 mg/L(6) NOEC - Survival = 500 mg/L NOEC - Growth = 500 mg/L IC25- Growth >500 mg/L|5) Notes- 1. Targeted test concentrations. 2. Control consisted of EPA moderately hard water and contained 3. Asterisks (*) indicates a statistically significant reduction in survival and/or reproduction as compared to the control group. 4. Not Applicable. Since test organism survival at this concentration was significantly reduced relative to the control group, reproduction data was not included in the reproduction analysis. 5. Reduction test organism reproduction at the 25 mg/L concentration considered abberant. NOEC reproduction value based on test organism reproduction in 100 mg/L concentration. 6. IC25values estimated based on test organism response in highest targeted test solution. Job Number 60175 Company Sanitized. Does not contain TSCA CBI OLVER la b o r ato r ie s TABLE 4 CHRONIC TOXICITY DATA SUMMARY COMPARISON TO METHANOL-SPIKED CONTROLS Toxicity Test Results Test Concentetia^' i m a* /1L W^ --Control with Methanol 5 10 25 Cenodaphnia Percent Survival 90 Average Reproduction 14 3 100 16 6 90 17 1 90 13 9 70 15 2 oin 100 70 500 40*(3) 172 NAW Toxicity End Points NO EC - Survival = 100 mg/L NOEC - Reproduction = 100 mg/L IC,5- Reproduction >500 mg/Lt5> Fathead t/linnow Survival Average Growth (mg) 95 0 407 98 0.468 95 0.416 95 0 430 100 0 442' 100 0 399 98 0 422 NOEC - Survival = 500 mg/L NOEC - Growth = 500 mg/L IC,5- Growth >500 mg/L Notes: 1 . Targeted test concentrations. 2. Control i n sisted of EPA moderately hard water and contained 500 A. methanol/L and nom m ' Asterisks (*) indicates a statistically significant reduction in survival and/or reproduction as compared to the control group. 4. Not Applicable. Since test organism survival at this concentration was significantly reduced relative to the control group, reproduction data was not included in the reproduction analysis. 5. IC25values estimated based on test organism response in highest targeted test solution. Job Number 60175 May 3, 2001 17 Company Sanitized. Does not contain TSCA CB1 OLVER labo r ato r ies Ji APPENDIX 1 MATERIAL SAFETY DATA SHEET Company Sanitized. Does not contain TSCA CB! OLVER la b o r a t o r ie s T iie MSDS format adheres to the standards and regulatory r e q u i r e m e n t s * of the United States and may not meet regulatory requirements in other countries. DuPont Material Safety Data Sheet Page 1 DU004S04 IFLUOROTELOMER INTERMEDIATE Ivisad 12-JAN-1999 CHEMICAL PRODUCT/COMPANY IDENTIFICATION Material Identification M is a registered trademark of DuPont. Company Identification MANUFACTURER/DISTRIBUTOR DuPont 1007 Market Street Wilmington, DE 19898 piONE NUMBERS , Product Information Transport Emergency Medical Emergency : 1-800-441-7515 : CHEMTREC 1-800-424-9300 : 1-B00-441-3637 HAZARDS IDENTIFICATION Potential Health Effects Eye contact may cause eye irritation with discomfort, tearing or blurring of vision. Based on related products, inhalation of spray or mist may cause ^ nasal, throat, or dung irritation. Inhalation of large amounts of respirable particles may be toxic to the lungs. Symptoms may be modest initially, followed in hours b y severe shortness of hreath requiring prompt medical attention. Carcinogenicity Information None of the components present in this material at concentrations ^ equal to or greater than 0 .1% are listed by IARC, NTP, OSKA or ASGIH as a carcinogen. 19 Company Sanitized. Does not contain TSCA CBI DU004604 DuPont M a te r ia l S a fe ty D a ta S h e e t Page 2 yyjtST AID MEASURES First Aid INHALATION If inhaled, remove to fresh artificial respiration. If air. If not breathing, breathing is difficult. give give oxygen Call a physician. SKIN CONTACT Flush skin with water after contact. before reuse. Wash contaminated clothing EXE CONTACT In case of contact, immediately flush^eyes with plenty of water for at least 15 minutes. Call a physician. INGESTION If of swallowed, do water. Never not induce vomiting. Immediately gave 2 give anything by mouth to an unconscious glasses person. Call a physician. Notes to Physicians Activated charcoal mixture may be administered. To prepare , activated charcoal mixture, suspend 50 grams activated charcoal m 400 mL water and mix thoroughly. Administer 5 mL/kg, or 3 for an average adult. -Y33BHS" "FIGHTING M E A S U R E S ________ Flammable Properties Flash Point Method : Does not ignite = PMCC Hazardous decomposition products including carbon dioxide, carbon monoxide, hydrogen fluoride, toxic gases or particles may be formed during combustion. These products may cause severe eye, nose, throat, and lung irritation or toxic effects. Extinguishing Media Water Spray, Foam, Dry- Chemical, C 02. Fire Fighting Instructions Wear self-contained breathing apparatus. Wear full protective., equipment. Company Sanitized, Does not contain TSCA CBt DU004604 DuPont Material Safety Data Sheet (FIRS FIGHTING MEASURES - Continued) Avoid breathing decomposition products Page 3 ACCIDENTAL RELEASE MEASURES _ ______ ;________ S a f e g u a r d s (Personnel) NOTE: Review FIRE FIGHTING MEASURES and HANDLING (PERSONNEL) sections before proceeding with, clean-up. Use approprxa e PERSONAL PROTECTIVE EQUIPMENT during clean-up. Spill Clean Up SoaX up with sawdust, sand, oil dry or other absorbent material.. Shovel or sweep up. Accidental Release Measures Flush spill area with water. _ _______________________________________________________ handling and storage _ _ _ ________________ Handling (Personnel) Avoid contact with eyes. Wash thoroughly after handling. Do not store or consume food, drink, or tobacco in areas where they may become contaminated with this material. Avoid circumstances a produce respirable particles unless suitable ventilation and respirator are used. Storage -"Keep container tightly closed. Keep away from open flames and heated surfaces above 20 0 degrees C (392 deg F) . e x p o s u r e c o n t r o l s /p e r s o n a l p r o t e c t i o n ____ ______ Engineering Controls Keep container tightly closed. Use only with adequate ventilation Vent heated extruder or dryer fumes outside work area. Do not aerosolize. In spray applications, use airless type pressure spray equipment at less than SO psi, and exhaust ducts, drxp pans, m r other design features to minimize worker exposure to m a t s and overspray. Keep away from open flames and heated surfaces above 20 0 degC (392 degF). 21 Company Sanitized. Does not contain TSCA CBI DU0Q46Q4 DuPont M a te r ia l S a fe ty D a ta S heet Page (EXPOSURE CONTROLS/PERSONAE PROTECTION - Continued) 4 Personal Protective Equipment EYE/FACE PROTECTION Wear safety galsses or coverall chemical splash goggles. RESPIRATORS Wear NIOSH approved respiratory protection as appropriate. PROTECTIVE CLOTHING Where there is potential for skin contact have available and wear: as appropriate, impervious gloves, apron, pants. and jachat - Exposure Guidelines Applicable Exposure Limits Perfluorobutyle thylene PEL (OSHA) TLV (ACGIH) kEL *(DuPont) : None Established : None Established : 100 ppm, B Hr. TWA * AEL is DuPont's Acceptable Exposure Limit. Where govemmentally imposed occupational exposure limits which are lower than the are in effect, such limits shall take precedence. Exposure G u i d e l i n e Comm e n t s No AEL has been established for this product. Other products with fluorinated material components have an AEL of 0.1 mg/3 to 1 mg/m3 (8 hour TWA) for respirable size aerosol particles. Air monitoring studies conducted at customer sites indicates tbat the use of the recommended low pressure (less than 60 psi) airless type, garden type or deck_ specific hand pump sprayer with spray tip orifice minimum of 0-031 inches in diameter does not produce respirable size aerosol particle concentrations near the AEL. " PHYSICAL AND CHEMICAL PROPERTIES Physical Data Boiling Point % Volatiles Solubility in Water Odor Form Color Specific Gravity 58 C (136 F) 0 7S O m m Hg 100 WT^s Negligible Ethereal Liquid, Clear Colorless 1.4 Company Sanitized. Bgps not contain TSCA CBl DUO04604 DuPont M a te r ia l S a fe ty D a ta S h e e t Page 5 STABILITY AND REACTIVITY Chemical Stability Stable at normal temperatures and storage conditions. Incompatibility with Other Materials None reasonably foreseeable. Decomposition Hazardous decomposition products including carbon dioxide, carbon monoxide, hydrogen fluoride, toxic gases or particles may be formed during combustion. These products may cause Bevere eye, nose, throat, and lung irritation or toxic effects. Polymerization Homopolymerizati'on will not occur. Copolymerization can occur in the presence of free radical sources, heat or UV light. TOXICOLOGICAL INFORMATION Animal Data Inhalation 1 hour ALC: Oral LD5Q: >7,178 ppm in mice >25,000 mg/kg in rats The product is not a skin irritant, is a mild eye irritant, and is untested for skin sensitization in anima ls. Repeated exposure to high levels (5 vol^) produced blood changes (decreased -platelets and increased monocyte) . Tests in animals demonstrate no developmental toxicity. The product does not produce genetic damage in bacterial cell cultures but has not been tested in animals. Tests for carcinogenic and reproductive activity have not been performed. DISPOSAL CONSIDERATIONS Waste Disposal " Treatment, storage, transportation, and disposal must be in accordance with applicable Federal, State/Provincial, and Local regulations. 23 Company Sanftfceef. Does not contain TSCA CBf DUO 04 604 D uP ont M a te r ia l S a fe ty D a ta S heet Page 6 TRANSPORTATION INFORMATION _ Shipping Information Not R e g u l a t e d as a hazardous m a t e r i a l by DOT, IMO, or IATA REGULATORY INFORMATION U .S . F e d e r a l R e g u l a t i o n s TSCA Inventory Status : Reported/Included. TITLE III HAZARD CLASSIFICATIONS SECTIONS 311, 312 Acute : Yes Chronic : No Fire : No Reactivity : No Pressure : No l ____ _______ _ ______________________ OTHER INFORMATION NFPA, NPCA-HMIS NFCA-HMIS Rating Health Flammability Reactivity :1 :0 :0 Personal Protection rating to be supplied by user depending on use conditions. The d a t a in this M a t e r i a l S a f e t y Data Sheet relates only to the^ specific material designated herein and does not relate to use in combination with any other material or in any process. Responsibility for MSDS : MSDS Coordinator _ Address : DuPont Chemical Solutions Enterprise ' Wilmington, De. 19838 Telephone : 800--441--7515 # Indicates updated section. T h i s i n f o r m a t i o n is b a s e d u p o n t e c h n i c a l i n f o r m a t i o n b e l i e v e d to b e reliable. It is s u b j e c t to r e v i s i o n as a d d i t i o n a l k n o w l e d g e and. experience is gained. End of MSDS 24 Company Sanitized. Does not contain TSCA CBI APPENDIX 2 SOLUBILITY DETERMINATION M TEST PROTOCOL 25 Company Sanitized. Does not contain TSCACBI OLVER laboratories Test Protocol for Determining, the Solubility of in Water 1 Obtain sample of authentic product from DuPont. No more than 100 mL should be required 2 Calibrate the GC/MS system using samples of the authentic product. At the same time, determine a R R F J o n fliP n relation to an internal standard having a retention time similar to that o f H ^ s m c e f lM B is claimed to exhibit negligible solubility in water, prepare calibration standards b^nssolving carefully weighed quantities of the product as received in a suitable solvent Methanol is suggested. The calibration curve should be constructed using a minimum of four, and preferably five, calibration standards 3 Equilibrate] with laboratory pure water as follows a Place approximately 25 mL of the product as received in a clean 2L separatory funnel. Add 1L of laboratory pure water c Shake vigorously to intimately mix the two phases, venting to atmosphere as needed to relieve pressure Allow the phases to separate, then repeat both steps a minimum of five (5) times d After mixing, allow the funnel and its contents to stand undisturbed overnight (to ensure complete phase separation) e Remove a portion of the aqueous phase (upper phase) using a clean transfer pipet Place the sample in a 40 mL VOA vna^^iuipped with a Teflon-lined cap Makeihe transfer quickly to avoid loss o tflH ^ to the atmosphere When full, seal the vial with its cap such that zero haraspace exists after the cap is secured Prepare three such vials for subsequent analysis f After removing analytical samples, measure and record, i) temperature of the aqueous phase, and n) atmospheric pressure 4 Analyze all three samples for the presence Quantify concentration in units of mg/L relative to the calibration curve and RRF, as determined in Step 2 Safety Considerations The toxicity o f ^ J H although not believed to be high, has not been well-defined All prepara tive steps should tKe place in a hood Standard and customary measures should be taken to guard against skin and eye contact. Should contact occur, follow the procedures outlined in the attached MSDS ?c C o m p a n y Sanitized. D o e s not contain TSCA C B APPENDIX 3 SOLUBILITY DETERMINATION ANALYTICAL DATA 27 Company Sanitized. Does not contain TSCA CB1 OLVER LABORATORIES File . c \V 012 201 ',700122 02 Operator Acauired : BP : 22 JAN 1 9 .02 Instrument Trio-1 Sample Namme: 1000 NG STD Mise Info : 25mls Vial Number : 0 D using Abundance 110000 TIC V 0012202.D C u r A i o&?a h /CETUt r" (jT riP K iT Y J ov Tim e-> 3 00 3 20 P 3 40 II -- 3 6 0 3 BO ............1' I '----!,T-.-TTT| I n i -r 4 00 4 20 4 40 4 60 4 80 5 00 r-r-i-- -i--1I 111r 1' ` ' I 5 20 5 40 5 60 5 80 6 00 4,bun0ance Scan 49 0 (4 083 min) V0012202 0 77 25000 20000 15000 10000 50001 69 t i/z - > 44 : o ' l ' : i I i ' 30 40 50 57 100 . I ,108 , : i'l 'l - r - l - M-p ----- ,-------1 i----- 1 * j-i 6 0 70 BO 9 0 10 0 11 0 157 __ 181 207 I_, I,119 127 145 I !6 3 i--,*----r-4,------ n ----- r - 1, . j I . | .`i-nj - ----- T ----- I- ' P r P ~ 120 130 140 150 160 170 180 190-- 200-- 210_ 28 Company Sanitized. Does not contain TSCA CBi Response Rateo 14- 12- 10-J J 6- / ~' " I ' 2 Amount Ratio Resp Ratio = 3.49e+000 * Amt + 1.33e+000 Coef of Det (r*2) = 0.991 Curve Fit: Linear Method Name: C :\V012 5 0 1 ^ ^ B 2 .M " Calibration Table Last Updated: Wed Jan 24 07:52:06 2 Company Sanitized. Does not contain TSCA CBI 29 Fils Operator Acquired Instrument Sample Name Misc Info Vial Number C : \ HFCKEM\1 \DATA\VO 119 C1 \VO C119 0 3 . D BP 1.9 JAN 1 1 3 :4 5 u s in g AcqMethcd TriQ25 ML 2 5m ls 0 H20 EXTRACT ^ oloV ^ O f 30 Company Sanitized. Does not contain TSCA CB1 File Operator Acquired Instrument Sample Name Mise Info Vial Number C .\H?CHEM\1\DATA\VO 1 1 901\VO 0119 Q8.D EP 19 JAN 1 13:45 using AcqMethod Tr 25 ML H20 EXTRACT 25mls 0 Scan 498 (4 15 0 min) V 0 0 1 1908 D fjh iS n e u H oF 1 m /z- > CD O O 207 108 131 157 181 93 t , 145 U'' I " " l .... 1 " ' I` 1A'-''T11 "I" ''' ,- r - 4' IT-'X' ' I . ' " I'1--I-P'P'" ' , I 1-6'I9' ' 227 1' 8` 8I 1191'5 219 ` JU 1' : 30 40 5 0 60 70 80 90 1C0 110 120 130 140 150 160 170 18 0 190 2 0 0 210 220 2 j 0 31 Company Sanitized. Does not contain TSCA CBI I APPENDIX 4 TOXICITY RANGE-FINDING TEST DATA 32 Company Sanitized. Does not contain TSCA CB1 OLVER LABORATORIES I K Company Sanitized. Does not contain TSCA CB! OLVER LABORATORIES INCORPORATED ENVIRONMENTAL BIOLOGY LABORATORY TEST SUMMARY SHEET CLIENT TOXICANT/EFFLUENT JOB NO on S PERMIT NO v/A PAGE I OF l TP C T DATC"^ ACUTE TOXICITY TEST RESULTS Cenodaphma l/z5 - | / z . l) o 1 Fathead Minnow 1/2._ Id CHRONIC IO X IC IIY T EST RESULTS Cenodaphma Fathead Minnow TFRT CONDITIONS TEST ORGANISM AGE DILUTION WATER SOURCE AERATION aJ TEST ACCEPTABILITY CONTROL SURVIVAL (a90%) F P A -M H W OLVER LABS conlinuous loo/. 2. J ams EPA-MHW Ol VER LABS conlinuous Io n / TEST ORGANISM AGE DILUTION WATER SOURCE AERATION CONTROL SURVIVAL (80%) NO OF CONTROL FEMALES % CONTROL FEMALES WITH 3 BROODS (60%) EPA-MHW OLVER LABS continuous EPA-MHW Ol VER LABS continuous AVE NO YOUNG/SURVIVING FEMALES (15) STATISTICAL RESULTS SURVIVAL IN 100% L C 50 95% C I METHOD . loo/ >5 m3 h . fJD * MD AVE W T/SURV CONTROL (0 25 mg) 1O/. > 6 mA/t- MD ND SURVIVAL IN HIGHEST ( ) CONC NUMBER OF REPLICATES NUMBER OF ORGANISM/REPLICATE NORMAL DISTRIBUTION? HOMOGENEOUS VARIANCE? NOEC METHOD NOEC SURVIVAL NOEC REPRODUCTION/GROWTH SG SG SG COMMENTS f ivlDa. NrvF (_ vu. -`ro |n.So.fKQ<jrV Il UEMPLATErDIODENCIMlIOADMIMTESTSUM WPD Revised March 21. 2001 \ Company Sanitized. Does not contain TSCA CB1 OLVER LABORATORIES INCORPORATED ENVIRONMENTAL BIOLOGY LABORATORY CLIENT I W c u f t * TOXICANT/EFFLUENT TEST SUMMARY SHEET JOB NO Io l~l5____________ PAGE O F ... L PERMIT NO M/A _____________________ __ ______ ACUTE TOXICITY TEST RESULTS Cenodaphnia Falhead Minnow CHRONIC TOXICITY TEST RESULTS Cenodaphnia TFST DATFfS^ z/i -T -I'slo l 4 /l-W lo l TEST CONDITIONS TEST ORGANISM AGE DILUTION WATER SOURCE AERATION U3 TEST ACCEPTABILITY CONTROL SURVIVAL (>90%) /. ^ 4 VOouvs EPA-MI-IW OLVER LABS conlinuous 1n i l / . 1 EPA-MHW OLVER LABS conlinuous - In n '/ TEST ORGANISM AGE DILUTION WATER SOURCE AERATION CONTROL SURVIVAL (*80%) NO OF CONTROL FEMALES % CONTROL FEMALES WITH 3 BROODS (*60%) EPA-MHW OLVER LABS conlinuous Falhead Minnow EPA-MHW Ol VER LABS conlinuous STATISTICAL RESULTS SURVIVAL IN 100% C H ^Vve v t C v i c } 1r qs% n i METHOD ` lo o -/. > loo N)t rD-v "fc ro D AVE NO YOUNG/SURVIVING FEMALES (*15) AVE W T/SURV CONTROL (*0 25 mg) Ion/. > InTM mpi/L. MD MD SURVIVAL IN HIGHEST ( ) CONC NUMBER OF REPLICATES NUMBER OF ORGANISM/REPLICATE NORMAL DISTRIBUTION? HOMOGENEOUS VARIANCE? NOEC METHOD NOEC SURVIVAL NOEC REPRODUCTION/GROWTH SG SG SG COMMENTS -fr MirE &*rkxrr.^<xU<L 7 V morkV-K^) I! rtEM I' LATE\UIOBEIICHWOADMIN\TESTSUMWPD R e vise d M arch 21, 2001 S a m p le In form alion C lie n t P la ^ o T : P erm it N o N/ ' T o xica n l/E fflu en t 5 m-jjL.I * S a m p le Typ e r3 7 a G r a b C o ll e c t e d __________A M / P M // C o m p o s ite C o llec te d F r o m ________ A M / P M (D ate) _J l_____ ______ ( D a t e ) T o ___________ A M / P M // (D ale) Job No (a o /~~75 S a m p le N o __ TR C ro /A m q /L In itial p H Initial D 0 N /A n /A m q /L A d ju s t m e n t s _______________ _ ^ TR3 I 4 .r . ACUTE TOXICITY TEST T e s t In fo rm atio n A n a ly s l( s ) S r r > ( J|?, rvj T e s t S p e c ie s P- rvom< tos C u ltu re N o _______ ___ A g e Z. d . ^ $ Length (s S D ) a h ~ 1 o . Q 5 W e ig h t ( r S D ) a.Mt o -3^ T est M ode S 'R h 'c . D ilu tio n W a te r & PA im u J Start of T e s t 1E n d o f e s t AM^ / l z 5/ of (D ate) L7r3^> A M aP m 1 foT) & 1 ( D a t e ) T e s t C o n ta in e r S iz e T e s t S o lu tio n V o lu m e < * 0 m u ____________ 'loo m e c M D is so lv e d O x y g e n (T im e /T e s t S o ln /C o n c ) A eratio n I L L J. L/ _____ _____ -------- -------- -- -------tJ/ A B eg in n in g D a te /T im e /R a le P h o lo p erio d 1 6 -h o u r day/O -h o u r night Cone or % 5 .0 n \ V c Rep A N u m b e r o f Live O rg an ism s 0 24 48 ID /C fO % S urvival D is so lv e d O x y g e n (m g /L ) 0 24 48 pH 0 24 48 JO o/ 7 -B 7P 7 7 i l - 7 , 7 T e m p e ra tu re (C ) 0 24 48 5 85* 37 In itial A lk alin ity (m g /L as C a C O J In itial H a id n e s s ( m g /L a s C a C 0 3) C o n d u ctivity L im h o s /c m ) In itia l/F in al 50 IO 0 3 )7 AI .0 Or\a)) L 10 / / o l o o ' / . 7 .? ? l.o T 7 n - 7 7 Z 5 2 5 3 5 rA T E Company Sanitized. Does not contain TSCA CBI 0 ' " W l_ A 10 / /O 0 6 / 7 -X -70 i . i 1 1 87 37 3/ A 10o o \ h /, i a/ o fo | /( 7 ,5 ? 7 ,o 7 -8 1----- "------------------ -- i n z 85~ \C a a - \ - r o A 1O 7 ^) o I 0 0 / 7 i t , 7 - 5 7 .7 - i n Z 5 f l S l . (pO A n a ly s t's Im li a ls /T im e T 75 / n L/h9r 4 ' loP'i 1h 5 ^ 5 )5/n Ln\D 5zr\ UMD H U 5m L-wO a N o te s C -i*-r 7^3 a 1 310 80 2^ Sj ; J_- l / . | j o | Condition o(Organisms atTest Imtialion/End H<ftV\VvM , Oorrocx) J \-l Q I }-h -- fl.Q_Cjarl.iL N \Tcmplales\UioDefich\acule\rOXTEST WPD OLVER LABORATORIES S a m p le In form atio n C ile n i rJn .iP r.n ~ t P erm it No N /.~ T o xican l/E tflu en l IS a m p le T y p e __ M G ra b C o llected C o m p o site C o llec te d F r o m ________ A M / P M T o ________ A M / P M A M /P M /__L (D ate) /______ ( D a l e ) /______ ( D a l e ) Job No , , S a m p le N o _____________ . TRC N /A m q /L In itial p H n / A ____________ In itial D O aj/ a m q /L A d ju s t m e n t s ___________ 4 ^ __________ CA I o -f' ACUTE TOXICITY TEST T e s t In fo rm a tio n liA n a ly s l( s ) 5<~n ; $ r J _______ C ic.T e s t S p e c ie s c A A a ________ C u ltu re N o Age z-\ W > Length (s S D ) N /A W e i g h t ( x S D ) ___ N / A Jest M ode 5 - H h c D ilu tio n W a te r & PA m H ixJ Q 0S ta rt o f T e s t _ -7 A M /) / /Z 5 / cl 7 / 5 ..E n d o t T e s t --------_ _ T e s t C o n ta in e r S ize ^ ) /9 7 l bl >0 i*nl'2-S m L. T e s t S olu tio n V o lu m e (D a le ) (D ale) D isso lve d O xygen (T im e /T e sl S o ln /C o n c) // 7 /______ L__ L A eratio n B e g in n in g D a le /T im e /R a le P h o lo p e rio d 1G -hour day/O -hour n iy h l Company Sanitized. Does not contain TSCA CBS C one or % 5 .0 rr'.S// Rep A p> N u m b e r o( Live O rganism s 0 24 48 5h cA 7 f % S urvival D is so lv e d O x y g e n (m g /L ) 0 24 48 pH 0 24 / O / T 7-8) 7 . 7 _lL_ n coT e m p e r a lu r e 48 0 24 48 1-3 75 2$ In itial A lk alin ity ( m g /L a s C a C 0 3) Initial H a rd n e s s ( m g /L a s C a C 0 3) C o n d u c tiv ity (/m ih o s /c m ) In itia l/F m al ( ? o /0 O 3 i2 S 3 / f /'" I1 .0v m i7WViL ' A 5 5 A t m.V, A P, *s A <r 5 ? / g o / h At 7 P q-h 7 7 7 .7 T 5 7 /D / 7-8 !(* 7 . 7 7-8 J 1 $ 2 5 OS 3 5 7 ? 1-3 2 S i S 75 31 s " X 0 O' A ------- ------- J-- & 5 I b b /' 7 .8 7 -u 7 7 7-8 5 s) 7 % 25 os 5 5 " UI A 6 A n a ly s t's Im i a ls /T im e 5 # 5 5 ? fo O '/ 7-8 7'U 5 o ^V 5HmIPch^ / ,,' T S I I n) Sffl SfJ 7-0 Srr) fl m S) S' 2 5 0-5 S/n S.I C o m m e n t s ~X A & . 9 'M L / 5 P ..A L iC o n d flio n of nmamsms a l Tesi In tlia lio n /E n d L \ 4 z J---- /M iL i................................................ ........... H, f *a \^Yv>i ,--9 0 r PO^^ j ft 11 --f \ i \ _n* o<1a crtl_Jii-*-,-f--r-h---?-- n nnparq / P ------- d "* /m n StrxJ "J s (p ^ r S' 3>i to^ s ~ /3 I( N o te s ( C c t T b 0[/l # 3 T A f i l / O l _i A o m > e/ / 0 4-ho. <<?ncJ Crr 't ~ M 7 ^ * N \Templ3 t05\BioOencH\arute\TOXTEST WPD OLVER. l a b o r a t o r ie s Company Sanitized. Does not contain TSCA CB1 S a m p le In fo rm atio n C lien t 'D 'a P P e r m i t N o _____ T o xica n l/E fflu en l S a m p l e T y p e ___ G r a b C o lle c t e d _________ A M / P M C o m p o s ite C o llec te d F r o m ________ A M / P M To A M /P M // (D ate) J ______ ( D a l e ) J ______ ( D a l e ) Job No (ooHS S a m p le N o TR C N /A m g /L Initial pH N /A Initial D 0 n /a m g /L A d ju stm en ts m /A p*> I o f \---------------- ACUTE TOXICITY TEST T e s t In fo rm a tio n A n a ly s l(s ) s m . S P iY o l IQ\S t a r t o f T e s t . S ' - o o A M / 6 0 ) / 0T e s t S p e c ie s 3 3 P iiA ________ E n d o f T e s t _. ____ ________ A M f r t v P C u ltu re N o J Lt o A i . , . U . u A C . i t W ^ T e s l C o n t a in e r S i z e _ 3 -------------l-Y-- ll (D ate ) (D a le ) Age . T e s t S o lu tio n V o lu m e Length (x S D ) W e ig h t (x S D ) Test Mode xi/A WA D isso lved O x y g e n (T im e /T e s l S o ln /C o n c ) // / / _ _ J ___L W t LA e r a tio n D ilu tio n W a te r B eg in n in g D a le /T im e /R a te .. /V /A P h o lo p e rio d 1 6 -h o u r d a y /8 -h o u r night Cone or % lo o o fm / Rep A & N u m b e r o f Live O rganism s 0 24 40 % S urvival D is so lv e d O x y g e n (m g /L ) 0 24 48 5 5 5 7 lo o / 7 -p i 7 - * 7 . ? 5 5 5^ pH 0 24 48 7 ? " 7.7 I S T e m p e ra tu re (C ) 0 24 48 In itial A lkalin ity ( m g /L a s C a C 0 3) a5 _S S l G>H Initial H a rd n e s s ( m g /L a s C a C 0 3) C o n d u c liv ity (n m h o s/cm ) in itia l/F m al I OO 539 \UU n / L A- E 5 5 5 it /Q 0 '/ 7 , I S 7 -t 7 .7 35 A b ------------ 1-- ^7 5 57 l o o / 7 8 7J 1? 5 5 IT I 7 . 7 1, (d zS 3 5 - 5 . 5 cL-J tZ _ 5 3 L -t 7 i s' A n a ly s t's Im li a ls /T im e rJ / T 3 D3Pd ^ P a t** 5 /r\ &rr\ S/n C om m ents ------------------------------------------------------------ --------------------------------------------_ _ _ _ _ ---------------- ------------------------------------------ C o n d itio n ol O rg a n ism s at T e s t Im liatio n /E n d I Q, O o r m u l .H C H ~ ^ Y , Q- l . N \fenipldlbf5\iuenc.lAdCulc\TOXTEST WPD N otes #3 V 2 i/oJ OLVER LABORATORIES Sample Information Cileni 'D ^P o rA -. Permil No ' ___ Toxicanl/Effluenl Sample Type ;_ Grab Collected ____ Composite Collected From ______ AM/PM To A M /P M A M /P M / // (D ate) /____ (Dale) / . (Date) Job No Loo /lS S a m p le N o TRC. N/A m q /L Initial p H N /A Initial D O n /A m a/L A d ju s tm e n t n /A T e s t In fo rm a tio n ' Analyst(s) s tn . S jL r i Tasi Spadas p . p a m A t C u ltu re N o P i a n Age e < x > \V L e n g th ( R S D ) ________ W e i g h t ( x S D ) _______ Test Mode Dilution Water EPr _. ACUTE TOXICITY TEST .Start of Tesi -3 IT O AM/@ ? -I I ! \ (Dale) End of Test 3 5 j 3 -- T e s t C o n ta in e r S ize to / 0 _L (Date) nr\L T e a l S n ln lio n V o lu m e S?*5 r *N U ------------ - D is so lv e d O x y g e n (T im e T ie s t S o in /C o n c ) ' / I______!__1______I--- L A e r a t io n _________ _____________________________ -- B eg in n in g D a le /T im e /R a le Pholoperiod 16-hour day/8-hour night Cone or % Rep loop tng/. A Number of Live Organisms 24 40 ID to I % Survival Dissolved Oxygen (mg/L) 24 40 pH 24 /oO/- 1 & iS L k l l f - 7 z l Temperature ("C) 48 1 5 25 24 40 35 7 5 Initial Alkalinity (mg/L as C a C 03) (a t-\ Initial Hardness (mg/L as C a C 03) Conductivity (imhos/cm) In itia l/F in a t 539 \0O lOo mc^/L__A LCl lo O I 0 0 Y. 7 f t T O M 9 - 1 7 J ^5 3 5 R 5 Crsn-Vr-a| A lo IV l o l b '/ M 7,0 7 & 7 1 5 2.5 3 ^ 3 5 " 331/ ompany Sanitized. Does not contain TSCA CBf Comments Z'-TQprr, Jrn Condition ol Organisms at Test Imliation/End 5 EfJ 5rn sp7 VNgaVfti^ , n o r m a l -- i -- H C Q / N ITpmplatesIBioDendAaculetTOXI EST WPD Sv(J Sm lS.rO S'2 rV Notes Cr>j # 3 ' / z6/t>l LC-5r> > loop O t , n?--l(I OLVER LABORATORIES APPENDIX 5 ACUTE TOXICITY TEST DATA Company Sanitized. Does not contain TSCACBI OLVER la b o r a to r ies Company SanHzed. Does not contain TSCA CB1 OLVER LABORATORIES INCORPORATED ENVIRONMENTAL BIOLOGY LABORATORY TEST SUMMARY SHEET CLIENT Dufcnt _ TOXICANT/EFFLUENT JOB NO PERMIT NO Acu,-K TjXxc-i~Tj T id in g ACUTE TOXICITY TEST RESULTS ( c n l l 6 ___________ PAGE __ !__ O F ___/ N /A ______________________________ CHRONIC TOXICITY T EST RESULTS Ceriodaphnia Fathead Minnow Ceriodaphnia TEST DATEfSl Z j IM -Z./lCe/ol z/ h - Z / Jfa/o/ TEST CONDITIONS TEST ORGANISM AGE DILUTION WATER SOURCE AERATION A hour* EPA-MHW OLVER LABS continuous 3 .vjs EPA-MHW OI.VFR LABS continuous TEST ORGANISM AGE DILUTION WATER SOURCE AERATION EPA-MHW OLVER LABS continuous Fathead Minnow EPA-MHW OI.VFR LABS continuous o TEST ACCEPTABILITY CONTROL SURVIVAL {z 90%) loo/ CONTROL SURVIVAL (*00%) NO OF CONTROL FEMALES % CONTROL FEMALES WITH 3 BROODS (60%) AVE NO YOUNG/SURVIVING FEMALES (15) STATISTICAL RESULTS SURVIVAL IN 100% LCW 95% C I METHOD 35/ >5<30 "Yj/l ND* wr> AVE W T/SURV CONTROL (0 25 mg) /mi/. > 5 oo m 5 /L N fc> WO SURVIVAL IN HIGHEST ( ) CONC NUMBER OF REPLICATES NUMBER OF ORGANISM/REPLICATE NORMAL DISTRIBUTION? HOMOGENEOUS VARIANCE? NOEC METHOD NOEC SURVIVAL NOEC REPRODUCTION/GROWTH SG SG SG iniCMPLATEUlOQGNCinmOAUMJimeSTSUM WTD R e vise d M arch 21, 2001 Sample Iniormaiio Client' - Permit No n /A Toxicant/Effluuent Sample Type3 s1i Grab Collected ______ AM/PM Composite Collected F r o m ________ A M / P M To _______ AM/PM / / // (Dale) J ____ (Date) _____(Dale) Job No /7 T Sample No wM T RC Initial dH Initial D 0 Adiustments N/ ma/L ma/L P3 i f 7. ...Z ACUTE TOXICITY TEST Test Inlormation 3,^0 / )fa/oTAnalyst(s) s iA i 1 f. n> Start of Test / 30 Test Species C`.enn'baniu<L ctubia. End of Test I AM/@ 2. / I H I o l (Dale) AM/ggft A (Date) Culture No ,'n d m t/u o l Test Container Size 3p m I Age c ?<-/ h r s ___ Test Solution Volume 2s .t Length (r SD) Weight (x SD) Ja LL Dissolved Oxygen (Time/Test Soln/Conc) / /______/ / // Test Mode ifc.h c. Aeration j / A Dilution Water EPA /nr/uu Beginning Date/Time/Rate Pholoperiod 16-hour day/8-houi night Company Sanitized. Does not contain TSCA CB1 Cone or % Rep --f*D-k:O----fcro* m------- A & c D Number of Live Organisms 0 24 40 % Survival Dissolved Oxygerl (mg/L) 0 24 40 55 1 s 7O S5 `V 9 5 / - S? 5 5 57 pH 0 24. 48 1 ? I S 7 .2 Temperature (C) 0 24 40 3b Initial Alkalinity Initial Hardness (mg/L as CaCO-,) (mg/L as CaCOj) Conductivity (imhos/cm) Initial/Fmal 3 0 A- S S S' --a1/-o--O----jp~fp--m------ A 6 c. C 5 ? 08 f sf R) / 5r 55 R/ ' 1 . 0 T f 1 8 7 9 Sb 2 b ^> 335 T-o--o----f B^U-M5-- A fi 5 S' 1s 5 5 5 / |O0 / 7.0 7 8 7 f7 7`S' 3 pT'' S S >^ (1 5 S ) s ' f Analyst's Inili iIs/Time T T Comments 5J 5 jJ Condition of Organisms at Test Imliation/End f) (W7/u .<-6 L 6U> iliS .01 Notes l'o r b a i d " T- i j s 'foi 5oa " '`Ml. ftoCM0-/ /o n R U n try I $ h /-A,i/T f.-ne-Z/iQno i a p o m re d he aldhu / napyci | N \Templaies\8ioOonch\acul0\TOXTE5T WPD OLVER LABORATORIES Company Sanitized. Does not contain TSCA CBt N \T enpIdlos'DtoDunciAocutc\TOXT EST WPD LABORATORIES I Company Sanitized. Does not contain TSCA CB! Sample Information Client Permit No ___ Toxicanl/Effluenl Sample Type _ Grab Collected AM/PM / / Composite Collected (Date) From _____AM/PM J ___ (Date) To ______ AM/PM J ___ (Dale) Job No (p u ) 1 5 Sample No AJA TRC mq/L Initial oH Initial D0 rrm/L Adiustmenls J ACUTE TOXICITY TEST iTest Information Analysl(s) s / n Line1 Test Species Culture No Jiig .fi Age ______ --30--------- I n n n lh (< S D 0,0^ W e ig h t (>< S D ) a H a 1 c Start End Test Test o( Test ol Test. 1a5-0op AM/Pt^t g V/1 l o i 'M W 1 / Ih l T (Dale) (Date) Container Size ___(_p_o_o__m_I_--______ Solution Volume `-to o mL______ L Dissolved Oxygen (Time/Tesl Soln/Conc) // // // Test Mode 5-kh'C______ Aeration _---------------- Dilution Water mH<~j Beginning Dale/Time/Rale Pholopenod 16-hour day/8-hour night Cone or % Rep Number of Live Organisms 0 2d 40 % Survival Dissolved Oxygen (mg/L) 0 24 48 0 pH 24 48 Temperature (C) 0 24 48 Initial Alkalinity Initial Hardness (mg/L as CaCOJ (mg/L as CaC03) Conductivity 0/mhos/cm) Imtial/Final 5dC Pfm A I n / 1 0 / OO /' 7.B 7 0 78 7 5 7 7 25 25 (eXL s i n I a lb / 00 / 3o2L /T o g A 1 0 1 0 (0 00 t "7 A 7 -0 U A 7 P) 7 . 5 " 7 7 7 5 2 5 2 5 8 t o 10 1 1 o o i - 3 ? /5 /n < 5 5^ 3i f 3oO PprTi A R fZ 0 0 f p m A 6 1 0 0 to I O \6 10 1 0 t o I 1D to lo /oo 7. 7 - 8 U too t. (o-(p 7 .& 7 5 7 7 160 7 ' P) 1 . 0 A 1?! 7 - 8 7 5 7 7 loo ' 2 5 ,,7 5 ... 2 5 3(7/0 25 5 5 _ 2 -/ T T c fi 3e3r^c) 7z/ 14/ Co,vR> I A 6 I Analyst's liutials/Time Comments 10 , 0 t o /o m th 5 to Condition of Organisms at Test Imlialion/End t o > 60 /' uW O 7 l x /p b 7 - 8 Vi t-fhD VJAV) S s fi 1.5 7 7 25 25 V i LmT> V\ffxO )0>rr lwD LimP (e O Noies C /L r L u $ Ll ^ S l o 0 5 00 m \ J ----------------- ---- , norm g I/ H<aI/K] HirCeroat N \Templaies\BioBench\aculeYl OXTEST YVPD OLVER LABORATORIES m. W W Sample Information Cileni ___ LA- Permit Ho N Toxicant/Eftluenl Sample Type _ Grab Collecled _____ _AM/PM Composite Collected From ______AM/PM To AM/PM / / // (Date) J ____ (Dale) J ____ (Date) Job No feoH E Sample No A)/A_______ T R C ________ m a /l Initial pH __ Initial D O mq/L . Adjustments _______ P. 7- O'f 2. ... ACUTE TOXICITY TEST Test Information Analyst(s) "Zm / l~mt> Start of Test 2 -nn AMlfu) ^ I (Date) Test Species P fV*.^ faC End of Test, i 5 0 _Atv#M / i W p f (Dale) Culture No Age -3 . 5 Test Container Size _ Lo o p / n L Test Solution V_o_lu_m_e H<Pi. rn t~_____ I ennlh fx SDt n H tT t o o<- cm Dissolved Oxygen (Time/Test Soln/Conc) Weight (x SD) -I 0-21 mtj ___ I------/------ ----- L------L------ ------L------L Test Mode S-ki-fi?. Dilution Waler Erf1A / n u n Aeration Beginning Date/Time/Rate Photopenod 16-hour day/B-hour night Cone or % Rep Number ol Live Organisms 0 24 -to % Survival Dissolved Oxygerl (mg/L) 0 24 40 0 pH 24 40 Temperature (C) 0 24 40 Initial Alkalinity Initial Hardness (mg/L as CpC03) (mg/L as CaC03) Conductivity (f<mhos/cm) Imlial/Final A 1 0 1 |0 loo 1 7 - 8 l x 7- 75 I f - 3 D2 ^ / ( m i dH ) y~t>n J* rz ) n I 10 1 0 6 ( / l\X Company Sanitized. Does not contain TSCA CB1 * 1 Analyst's Imti als/Time MfcH Comments imp 1 Condition of Organisms at Test Iniliation/End Sn-| LWt Srr) UpoO U vtT) z>sn U^O \tfAQ Notes Hec-lFN-j , v-i a r m r j / . Oorrfic' N \T6mplals\BtoGanch\acuIe\TOXTEST WPO 4X R ' P/ls'/o f OLVER LABORATORIES APPENDIX 6 CHRONIC TOXICITY TEST DATA Pimephales prometas 45 Company Sanitized. Does not contain TSCA CBI OLVER la b o r a to r ies I t Company Sanitized. Does not contain TSCA CBi TEST SUMMARY SHEET OLVER LABORATORIES INCORPORATED ENVIRONMENTAL BIOLOGY LABORATORY CLIENT TOXICANT/EFFLUENT.' JOB NO _ G>on 5 PERMIT NO N/A PAGE OF ACUTE TOXICITY TEST RESULTS Ceriodaphnia Falhead Minnow CHRONIC TOXICITY TEST RESULTS Ceriodaphma TEST DATE(S) TFST CONDITIONS TEST ORGANISM AGE DILUTION WATER SOURCE AERATION EPA-MHW OLVER LABS continuous EPA-MHW Ol VFR I ABS continuous TEST ORGANISM AGE DILUTION WATER SOURCE AERATION EPA-MHW OLVER LABS continuous TFST ACCEPTABILITY CONTROL SURVIVAL (90%) CONTROL SURVIVAL (80%) NO OF CONTROL FEMALES % CONTROL FEMALES WITH 3 BROODS (60%) Falhead Minnow zj ^--xlzolol i -ZH ho. EPA-MHW OLVER LABL continuous STATISTICAL RESULTS SURVIVAL IN 100% l c 50 95% C I METHOD COMMENTS AVE NO YOUNG/SURVIVING FEMALES (15) AVE WT/SURV CONTROL (0 25 mg) SURVIVAL IN HIGHEST f 5oo "\3/o) CONC NUMBER OF REPLICATES NUMBER OF ORGANISM/REPLICATE NORMAL DISTRIBUTION? HOMOGENEOUS VARIANCE? NOEC METHOD NOEC SURVIVAL NOEC REPRODUCTION/GROWTH qzR R/ IO S ND G V;s R No G S i i S tdtd'SG IXiM.-H!) 5oo r^a/t-- Soo >gaO "'S/l. li \ 1EMPLATP'DtOBMCH\8 tOADWlM\TESTSUM WPD Revised March 2 \ , 2001 Company Sanitized. Does not contain TSCA CBI TEST SUMMARY SHEET OLVER LABORATORIES INCORPORATED ENVIRONMENTAL BIOLOGY LABORATORY CLIENT D iaPartiTOXICANT/EFFLUENT JOB NO U ol~~i5__________ PAGE ___ L . O F -- L PERMIT NO m )A____________________________ ACUTE TOXICITY TEST RESULTS Cenodaphnia . Fathead Minnow CHRONIC TOXICITY TEST RESULTS Cenodaphnia t1ctoc t1 UnAnT1Fu/lQO\i TEST CONDITIONS TEST ORGANISM AGE DILUTION WATER SOURCE AERATION TEST ACCEPTABILITY CONTROL SURVIVAL (90%) FPA-MHW Ol VER LABS continuous FPA-MHW OI VER LABS continuous TEST ORGANISM AGE DILUTION WATER SOURCE AERATION #CONTROL SURVIVAL (60%) NO OF CONTROL FEMALES % CONTROL FEMALES WITH 3 BROODS (60%) FPA-MHW Ol VER LABS continuous Fathead Minnow z //3 -z /z // / - Z>4 hrs FPA-MHW Ol VER LABS continuous ^57. STATISTICAL RESULTS SURVIVAL IN 100% l c 5q 95% C I METHOD f COMMENTS C oaLvO oortV, AVE NO YOUNG/SURVIVING FEMALES (15) AVE W T/SURV CONTROL (0 25 mg) SURVIVAL IN HIGHEST ( 5oo ^ 3/0 CONC NUMBER OF REPLICATES NUMBER OF ORGANISM/REPLICATE NORMAL DISTRIBUTION? HOMOGENEOUS VARIANCE? NOEC METHOD NOEC SURVIVAL NOEC RfPRODUCTION/GROWTH (.So o o f w *-W ~ o \ PSr-- ' L,`wr o Hzfi R ft'/ H IO S N n G Vci R NO G Vcs S SAm I'$ G 5 oo <r >\/i 5 qo ^ / l __ > 5 DO m j/, N\TGMPLATE'B1086NCH\BI0A0MIHMFSTSUMWPD Revised March 21, 200i Company Sanitized. Does not contain TSCA CB1 > \ is OLVER LABORATORIES AQUATIC TOXICITY T E S T S A M P L E U S E S H E E T FO R STA N D A RD SYNTHETIC DILUTION W A TER Client' 0 3 f ^ o -v Effluent/Toxicant Synthetic Dilution Wa` Job Number Cp o )~7 *5_______ Permit No _________ _ oderatelv Hard Water (MBW1 Page_L_ofJ-- Testing Requirements 48-Hour Acute Cenodaphma Test 48-Hour Acute Fathead Minnow Test 96-Hour Acute Fathead Minnow Test 7-Day Chronic Fathead Minnow Test _____ 3-Brood Chronic Cenodaphma Test _____ Other_____________________________ j- TFRT HAY 1 23 Carboy No /Identiricalion tf i Pieparaliori Dale j./2/ol Alsh) < ?/(3 /o I Time & Day of Use 19j Hdt | a 0 m <&>2i N p \ l'iDamr@i}& J5 / I Age of Dilution Water1' ' 3D Alkalinity (mg/L) (Acceptable Range 60-70 mg/L) j-7 rJ dot 5 Po ..............(..0..--c| oici 5 Po p Hardness (mg/L) (Acceptable Range 80- dH n n (mn/\ ) Aeraiion 3 00 - -- 7f . ?u .......... ND- n$ Continuous 2V 3 00 1 . ND 7J Conlinuous 7P 307 in ND 1? Continuous 4 #3 2 / 1? h i 3 days 5 16 1 7 LEV 2 ^am^ S / ' 7 / 0 | Q /lp /o l 5?,/ H / D 1 * am/^fj R / I ^ / / A 3 m / 0 > / / 7 / 1 4 ay ) (oO <b 0 Loo (p H % 3 7 7 .? ND 1 . Continuous 7 ^ _____ ND 1,9 Continuous 313 S .O ND 7 ..g _______ Continuous lo b in 17 ND 7.8 Continuous COMMENTS m Svnlhelic dilution water is prepared wilh laboratory deionized waler and leagsnl grade chemicals (EPA/600/4-9,1/0021 (2) Each balch of diluhfen waer is no! used tor more than 14 days following .the preparation datg------------------------ -- ------------------------ ND = Nol Deleclable-------------------------------------- ----- ----------------------- -- ------------------------------------------------- -- -- --------------------- OLVER LABORATORIES O LVER laboratories LARVAL FATHEAD MINNOW SURVIVAL and GROWTH TEST SURVIVAL DATA SHEET CLIENT X l 4 2 a 2 PERMIT NO _________ EFFLUENT/TOXICANTO__s . DILUTION WATER f Q PHOTOPERIOD 16 nr Day/8 hr Night CONC "5 REP A B C D A B C D START 10 10 10 ' 10 10 10 10 10 1 10 ( 0 6 lo 10 lo 6 2 10 IO IO l 10 io IO IO JOB NO ( t OI 7 s _______ PAGE / . o f TEST ORGANISM AGE . `I H J u ' i ( START of TEST A M p U \J L J J 3 J O END of TEST l 1^ A ! V I Oj NUMBER SURVIVING PER DAY 3 456 6 1O to ) If) l o le IO |(1 I O O 9 ( 1 0 lo I o 7 io I 9 io (o I O \ i o t 0 IO " 9 9 77 Io I O (o !0 10 10 l o l o l o l o COMMENTS TEST SOLUTION VOLUME 250 mi TEST CONTAINER SIZE 600 ml FEEDING 0 1 ml BRINE SHRIMP NAUPLII 2-3 TIMES PER DAY - 16 M jjL A B C O 10 l o 1 0 10 l o \ o /O 0 10 ( I O IO lo i o i I 10 l O 13 [ 0 l o i o I O 13 10 I O (.0 ~ T 9 9 fi y^ I l A 10 i o B 10 1 0 C` 10 (0 D 10 0 : f) l 6 IO I \ 0 ( 0 |0 v, Y*) \l_ A 8 C D 10 l 1 0 0 10 l o [ 0 IO 10 I O \ l o 10 I O 1 io lo 0 7 ? i o 1o / o IO 10 1o I O q l a lo /o i / O lo Io Iff i o io i o ( o lo ,0 10 lo 1 o J (c> I O 1OlY^ji analyst A B C D COM M ENTS 10 / a 10 / o io IO 10 l o IO 10 O l im T) f i f l-Hi n i 1 I 1 d IO 1o 1 IO io lo 16 l o /A V fitsl 1&P Q i'if Orejan i sms \o IO / o 10 IO IO 10 /> O lo J0 IO U" D CLP/ V q r h a l-th - u r / -its 0 m Orr>plrftoo ___ N 'Templatcs\BioBench\clvc>mcviFHMSl,'RV W ?D 49 Revised November I ?Q0Q Company Sanitized. Does not contain TSCA CBI O LVER LABORATORIES r.\ IF N T D u f n n t - PERM 1T NO E F F L U E N T /T O X IC A N T . DILUTION WATER B?f> m H uJ PHOTOPERIOD 16 hr Day/8 hr Night CONC 5 oo REP A B C D STA R T 10 10 10 10 A 10 - / &iS u B Ci D ----------- A B C D 10 10 10 10 10 10 10 12 lo } IO lo t o lo I D [O / lo to iO lo (0 7 --l o-- 3 /d > 1 IO 10 !o in 0 LARVAL FATHEAD MINNOW SURVIVAL and GROWTH TEST SURVIVAL DATA SHEET JOB NO /yW?S~ _ PAGE _ Z _ o f ^ _ TEST ORGANISM AGE. -ZM ( i-ZU VwsA START of TEST 3 ;6> A M & _ 2 J J J 0 L END of TEST 7 ^ AM/ ! XTZoi a I 45 R lo /o 9 iO lo / o /o I D lo J O lo 9 67 COMM ENTS lo /0 TE S T SO LUTIO N VOLUM E. 250 ml T~ TE S T C O N TA IN E R SIZE. 600 ml 9 1 0 /< ? l o /> FE E D IN G 0 1 m l BRINE SHRIMP N AUPU I l o } 0 2-3 TIM ES PER DAY / o 10 ? ?. A 10 B 10 C 10 D 10 A 10 B 10 C 10 D 10 A 3 C D a n a ly s t COMMENTS 10 10 10 10 MGH 5 id 7~o U rV 2 *p 5 (lb J Co.V+orJ_# I &/0 '0 f f t a h '.i rr\S A p p e a r p 4 l- t f y Cf-t -fe V-f- I n r h - h o / ) * C o m p Ic T ? N 'Tctnplatcs\iocnch\chroi\ic\FHMSUl\V V/?D 50 Company Sanitized. Does not contain TSCA CBI Revised November I 2000 O LVER LABORATORIES LARVAL FATHEAD MINNOW SURVIVAL and GROWTH TEST GROWTH DATA SHEET CLIENT _ Q u OQi } l PERMIT NO JOB NO V 01?*? ANALYST L r ^ Deciea vveigiuI N IT IA L B A L A N U f c U A U D K . H 1 1>JJN U n t U i N e x CONC REP F O IL W E IG H T (m g ) F O IL W E IG H T +F IS H W E IG H T of F IS H NO of S U R V IV IN G FIS H CoYY . A 10(p 0 (p B C n2 70 0 ? i oL, 110 H i III 7<j l/5~ U 7 5 HO V 12 3 11 7 72 H o7 0 7 i0 Q)n\ro l A 77.79 B 90 3 9 C 90.07 D i /o3\ 0 2 10? a 7 3 ?2 19 7 7 i Gb 72 5 i7 3 .5 0 3 s.V 1,0 to 16 f 7 10 "S/l A / 03 7(a B 09 n C r / oo D ?o s7 A ?5o2 B > f 5? C , b<?. o7 D 77 00 0<k 7 (j 20 9 2 ?9 75 27 50 12 2 3 72 HS 21 0 7 5 00 7.30 5 71 9 7\ M S7 3 7io 7 71 3 93 o 7 to 0 to 6 /0 ? A ?0 00 93 ?? 3 92 ? 75 B 7777 C ? 7 r>7 lo2 7 7 75 2% 5 0.3 H 17 0 7- D 79.10 02- 27 9 - i 7 10 5o ^ 1^ A B C D 77. SI 92 27 97 !<? T V 7-0 To. 9 5 $0 3 7 72 7b 7VSV 7 97 9 /o 3.71 9 37 0 /> /O 0 PAGE I of 2 7 , -'-Ht _J---- __________ AVERAGE * PERCENT W E IG H T P E R F IS H S U R V IV A L .972 - 511_____ 312 709 /oo / 0 0 '/ 9o Y ' /00 0 S l7 350 ?>S3___ *9/o /o o /. 00 /___ 7 6 '/, 36 / .576 970 577 v,z/ ton / 9o / ..... 0 6 ' / loo 7 9sH . . H7LU Y Y / ........ ... . 373 too V loo / to o './ :- _______ 70 / 332 . 563 9 ) 7 w _ 7 73 .9 / 0 33? v?y Ho /- O o '.L ______ %7 00 7 00 V ' /o o 3.. _______ too V 'oo >' N \Tcmplaics'>BioEcnch\chronic\FKMGRWTH WPD ^^ Revised November 1 2000 Company Sanitized. Does not contain TSCA CBi 3o r 5 > _ O LVER LAB ORATO RiE S LARVAL FATHEAD MINNOW SURVIVAL and GROWTH TEST GROWTH DATA SHEET CLIENT "P u -P o ^ PERMIT NO ______ JOB NO ( i 0 / 7 5 ANALYST Im D PAGE 7 of 2 INITIAL BALAN CE CALIBRATICDN CHECK Excected weiqnt CONC REP FOIL WEIGHT FOIL WEIGHT WEIGHT of (mg) + FISH FISH "31/ UU UIL) / NO of AVERAGE * SURVIVING FISH WEIGHT PER FISH PERCENT SURVIVAL A 76 7 7 9/ 77 B Lt 7 7 7 o rt? C 7 7 /5 7 /T - 0 9 5 75" ?9 35 Lrrc h :? 3 l 3 .7 3 3 3/ to > '0 to /o .9 7 7 i q .o I l - ____ - .3?. 3 ________ / d V - _ 5 9 6 _______ _ / M 7 _____ -3 3 / /O 0 /- . 500 A /P P /,7 B 5 7 <?7C 7 7 /> D l ? 9 5-7 / 0 5 * <55 H 0Z 7 3 7V 77. ? 0 H 93 7 17 7 77 7 7J! /o 1 /0 10 993 . 7 /7 9 7 % ______ i3 ~ t / o o ' / ____ t o o /-. lo o '/ A B C D A B C D A B C D A B C D h l N A L d A L A N U t O A L i o r w i h- ' in COMMENTS r li I F t iJu\^~ Qr\ "Un ^r-jvVieJ n a r n k r ^ , ,/ . 'Lia u N 'Templaies\Bio3cnch\chromc\fKMGRWTH W?D ^^ Rcvibcd November i 2000 Company Sanitized. Does not contain TSCA CBI CHRONIC TO XIC ITY TEST V CHEMICAL ANALYSIS DATA SHEET -. Page >f y OLVER L A B O R A T O R IE S c lie n t T ) i <n n n f ~ JOB NO U O rtS Pr cErRu vMi iI Ti N O - E F F L U E N T /T O X IC A N T _ D IL U T IO N W A T E R EPQ 7*1 HW TEST IN IT IA T IO N D A T E X l 0 j o \ ------------------ TEST C O M P L E T IO N D A T E A - / P I------------------ T E S T O R G A N IS M P 0 re A c la. S______ P H O T O P E R IO D 81 6 - H o u r D a v / - H o i j r N ig h t, L I G H T IN T E N S IT Y _5P-1,,QQUrS-- ----------------------------- IN IT IA L pH D .O (m g /L ) T e m p e ra tu re (C ) C o n d u c tiv ity (u m h o s /c m ) H a r d n e s s ( m g /L a s C a C 0 3) DAY 1 1 ft 7-8 3oO DAY 2 75 19 35 3oo DAY 3 73 7S 7 ,7 ,577 DAY 4 7? 7? 35 3o 7 DAY 5 7 -5 7-? 73 315 AY 6 DAY 7 0 .0 7 3 7S7 7 ? 3 .3 i 5 _ 3 5 3/3 A l k a l i n i t y ( m g /L a s C a C 0 3) A n a ly s t's In itials 5m 5 (1 i\J L m D (JriD 5iM unP F IN A L pH D .O . (m g /L ) T e m p e ra tu re (C ) C o n d u c tiv ity (^ m h o s /c m ) A n a ly s t's In itials ____________________________ 75 7 5 7 % io,0 3 . l 3 ? 73 55 7 -7 3 -3 73 73 ---------- 17 5 ds lb 00 3^ S0 u n D 313 3 3 7 2 9 6 L W twoLtnO S R pJ / * / CO M M ENTS L l'n .n a u ---------- C. roi TntcieAnb, 'anf.rc/1. 1 1Jlp\ J IN IT IA L DAY 1 DAY 2 DAY 3 DAY 4 DAY 5 DAY 6 DAY 7 CO M M EN TS pH 7 . ? D .O . (m g /L ) T e m p e ra tu re (C ) C o n d u c tiv ity (u rn h o s /c m ) I7 15 300 H a r d n e s s ( m g /L a s C a C 0 3) A l k a l i n i t y ( m g /L a s C a C 0 3) 7O A n a ly s t's In itials U ^D 75 75 25 77 7 7 ,5 300 27 G ?o 303 76 60 S rJ U n o 75 3 -7 75 7 .? ,3n 7 25 35 72 G o urn w _Z 7 75 77 75 35 3 ) 3 31H 7 2 Ctfpio: (ztfbH * * - 5 2 LpO i7 ^ / o ( ^ 7 : (ACCmT' F IN A L pH D 0 (m g /L ) T e m p e ra tu re (C ) . 75 (o.O 55 77 50 IKS' 77 5X 35 C o n d u c tiv ity (jim h o s /c m ) A n a ly s t's In itials 316 J P 330 ^ 0 LfflQ Y T ) N \TEMPLATP.BIOBENCH\CHRON|C\CHRONCHE W P0 75 31 35 272 W 7-7 75 7 5 7 - 2 (? 0 6 O So 7 5 333 375 0A i m O Revise November 1 2000 53 Company Sanitized. Does not contain TSCA CBI 54 Company Sanitized. Does not contain TSCA CB1 CHRONIC TOXICITY TEST CHEMICAL ANALYSIS DATA SHEET Pag 2, of _h_ O LV E R L A B O R A T O R IE S CLIENT JOB NO /gO l f O . PERMIT NO EFFLUENT/TOXICAN' DILUTION WATER. E R INITIAL T E S T IN IT IA T IO N D A i E ^ I l l / o i . ----------------- T E S T C O M P L E T IO N D A T E . # 7 7 <3 / ------------------ T E S T O R G A N IS M PH O TO PER 1C D P Q r c r i t la ^ ffi-H nur D a v /3 -H o u r N ichj L I G H T IN T E N S I T Y _ 5 Q - 1 Q.Q ft-C--------------------------- CLUONNDCCE NN T R A T IO N SO ? p K DAY 1 DAY 2 DAY 3 DAY 4 DAY 5 DAY 6 DAY 7 COMMENTS pH D O. (mgIL) . Y -.r 1-5? T-.r I S Temperature (C) 9.5 7 5 Conductivity (umhos/cm) 7)60 Hardness (mg/L- as CaC03) 7 .7 9 -f 75 7? as 307 1 ) 3 0 i l _ 75 YJ 73 7 5 73 75 3 W 3 /3 3 i- Alkalinity {mg/L- as CaCOJ Analyst's Initials FINAL pH D.O. (mg/L) Temperature (C) Conductivity (mhos/cm) Analyst's Initials UTiO S lO / JrO L M D JN T O 7 r5 7 3 7 7 O jo 7? 7 5 :*5 7 5 B n 3 i3 7 /5 J lc J UrLO U m 7 7 7 -5 7 7 7 5.0 3 - 7 K L - 75 15_ 3 3 | 33 6 J w t o ImD ____ 1 ----------- ------ A.-_- . INITIAL CONCENTRATION 7 S ' 7Q pn DAY 1 DAY 2 DAY 3 DAY DAY 4, 5 DAY DAY 7 6 COMMENTS pH D.O. (mg/L) Temperature (C) Conductivity Lumhos/cm) Tlardness (mg/L as CaCOJ 7? 7^ 75 3oo 77 7J 75 3^0 77 3 ? 77 7 * 7 5 15 397 Tv? 7 7 _o_ 1 9 1-s 7 ^ 7 Y b 7S 3 1 V 7 /3 3l4 Alkalinity (mg/L as 0aCO3) Analyst's Initials LmO i m o U n j) < 7 7 35(3 LmO FINAL pH D O. (mg/L) 7- 7 3 7 7 GO 5 0 3 7 Temperature (C) 7 5 975 75 Conductivity (unhos/cm) 3 03 3I j ]| Analyst's Initials T O LmO UyP N \T=MPLAoBBIOBENCH\a-iRONiaCHRONCHE WPO 7 3 7-55 .0 3 -9 05 5 7 /p 371 T O ftA j-j- 73 70 K Jri/7 3.7 35 370 5^? R ev ise NGvemer 1. 200 Company Sanitized. Does not contain TSCA CBt CHRONIC TO XIC ITY TEST CHEMICAL ANALYSIS DATA SHEET A ~" Page H of 9 OLVER L A B O R A T O R IE S g * ^ c l ie n t _ D i) , p n n h P B m L JOB NO ( 3pjl T 5 ~ ------------------ P E R M IT N O __________ EFFLU EN T/TO X 1C A N T _ D ILU TIO N W A T E R : r J A PI /H J ZU/Z/olT E S T IN IT IA T IO N D A T E / - ..____ l X l i o UT E S T C O M P L E T IO N D A T E X l M l O t TE S T O R G A N IS M P 0rc,r\<~ltxs________ PHO TG PERIO O 1 6 -H o u r D a v /8 -H o u r N ight L IG H T IN T E N S IT Y J 5 Q-.1QP ft-C. IN IT IA L 1D A Y C O N C E N T R A T IO N S O Pi?TM 2D A Y DAY 3 DAY 4 DAY 5 6D A Y DAY 7 COMMENTS pH D.O (m g/L) T e m p e ra tu re (C) C o n d u c tiv ity (p im h a s/cm ) H ardness (m g/L as C aC O J A lk a lin ity (m g/L as C aC O J A n a ly s t' s In itia ls 72 7t V5 3oo QP Uv)0 1 -9 1 -5 7 ? 1 1 2,o 7^ 1 1 1% I t l i 13 3 3 75 2 5 %5 25 i5 3 oo ,30> 3oT- 3J9 3)3 3 t L <a )0 7 l oV 91 I1 IO (d3- (oT- (pQ (p0 i M LxrD LW SW Sp IM ) FIN A L pH D .O (m g /L ) T e m p e ra tu re (C) C o n d u c tiv ity (u m h o s/cm ) A n a ly s t's In itia ls 7 .5 1 3 7.3 v 3 7 3 1 -5 (p .O 3 5 U 3.2 3 A 7 7 1 5 1 5 2 5 ' l l 7 7 75 3)1 ?)I3. 315 331 3 7 I P 3x) LmO two S tl M LmO UnD IN IT IA L C O N C E N T R A T IO N [ O V P!Y> DAY 1 DAY 2 DAY 3 DAY 4 DAY 5 DAY 6 DAY 7 COMMENTS pH D .O (m g/L) T e m p e ra tu re (C) 7r 15 21 C o n d u c tiv ity tim h o s /c m ) 3 0 H a r d n e s s ( m g /L a s C a C D 3) 7 8 771 7 * ?3 7 7 I t l i 7-9 25 25 7 3 3 00 301 3 o l 3 )3 7.0 7 .9 73 7 * 75 35 3)3 3 W Alkalinity (m g /L as C a C O J A n a ly s t's In itia ls LM0 $7 N Lm o Lm D 5 ^ 7 T p " LlYlO FIN A L pH / . $ 7 3 . 7 3 D O (m g/L) Cp o .3 7 . 7 3 T e m p e ra tu re (C) 35 35~ 0 (Y ), C o n d u c tiv ity p jm h o s /c m ) 3S3 303 A n a ly s t's In itia ls 57/9 uvn Urrsf) n \tem platbbiobENch \ch r o n !C',ch ronch e w fo 73 -7.3 3 0 3- ^ 7 5 xb 3 3 ? 311 Sfi 73 7 9 7 7 9-7 35 ,923 377L/d D Lm o Company Sanitized. Does not contain TSCA C tt R evise N ovem ber 1. 2000 A. TEST FOR NORMALITY OF SURVIVAL DATA T itle F ile prom elas S u r v iv a l-2 /1 3 /0 1 T ransform ARC S IN E (S Q U A R E R O O T ( Y i) S h a p iro - W ilk 's T est f o r N o rm a lity D= W= 0 1560 0 8233 C r i t i c a l W = 0 8 9 6 0 (a lp h a = 0 01 , N = 29) W = 0 9240 (alph a = 0 05 , N = 28) Data FA IL n o r m a lity t e s t (alph a = 0 .0 1) T ry a n o th e r tr a n s fo r m a tio n . W arning 1 The f i r s t th re e h o m o geneity te s ts are s e n s itiv e to n o n -n o rm a lity and s h o u ld n o t be o e rfo rm e d w it h t h i s d a ta as i s B. TEST FOR HOMOGENEITY OF VARIANCE T itle -File. D u p o n t|H B H T o x ic ity -P pro m e la s S u rv iv a l-2 /1 3 /0 1 ~ T ransform ARC S IN E ( S Q U A R E R O O T ( Y ) } H a r tle y 's T e s t f o r H om ogeneity o f V a ria n c e B a r t l e t t 's T e s t f o r H om ogeneity o f V a ria n c e These two te s ts can n o t be p e rfo rm e d because a t le a s t one g ro u p has zero v a ria n c e D ata FAIL to m eet h o m o g e n e ity o f v a ria n c e a ssu m p tio n A d d itio n a l tra n s fo rm a tio n s are u se le ss Olver Laboratories Incorporatrd V 1J.16 South M ain Street Blacksburg, V irginia 24060 Phone (540) 552-5548 FAX (540) 552-1715 q7 Company S a n itiz e d . D o e s not contain TSCA CBI AryaAuS'S- C p m w i s . m 4 p S-VlrvW d GirA-g>\ S J C. STEEL'S MANY-ONE RANK TEST T itle F ile GROUP Dupont jB H jp T o x ic itv - P ' p ro m e la s S u r v iv a l - 2/13 / 0 1 T ransform ARC S I N E (SQ UAR E ROOT (V) ) S t e e l's Manv-One Rank T e s t IDENTIFICATIO N TRANSFORMED MEAN Ho C o n t r o l- c T r e a t m e n t RANK SUM C R IT . VALUE SIG DF 0 . 0 5 1 C e n tra l 1 3713 2 5 m g/L 1 3713 18 00 10 00 4 00 3 10 m g/L 1 3358 17 50 10 00 4 00 4 25 m g/L 1 3303 16 00 10 00 4 00 5 50 m g/L 1 4120 20 00 10 00 4 00 . 100 m g/L 1 4120 20 00 10 00 4 .0 0 7 500 m g/L 1 3713 18.00 10 . 00 4 00 C r it ic a l va lu e s a re 1 t a ile d ( k = S ) Olver Laboratories Incorporated 1116 South M am Street sS Blacksburg, Virginia 2406 Phone 15401 552-5548 F-VX 15401 552-1715 58 Company Sanitized. Does not contain TSCA CB! t^o-W ^.no.\u--?,i's ComoftivS.-'.n Cqq-WoIS A. TEST FOR NORMALITY OF GROWTH DATA T itle F ile Dupo: o x ic ity -P p ro m e la s G r o w t h - 2 / 1 3 / 01 T ransform - S h a p iro - W ilk 's T est fo r N o rm a lity NO T RANSFO RM ATIO N D= W= 0 0809 0 9114 C r i t i c a l W = 0 8960 (a lp h a = 0 01 , N = 28) W = 0 9 2 4 0 ( a lp h a = 0 05 , N = 28) D a ta PASS n o r m a l i t y t e s t ( a l p h a = 0 01) C o n t in u e a n a l y s i s B. TEST FOR HOMOGENEITY OF VARIANCE T itle F ile D u p o n t, ' T o x ic itv -P p rom elas G ro w th -2 /1 3 /0 1 T ransform NO T RANSF O RM AT IO N B a r t l e t t 1s T e s t f o r H o m o g e n e i t y o f V a r i a n c e C a l c u l a t e d B1 s t a t i s t i c = 1 2700 (p -v a lu e - 0 9 D a ta PASS B1 h o m o g e n e it y t e s t a t 0 01 l e v e l . C o n t in u e a n a l y s i s C r i t i c a l 3 = 16 8119 = 12 ,591c (alph a = 0 01, d f (a lp h a = 0 05, d f 6) 6) Olver Laboratories Incorporated I11S South Mam Street si Blacksburg, Virginia 24060 Phone (540) SS2-BSAS FA X (540) 552-1715 59 Company Sanitized. Does not contain TSC CBS |\riciAuS'5>- Cdrr\e>c^-( '.SnA ~T~o 'SA-ty-iAo./.d-- c. a n a l y sis of variance of dry w eight data T itle F ile Dupont o ;tic ity -P pro m e la s G ro w th -2 /1 3 /0 1 T ransform ANOVA T a b le NO TRANSFORMATION SOURCE B e tw e e n W ith in (E rro r) T o ta l DF 6 21 27 SS 0 0117 0 0809 0 0926 MS 0 0020 0 0039 F 0 5065 (p -v a lu e = 0. 7965) C r i t i c a l F = 3 B117 *, = 2 5 7 2 7 (a lp h a = 0 01, d f = 6,21) (a lp h a = 0 05, d f = 6,21) 'S in c e F < C r i t l e a l F F A I L TO REJECT Ho A l l e q u a l ( a l p h a = 0 . 0 5 ) D. DUNNETT'S TEST T itle F ile Dupont p ro m e la s G r o w th - 2 /1 3 /01 T ra n s fo rm NO TRANSFORM AT ION D u n n e tt' s Test 1 - GROUP ID E N T IF IC A T IO N TABLE 1 OF 2 TRANSFORMED MEAN Ho C o n t r o l T r e a tm e n t MEAN CALCULATED I N ORIGINAL UNITS T STAT SIG 0 05 1 C o n tro l 0 .4 1 9 8 0 4198 2 5 m g/L 0 .4 6 B 3 ' 0 .4 6 8 3 -1 1053 3 10 m g/L 0 .4 1 6 0 0 .4 1 6 0 0 0855 4 25 m g/L 0 4295 0 `4295 -0 .2222 5 50 m g/L 0 4415 0 4415 -0 4957 6 100 m g/L 0 3985 0 3985 0 4 B43 7 500 m g/L 0 4217 0 .4 2 1 7 -0 04 56 D unnett c r i t i c a l va lu e = 2 4600 (1 T a ile d , a lp h a = 0 05, d f [u se d ] = 6 ,2 0 ) (A c tu a l d f = 6,21) Olvcr Laboratories Incorporated V 1116 South Mam Street is Blacksburg, V irginia 24060 Phone (540) 552-554S FAX (5401 552-1715 C mPani' 60 D o noi c o n u m y o ,, - , Qo-Vo, ^oaW S'S- irT\-)Q<{ Gcu->~Y>o\ S T itle F ile D u p o n t - f g & r o *x i c i t y - P ' D rom elas G ro w th -2 /1 3 /0 1 ' T ra n s fo rm NO TR AN SFO R M ATIO N Dunnett's Test T A B L E 2 OF 2 Ho C o n t r c l c T r e a t m e n t GROUP ID E N T IF IC A T IO N NITM OF REPS MIN SIG DIFF (IN ORIG UNITS) % OF CONTROL DIFFERENCE FROM CONTROL C o n tro l 5 m g/L 10 m g /L 25 m g /L 50 m g /L 100 m g /L 500 mg/ L 4 4 4 a 4 4 4 0 1079 0 1079 0 1079 0 . 1079 0 1079 0 1079 25 7 25 7 25 . 7 25 7 25 7 25 7 -0 .0 4 8 5 0 0038 -0 0097 -0 0217 0 0213 -0 0020 l INHIBITION CONCENTRATION (IC25) ESTIMATE T itle F ile Dupont ic ity -P GRP ID E N T IF IC A T IO N 1 C o n tro l T 5 m g/L 3 10 m g /L 4 25 m g/L 5 50 m g /L 6 100 m g/L 7 500 m g/L prom elas G ro w th -2 /1 3 /0 1 T ransform NO TRANSFORMATIO N MEAN SMOOTHED MEAN CONCENTRATION 0 4198 0 4583 0 4160 0 4295 0 4415 0 39B5 0 .4 2 1 7 0 .4 4 4 0 0 .4 4 4 0 0 4290 0 4290 0 .4 2 9 0 0 4101 0 4101 0 0000 5 0000 10 0000 25 0000 5 0 .0 0 0 0 1 0 0 .0 0 0 0 500 0000 IC p e s tim a te w itn p = 25 i s > 500 0000 O lvcr Laboratories Incorporated V 1116 South Mam Street Blacksburg, Virginia 24060 Phone 1540J 552-5548 F \ X (540) 552-1715 61 Company Sanitized. Does not contain T 5CACBV QoVc kncc\TuJc/.s - Caom o a . f \ e. ,>n ~Vt! fsOlg.~Wia.no\ C-C.o'VvpIs A. TEST FOR NORMALITY OF SURVIVAL DATA T itle F ile E u p o n ti T o x ic ity -P prom elas S u r v iv a l-2 /1 3 / 0 1 T ransform ARC S IN E (S Q U A R E RO O T ( / ) ) S h a p iro - W ilk 's T e st fo r N o rm a lity D= W= 0 1627 0 B62 5 C r i t i c a l W = 0 3960 (a lp h a = 0 01 , N = 28} W = 0 9240 ( a lp h a = 0 05 , N = 28) D ata FA IL n o r m a lity t e s t (a lp h a = 0 01) T ry a n o th e r tr a n s fo r m a tio n . W arning l - The f i r s t th re e h o m o g e n e ity te s ts a re s e n s itiv e to n o n -n o rm a lity and sh o u ld n o t be p e rfo rm e d w ith t h is d a ta as is B. TEST FOR HOMOGENEITY OF VARIANCE T itle F ile Dupont T o x ic it'. p rom elas S u r v iv a l-2 /1 3 /0 1 T ransform ARC SINE(SQ UARE R O O T(Y )) H a r tle y 's T e s t f o r H o m ogeneity o f V a ria n c e B a r t l e t t 's T e s t f o r H om ogeneity o f V a ria n c e These tw o t e s t s can n o t oe p e rfo rm e d because a t le a s t one g ro u p has zero v a ria n c e . D a ta FA.IL t o m eet h o m o g e n e ity o f v a r ia n c e a s s u m p tio n A d d itio n a l tra n s fo rm a tio n s a re u se le s s . Olvcr Laboratories Incorporated 1116 SoutU M a m Street Blacksburg, V irginia 24060 Phone (540) 552-5548 FAX (540) 552-1715 62 Company Sanitized. Does not contain TSCA CB1 C. S T E E L 'S MANY-ONE RANK TEST T itle F ile D upont^^j^N ^ci p rom elas S u r v iv a l-2 /1 3 /01 T ransform ARC S I N E [ S Q U A R E R O O T I Y ) ) S t e e l 's M any-One Rank T e s t - Ho C o n t r o l T r e a t m e n t GROUP ID E N T IF IC A T IO N TRANSFORMED MEAN RANK SUM CRIT VALUE DF 1 C o n t r o l w / MeOH 1 3 3 0 5 2 5 m g/L 1 3713 20 00 10 00 4 00 3 10 m g /L 1 3358 19 00 10 00 4 00 4 25 m g/L 1 3305 13 00 10 00 4 00 5 50 m g /L 1 4120 22 00 10 00 4 00 6 100 m g/L 1 .4120 22 00 10 00 4 . 00 7 500 m g/L 1 3713 20 00 10 00 4 00 C r it ic a l v a lu e s are 1 ta ile d ( k = 6 ) i Olver Laboratorios Incorporated V y 1116 South Mam Street Blacksburg, V irginia 24060 Phone (540) 552-5543 FAX (540) 552-1715 63 Company Sanitized. Does not contain TSCA CB1 A . TES T FOR N O R M A L IT Y OF GROWTH D ATA T id e F ile Dupont H T o x ic i t y -? p rom elas G ro w th -2 /1 2 /0 1 T ransform P! S h a p iro - W ilk 's T est f o r N o rm a lity NO TRANSFORM AT ION D= W= 0 0799 0 9735 . C r i t i c a l W = 0 .8 96 0 (a lp h a = 0 01 , N = 28) W = 0 .9 2 4 C ( a l p h a = 0 05 , N = 28) D a t a PASS n o r m a l i t y t e s t ( a l p h a = 0 0 1 ) C o n t i n u e a n a l y s i s i B. TEST FOR HOMOGENEITY OF VARIANCE T itle F ile Dupont T o x ic ity -P prom elas G ro w tn -2 /1 3 /01 T ransform NO TRAN SF ORMAT ION B a r t l e t t 's T e s t f o r H om ogeneity o f V a ria n c e C a lc u la te d B1 s t a t i s t i c = 1 1848 (p -v a lu e = 0 9776) D a t a P.ASS B 1 h o m o g e n e i t y t e s t a t 0 01 l e v e l C o n t i n u e a n a l y s i s C r i t i c a l B = 16 8 1 1 9 = 12 5 9 1 6 (a lp h a = 0 01, d f = 6) ( a lp h a = 0 05, d f = 6) Olver Laboratories Incorporated 1116 South M am Street CS Blacksburg, V irginia 24060 Phone (540) 552-5548 FA X (540) 552-1715 Company Sanitized. Does not contain TSCA CBI fr.nc-\uS'S- Coro-QC-.rX'vOri -Vo yog.TVxQ.n\ Cco~Vvp\^, C. ANALYSIS OF VARIANCE OF DRY WEIGHT DATA T itle F ile D u p o11n t 4 | ^ ^ ^ T ooxx :i c i t y - P 1P a p ro m e la s G ro w th -2 /1 3 / 0 1 T ranstorm AMOVA T a b l e NO TRANSFORM ATION SOURCE B e tw e e n W ith in (E rro r) T ota l DF 6 21 27 SS 0 0131 0 0799 0 0930 MS 0.0022 0 0038 F 0 5754 (p -v a lu e = 0 7456) C r it ic a l F = 3 8117 ^ = 2 5727 la lp h a = 0 .0 1 , d f = 6,21) (alph a = 0 05, d f = 6,21) ' S i n c e F < C r i t i c a l F F A I L TO R E J E C T Ho. A l l e q u a l ( a l p h a = 0 0 5 ) D. DUNNETT'S TEST T itle F ile D u p o n t. T n : o r.t t v - P prom elas G ro w th -2 /l3 /0 1 T ransform NO TRANSFORMATION Dunnett's Test TABLE 1 OF 2 Ho C o n t r o l : T r e a t m e n t GROUP IDENTIFICATIO N TRANSFORMED MEAN MEAN CALCULATED I N ORIGINAL UNITS T STAT SIG 0 05 1 C o n t r o l w/MeOH 0 4068 2 5 m g/L 0 4683 3 10 m g/L 0 4160 4 25 m g/L 0 4295 5 50 m g/L 0 4415 6 100 m g/L 0 3985 7 500 m g/L 0 4217 0 4068 0.4683 0 4160 0-4295 0.4415 0 .3 9 8 5 0.4217 -1 4X03 -0 2121 -0 5217 -0 .7969 0 . 1892 -0 .3440 D unnett c r i t i c a l v a lu e = 2 4600 (1 T a ile d , a lp h a = 0 .0 5 , d f [u se d] = 6,2 0) (A ctu a l df 6, 21) Olver Laboratories Incorporated 1116 South M am Street Blacksburg, V irginia 24060 Phone (540) 552-5548 FAX (540) 552-1715 g5 Company Sanitized. Does not contain TSCACBI p g -t^ Cn.^r.C'ivsr,n ~T0 m sioano\ C.rWs . T itle F ile Dupont *6 x ic ity -P prom e_as G ro w th -2 /13/0 1 T ransform NO TRANSFORMATION D u n n e tt's Test 'ABLE 2 CF 2 Ho C o n t r o l - : T r e a t m e n c GROUP ID E N T IF IC A T IO N NUM OF REPS M IN SIG DIFF ( I N ORIG UNITS) % OF CONTROL DIFFERENCE FROM CONTROL C o n t r o l w/MeOH 5 mg/L 10 m g /L 25 m g/L 50 m g /L 100 m g/L 50Q m g /L 4 4 4 4 4 4 4 0 1073 0 1073 0 1073 0 1073 0 1073 0 1073 26 4 26 4 26 4 26 4 26 4 2 6 .4 -0 0615 -0 0093 -0 0228 -0 03 4 8 0 0082 -0 0150 INHIBITION CONCENTRATION (IC25) ESTIMATE T itle F ile D u D cn t ^B B *T Q icici ty - P p ro m e la s G row th- 2 /1 3 /0 1 T ransform NO TRANS FORMATIOt GRP ID E N T IF IC A T IO N MEAN SMOOTHED MEAN CONCENTRATION 1 C o n t r o l w/MeOH 0 406B 0 .4375 0 0000 2 5 m g/L 0 4683 0 4375 5.0000 3 10 m g /L 0 4160 0.4290 10.0000 4 25 m g /L 0 4295 0 .4290 2 5 .0 0 0 0 s' 50 m g /L 0 4415 0.4290 5 0 .0 0 0 0 6 100 m g/L 0 3985 0.4101 1 0 0 .0 0 0 0 7 500 m g/L 0 4217 0 4101 5 0 0 .0 0 0 0 ICp e s tim a te w it h p = 2s is > 500 0000 OWer Laboratories Incorporated 1116 South M am Street Blacksburg, Virginia 24060 Phone (540) 552-5548 FAX (540) 552-1715 66 Company Sanitized. Does not contain TSCA C81 APPENDIX 7 CHRONIC TOXICITY TEST DATA Ceriodaphnia dubia 67 Company Sanitized. Does not contain TSC CB1 OLVER la b o r a t o r ie s OLVER LABORATORIES INCORPORATED ENVIRONMENTAL BIOLOGY LABORATORY CLIENT TOXICANT/EFFLUEN TEST SUMMARY SHEET JOB NO _ PERMIT NO 105 MM PAGE OF ACUTE TOXICITY TEST RESULTS c h r o n ic lo x ic iiY rEST RESULTS Ceriodaphnia Fathead Minnow Ceriodaphnia TFvST DATEfS} 0 --z li-il* 1 TEST CONDITIONS TFST O R G A N IS M A G F nil 1ITIDNl WATFR SOURCE AERATION FPA-MHW OLVER LABS continuous EPA-MHW OLVER l.ABS continuous / ` DILUTION WATER SOURCE AERATION l - f i I'X'S. EPA-MHW OLVER LABS continuous TEST ACCEPTABILITY CONTROL SURVIVAL (a90%) CONTROL SURVIVAL (2 80%) NO OFCONTROLFEMALES % CONTROL FEMALES WITH 3 BROODS (2 6 0 %) t o o '/ 10 lo / Fathead Minnow EPA-MHW Ot.VER LABS continuous AVE NO YOUNG/SURVIVING FEMALES (2 15) 18 -0 AVE WT/SURV CONTROL ( 2 0 25 mg) STATISTICAL RESULTS SURVIVAL IN 100% 1L^c50,, qr% r i METHOD SURVIVAL IN HIGHEST ( Soo yj CONC NUMBER OF REPLICATES NUMBER OF ORGANISM/REPLICATE NORMAL DISTRIBUTION? HOMOGENEOUS VARIANCE? NOEC METHOD NOEC SURVIVAL NOEC REPRODUCTION/GROWTH R<;PYoci o/l/CrVO Ho/ to 1 Yti S No- S bunfl P/H '5 S loo "' Pi/L lo ma h_ o f loorf^y L*- > 5 o o mfl/L G G G COMMENTS h i g. non- Cji/iAiositos, <nUr>t __r cjfan^L n o \ c . on^g c k -2-5 itx-Ml, g A i:_ c /> W h b r, 5 a s - iA un 1 U . o '3 iU 'J f c h 'llA J p i _Ajic%JLu. Q-fA \o'Q--r ! - tv ^ - Kln&C )> bg-liJH<* A o b g . M W EM PLM eW O D EH CH 'BK M O M im T CSTSU M W rO A Sggi f i W VHl----- P v ^ r ^ S f l U . A ' A ----R f f t < ^ c u ic,-k Ih r*-?1 d -ir------l u 0 m 3 /* R evised M arch 21, 2001 Company Sanitized. Does not contain TSCA CBI OLVER LABORATORIES INCORPORATED ENVIRONMENTAL BIOLOGY LABORATORY CLIENT TOXICANT/EFFLUENT TEST SUMMARY SHEET JOB NO La0 n 5 ___________ PAGE I O F ___ L PERMIT NO N/A______________________________ TFRT DATFS1 ACUTE TOXICITY TEST RESULTS Ceriodaphnia Fathead Minnow CHRONIC TOXICITY TEST RESULTS Ceriodaphnia 2/ z d - T / m / o) TEST CONDITIONS | TEST ORGANISM AGE DILUTION WATER SOURCE AERATION TFST ACCEPTABILITY CONTROL SURVIVAL (90%) PA-MHW OLVER LABS continuous EPA-MHW OLVER LABS continuous TEST ORGANISM AGE DILUTION WATER SOURCE AERATION V" CONTROL SURVIVAL (80%) NO OF CONTROL FEMALES % CONTROL FEMALES WITH 3 BROODS (60%) i --ft h rs . EPA-MHW OLVER LABS continuous BO/ .IQ____ Fathead Minnow EPA-MHW OLVER LABS continuous AVE NO YOUNG/SURVIVING FEMALES (15) 5 , ____ STATISTICAL RESULTS' SUFlVlVAL IN 100% LC,, 95% C i METHOD f I l _______________________________ C O M M E N ^ S ^ ^ L C p r X ^ \ U c A < ! / ^ ua'T c AVE WT/SURV CONTROL (0 25 mg) 'nvW .nO \ SURVIVAL IN HIGHEST l 5nn -w J CONC NUMBER OF REPLICATES NUMBER OF ORGANISM/REPLICATE NORMAL DISTRIBUTION? HOMOGENEOUS VARIANCE? NOEC METHOD NOEC SURVIVAL NOEC REPRODUCTION/GROWTH H o/. 1o 1 V.s S NO S S-kLS S too "'3/l. loo "Wl d>" 3 /i f ^1 -AXL Q- pt-r I L ' V riituVion oJaV-v-V ' G G G l?\|FMI,LAiE\UIODENCinOIOADMIIATESTSUMNATO R e v is e d M a rc h 21 2001 Company Sanitized. Does no! contain TSCA CSJ* OLVER LA B O R A T O R IE S AQUATIC TOXICITY TEST SAM PLE USE SHEET FOR STANDARD SYNTHETIC DILUTION W ATER Client tXpan-b _________ -- Effluent/Toxicant Synthetic Dilution W ale ^^^F/vM oderatelv Hard Water fMHW) Testing Requirements ___________ 18-Hour Acute Ceriodaphnia Test I __________ _ 10-Hour Acute Fathead Minnow Test ___________ 96-Hour Acute Fathead Minnow Test Job Number _________ Permit No 'N/A Page ___________ 7-Day Chronic Fathead Minnow Test ______ X 3-Biood Chronic Ceriodaphnia Test ___________ Other_____________________________ I of I TEST DAY Carboy No /Identification 1 4F3 Preparation Dale 2) Id I Time & Day of Use l am{0 Z /2 i) / f?| Age of Dilution Waled11 1 tw y Alkalinity' (mg/L) (Acceplable Rariqe 60-70 nig/L) 0 if Hardness (mg/L) (Acceplable Range 00TnOmn/l 1 Conduclivitv (i/mhos/cm) pH Total Residual Cl; (mg/L) D 0 (mg/L) Aeralion /Do 33) (e 'T-ff ND` 78 Conlinuous 2 /d-3 i n oi 3 a jfcfloi 4 ff M 2 I1) 0 1 5 a j i t /oi |3gpt/pm2 /2 1/O 1 j j 1 "a m / 7- / 22. / 0I ff^anlf&X / /o 1 ,l3 S>fpm'2 / ^ 0} 2 da-Lfi 3 clo.^ s 7 daq i 5 cRy r \00 38 ND ?& Continuous lo o l-s ND 1-8 Conlinuous Lt n 3 ii `-I <? ND Contlpuous 6=5 Ta 3 151 / ND 18 Continuous 6 T tq iff 1 7 f* 3- , ^ / W 01 ^ a m ( ^ 2 7-1*! 0 t Y cV > 4 5- (j) ? n 3 15 8 .0 ND 7J Conlinuous L>o 1 oO 32S 7 S' ND 7 -Y Conlinuous C O M M E N T S h i S y n th e tic d ilu tio n w a le r is p re p a r e d w ith la b o ra to ry d e io n iz e d w a te r a n d r e a o e n l g ra d e c h e m ic a ls fE P A /O O O /^ -O I/O O Z ) (21 E a c h b a lc h of d ilu tio n w a e r r s n o t u s e d for m o r e th a n 14 d a y s fo llo w in g Ih e p r e p a r a t io n d a le _______________________________________________ ` N O = N o t D e le c t a b le __________________________ :_______________________________________________________________________________________________________ OLVER LABORATORIES Cenodaphnia dubia S U R V IV A L A N D R E P R O D U C T IO N R E C O R D C L IE N T P E R M I T N O ___________ E F F L U E N T /T O X IC A N T B P Pi P H O T O P E R IO D 16 hr D a y /8 hr N ig h t C O N C E N TR A TIO N REP \Q. '.S u r v iv a l ------ 1 (A) ?/ m C^c\\r<o \ 3 (Ci 4 (D) 4 /F* 5 (F) 7 (G i 8 {HI J TOTAL 10 (J) _ Day 1 o o 0 o 0 0 0 0 0 0 o Day 2 0 O o o o o 0 o o o 0 JOB NO C<?n5__________ __ PAGE i o f --A -- TEST ORGANISM AGE K w.n ) START o f TEST gfc. .A M _ Z _ / _ Z o / j N _ END of TEST 3 A M J g J tfIZ _ L Z 5 L/j2-1_ ------------------_________________________ ______________________ r --------- j R E P R O D U C TIO N C O U N T/D A Y Day 3 o o o o 0 o o 0 o o 0 Day 4 L-14 Day 5 0' Day 6 q O 5 O8 o8 7o i 1 8* A 7 S' *7 H - 7 7` 5? 3 zq o o o o m Day 7 H l* H - J L __ 5" \* ii q 1z If _ 7 l_ TOTAL COMMENTS IX - 7 1 T E S T SO LUTIO N V O L U M E 15 ml T E S T C O N TA IN ER 5 n a/ S IZ E 30 ml FE E D IN G 0 1 ml TYC + .1 2 - ST/go 0 1 ml A LGA E/D A Y H \c?Winr^.S C O N C E N TR A TIO N ^ O% S u r v i v a l Cc*y4yoi / 1 ]V\tDriOVAcio\J\ _____________ T O T A L RHP 1 (A) 2 (B) 3 iC ) 4 (Di 5 (E) 6 (Fi 7 (G 8 (H 9(H 10 (J) Day 1 O O o 1X n o n o o 0 0 0 Day 2 O 0 __ o o o o o 0 0 0 R P P R O n ilC T IO N C O U N T/D A Y Day 3 Day 4 Day 5 Day S Day 7 O <3 Lp f o 5 o Ip ._ __> -- -- O7 0 q 0 7 7 q- u n 3 b> o 2 (O 3 7o q n 7 L> o 1o c H7 o o 0 7O5 3 0 3> a l 3o J l _ TOTAL 17 0 17 aSL n n ao 11 IOL _m _ COMMENTS C O N C E N TR A TIO N %S u r v i v a l \oO REP Day 1 Day 2 1 (A) 2 (Bi 5 3 (C) 4 (D 5 (E) S IF) 7 (G) 8 (H) 9 ID 10 /J1 TOTAL ____________A N A L Y S T ____________ 0 o 0 0 0 D 0 0 o 0 0 L 0 0 0 0 0 o 0 o c o 0 HA' N \TEMP'_ATE\5lOBENCH\CHRONIC.COReROD WPO R E P R O D U C TIO N C O U N T/D A Y Day 3 Day 4 Day 5 O S 5 o5 o 0 *7 o -q - o I 0 7 c? 0 HA o 77 0 77 0 3 C0 07 o vi as Sud -5 t? a Day 6 2 If fp ? Y 0 n n 0 0 3H Mf Day 7 H Lo Lp b b 9 8q i b (p(3 r TOTAL /7 7 ._ / 3 /7 D /7 /? /7 /6 Ito COMMENTS =X D EAD - = D IED P R E V IO U S LY =#S/X O F Y O U N G PRODUCED BEFORE A D U LT DIED Sgls] Resisea 'une CO -000 71 Companyifmmlzed. D oes noi containTSCA CBi C a n a d a p h rv a d u b ia SURVIVAL AND REPRODUCTION RECORD Ol_^.LaOfVtATEQBlRES C L IE N T _ J > U 2 2 n i - i P E R M IT N O _ ------- t lr t E F F L U E N T /T O X 1 C A N T D I L U T I O N W A T E R -----P---P-- A mmu JOB NO oH 5 _____T E S T O R G A N IS M A G E . AM/l^^i A^2-0!LS T A R T of T E S T / :3 Q . PAGE 3T P.1M h f S C th-,* hr E N D of T E S T 3^ KWlfik J _ j2 3 J - ) punfnPFRIOO 16 nr DaV/B hr Nl9hl REPCONCENTRATION ^rinval^O-- Day 1 Day2 1 (A) o J2_ O2 (Bl !L> mf)A_ OJSL 4 IDI (0 O o o _LL 6(FI J2_ 07 (G) J2_ o _Q _ 8(HI 0 9(II o o REPRODUCTION COUNTVOAY Day 3 Day 4 Day5 Day6 Day7 o 1T T j 2_ 5 5 <9 o H oo 3HO G ' (o O o o M3 3 3 8 o 3 o G 3 II to o J2 H- TOTAL COMMENTS "1 3 " i(c 13 11 11 /9 SL ~7T TEST SOLUTION VOLUME 15 ml TPSTCONTAINER SIZE 30 ml FEEDING 0 1 mi 'P 'C - 0 1 mi ALGA0OAY - J1 aI Tom-- CONCENTRATION RHP "/.Survivai=`TO REPRODUC3T1DNCOUNT/DAY Day1 R Day2 o Day3 p Day4 w Day5 DayS --- Day7 l ")m\ O o f. H o Lp 3 Z3 m3/i. fi fFt " ,' o o o o 0 o 0 n3 O <3 03 O o H (r <9 /r o o h-- f) o / 3 ? o 7(G 0 0 o ~~j= r 9> 1 L cfW\ o 0 o 3 A o % 0 0 o 3 "IT - O 2. 10(J) o o 0 4 1 10 TOTAL_ 0 o o 3# m 19 38 TOTAL IX Id cl _1Z_ /G / 2/v 18 II I e! 13 e! COMMENTS CONCENTRATION REP ASurvival0 REPRODUCTIONcount/day Day1 Day2 Day3 Day4 Day5 DayS Day7 TOTAL COMMENTS 1(A) o 0 o 2fBl o O o 3o ^5/l- 3fC 4.(D 0 0 0o 00 5(El o O 0 S(R o 0 0 7fGl o O 0 S/H 0 O n 9(H o 0 0 10fJl o TDTAf o 00 0o ___ ANALYST------- li) HA I U-ft" N.\TEWPLATBBiOBNCH\CHRONiCvCDREPRODWPO o 5o 0? o (& ro 5o W0 G (e l er 3 3 a/ J-k'3 {? 3 1r b3 15 3 3._ (9 L /X Z. 9 03 4 0// to/t 36) zA 6Lb 1 .2 11 X=DEAD 15 1 G - =DIEDPREVIOUSLY 5 i,'X=FOFvOUNG 53 PRODUCEDBEFORE <9... ADULTDIED Il /7 15 3." 15M Revised June 20 2000 7? Company Sanitized. Does not contain TSCAC81 Ceriodaphnia dubia SURVIVAL AND REPRODUCTION RECORD OLVER l_ABOfrATOR<eS JOB NO k 0n5_ PAGE of 3 . C L IE N T _ _ D ii it = . t e s t o r g a n is m a g e . -Ozy h f S ? A'/-J P E R M IT N O e f f l u e n t /t o x ic a n t _ r-ui I iT in w W A T E R __EPf\ '71 S T A R T o f T E S T / '-3Q_ A M E N D of T E S T _J_L AM L A. / z ? / O > PHOTOPERIOO 16 hr Dav/8 hr Night .... ....................-- ---------------- CONCENTRATION REP r-t Q Day 1 Day 2 Rf;produc TON COLNT/UA Day 3 Day 4 Day 5 Day 6 Day 7 TOTAL COMMENTS */ Slir\MYfll= -----1 (A) Jl i 0 _ Q _____ Q ____ ? O (J - o 5 5 Q Os o o 0 h* 5 <2__ O O O. 9 /x 7 /x // <39H / 3 ao t c " T pni i mnw VOLUME 15 ml TEST CONTAINER SIZE 30 ml / On rf'.ci h - Q O o 5 S 0s /7 o 0 o V3 O IO ; 9 FEEDING 1 4O 0 o0 S O 0 VV 0? 0 o /x l L 0 1ml TYC Q1 ini ALGAE/DAY i ___________ _ J _________ IQ IAL---- 10 (J1 0 o Q o o o D *7 .3 0 U O3 oq 9 3 HS o t\ 15 "7 T T CONCENTRATION REP %Survival 4 0 5 o o --R5/^ q (F) " C(F 7 (G) 9 fH) q fn 10 (J| TOTAL ... Day 1 o o 0 O o 0 o o o 0 0 Day 2 n o o 0 o 0 0 0 0 o ___ _ Day 3 o o o o 0 O 0 o 0 D 0 FHPRODUCTION COUNT/DAY Day 4 Day 5 Day 6 Day 7 3 OH // S 5 o IZ 5 OH L S' 5 Ofx -- -/ o 3 5 3 (5 o 7 / * F3 S6 *7 t o 75 33 3 ? /y o jofo o 9/y o /o / x /S ~ T T . TOTAL COMMENTS 15 / (7 /G \ 17 ----------- - m . ... - j 1 CONCENTRATION REP Survival RFPRnnncTION COUNT/DAY Day 1 Day 2 Day 3 Day 4. Day 5 Day B Day 7 TOTAL COMMENTS 1 (A) 2 (B 3 (C 4 fDl X= dead --= DIED PREVIOUSLY 5 (El tt/X = FOF YOUNG G {Fi FRODUCED BEFORE 3 (H) 9 (I) 10 (J! TDTAI ANALY5T .... a N\T.MPLATE'.B'OBNC'H\CHRCNIOCDREPf:?QD'* OA ilA 1 D t \ l S L fy 5U3 AOULT OIFD sygfE . -------- ---------- ---- Bompmy Si,llfe,d. Bo m noi c 0 ,,,aln TSC CBI CHRONIC TOXICITY TEST CHEMICAL ANALYSIS DATA SHEET page I o f _7_ OLVER l a b o r a t o r ie s CLIENT _ D ^ f c-0.jp- JOB NO Cp .13 PERMIT NO _______ EFFLUENT/T0X1CANT DILUTION WATER EPS m H uj INITIAL DAY 1 DAY 2 DAY 3 pH D O. (mg/L) Temperature (C) Conductivity (^m hos/cm ) Hardness (mg/L as CaCOJ > Alkalinity (mg/L as CaCOJ A nalyst's Initials 7 .8 7 -8 z5 3 2 ,4 l8 12 " I S' 23.L 5 m SL& 12 7 aS 33C SLft FINAL pH D.O (mg/L) 75 7H T -3 1M 11 H -T Temperature (C) C onductivity (mhos/cm) Analyst's Initials 3S3 6L ys 353 5l 6 tS 377 SUb DAY 4 78 78 i5 3 i5 TEST INITIATION DATE ,_j-_T_-a__I nl TEST COMPLETION DATE z / l ^ J p A TEST ORGANISM C m r A n i/mm duhi c, ____ PHOTOPERIOD 16-Hour Dav/B-hour Niqnl LIGHT INTENSITY 50-100 rt-C ) DAY DAY DAY 56 7 COMMENTS 7 1 fo 7 3 .5 3 1-1 7 5 2.5 3 15 3 2 8 sUS 52-N $Y/J 5L& 7 5 7 -1 35 347 3au 7U LA L -X 25 337- SH A- INITIAL DAY 1 PH . 1-8 DO. (mg/L) 78 Temperature (C) Conductivity (pmhos/cm) Hardness {mgTLas CaCOa) 2-5 100 Alkalinity (mg/L as CaCO.) Analyst's Initials .5m FINAL pH 7 3 D.O (mg/L) 7-7 Temperature (C) 2.S Conductivity (^mhos/cm) 383 Analyst's Initials aL DAY DAY DAY DAY DAY DAY 7 2 3456 7 S 7 - 7 ? 7 f ? 0 7 ? 7 ? 7 f i ? 7 ? - 1-8 2.5 2.S' IS 7 5 7 5 as 33b 33L. 31S' 3 15 3 * 5 3 3.5 100 joo 1 7T 33. DO l/M lh I'TLz (j3O' k>2 L0 ~- SlIS L& SeN SLiS 7 7-7 7 .4 7 . cl 7 H 7 7 (fi-1 7 .0 xS IT 2 5 7 5 358 377 377 375 SL&- US T 4 n 3(?7 7-0 57 25 32V 6L& 7-L L -7 337 COMMENTS ~Vyfa-n1*C-nWch4___ - 74 C o m p a n y S a iTffeecf. Di o e s m l co p a r i t A C B !  CHRONIC TOXICITY TEST CHEMICAL ANALYSIS DATA SHEEi Pase ~Z- of 3 O LV ER L A B O R A T O R IE S CLIENT _ P uf JOB NO fr t P E R M IT N O __________ E F F L U E N T /T O X iC A N T D IL U T IO N W A T E R : _ EPP m H P TEST INITIATION DATE __ - f c - Q IjO- TEST COMPLETION DATE / 2 3 .Q J --------------- TEST ORGANISM V n o d c p hni& rii, hm ,---------- PHOTOPERIOD 1S-Hoiir Dav/g-Hour Night LIGHT INTENSITY 50-100 ft-C INITIAL DAY 1 pH D.O. (mg/L) Temperature (" C ) Conductivity 0-imhos/cm) Hardness (mg/L as CaCOJ 7 -8 7 -8 z5 354 DAY 2 3 S' 3? 1? 33L DAY 3 3? 3f 05 33L DAY 4 3? 3? 25 3(5 DAY 5 DAY 6 DAY T 7 .7 7S 3 15 0 7J 25 315 32 3? 25 32? COMMENTS A lka lin ity (ng/L as CaCOJ Analyst's Initials FINAL pH D.O. (mg/L) Temperature (C) C onductivity (mhos/cm) Analyst's Initials INITIAL PH D O. (mg/L) Temperature (C) Conductivity (^mhos/cm) "Hardness (mg7L as CaCOJ 5m SL& SU5 $L(V i f c f J i r J 33 8H 25 3SH SLB 38 74 7-5 353 53 3 3 7W 7 -3 31 25 7 9 - 7 .O 3 -5 3 -5 337 337 SU5 5 i t J 3L U3 25 32S SL5 DAY 1 CONCENTRATION DAY 2 DAY 3 DAY 4 (Ti ^ / l DAY 5 DAY 6 7 -8 7-8 2 -5 79 38 2 .5 3 ? 7 P 7 e! O 3 S 1 8 7.? 7 .2 3.5 3.5 V? 3 3 L 3i 5 3 i 5 3 i 5 SL r.L 45 25 335 SUY ---------------- --- ------ DAY T COMMENTS 7 3- 25 325 , -T7] A lk a lin ity (m g /L as C aC O J A n a ly s t's Initials L5m 4L& FINAL pH 33 33 D O (m g/L) T e m p e ra tu re (C ) 3H 3H as" l 5 Conductivity (ymhos/cm) 353 A n a ly s t's In itia ls AL& C& U \TEMPlATBBIOBENCH\CKRONIC\C.-lRONCHE WPQ SL l /5 5 & J S/7 5L 3- 1 3' 2-5 373 st& 7 .5 7. 0 25 1,3 l.o 9 -5 3L L8 3b 345 337. 333 527 U Jy 7P Ir ? 25 33? SL .s. Revise Novem ber 1 2000 75 Company Sanitized. Does not contain TSCA CBI CHRONIC TOXICITY TES i CHEMICAL ANALYSIS DATA SHEET pase "5 of 1 O LV E R L A B O R A T O R IE S CLIENT __D w f on-Vg! JOB NO Oc 1.1 PERMIT NO EFFLUENT/TOXICANT DILUTION WATER. ---- :Pf /TNnL*J TEST INITIATION DATE. _feo .IoL TEST COMPLETION DATE, x ' f el 1oI TEST DRRANISM P?nndo nhn,a. duba-______ PHOTOPERIOD 1fi-Hour Dav/8-Hour Night LIGHT INTENSITY 50-100 ft-s_ INITIAL DAY DAY DAY DAY DAY DAY DAY 123 4 567 pH D O (mg/L) Temperature (C) Conductivity [umhos/cm] Hardness (mg/L as CaCOJ 7 -8 7 -8 *5 TS ? x5 33 L 1'S T? 33L 3 3 "? 7 }7-? 2,5 7 6 3lS 3 i 5 X .o 7S 7$ 3 IE 8S 1-3 a? 325 Alkalinity (mg/L as C aC03) Analyst's Initials 5 /n SL& 5 lA 5V SLV FINAL pH D.O. (mg/L) Temperature (C) Conductivity (unhos/cm) Analyst's Initials INITIAL 37 8 8 33 3H a5 35! <JL& iU L DAY DAY 12 T T 7 .3 1-2 3 - ` (/ . 2 3 - 0 3 ^ ?L 1 6 ? 1 5 2 S' 3 V 5 33 5 328 33T s u y 5Uh US' 2 5 TMe/L. DAY 3 DAY 4 DAY 5 DAY DAY 7 6 pH D.O (mg/L) T e m p eratu re (C) Conductivity (umhos/cm) ^Hardness (mg7L as CaCOJ 1-8 7-S 3-3^, 18 18 IS 33L T8 1-3 25 23 L - 1 5 3 S 7 .3 OY 2 fT 315 3 t 6 y .o 1.2 3 M? !* 1-3 3.5 3.2S Alkalinity (mg/L as CaCOJ Analyst's Initials J5ro SLS FINAL pH D O. (mg/L) 18 qM 11 Temperature (C) 2.5 T5 Conductivity (umhos/cm) 3 2 1 35 8 Analyst's Initials lA N'\TEWPLATc\BI06ENCH\CHRCNlC.ChRCNCHE.WPQ 5(i> iLliy T3 1 IS 3 i 7 .7 - I 7 5 A '5 348 5l& J .N 3 76 J 2 / J 5Li> 1 u T Ip b i L -* 1 5 22 3 3 0 3H I SIA i l A COMMENTS COMMENTS . Revise November 1 2000 Company Saniffeerf. Does no! confaFn TSCA CB1 WM OLVER L A B O R A T O R IE S CLIENT P u fo n T JOB NO '' PERMIT NO EFFLUENT/TOX1CANT DILUTION WATER: -- E PR iTiffui CHRONIC TOXICITY TEST CHEMICAL ANALYSIS DATA SHEET Page H or TEST INITIATION DATE {z-o f o L TEST COMPLETION DATE Z p j j . TEST ORGANISM C t nnrfyl/in/Q -H n/nc---------- DH O TO PE R lO C 15-H our D a v /8 -H our N ight LIGHT INTENSITY 50-100 ft-c INITIAL pH D.O. (mg/L) Temperature (C) Conductivity (jrmhos/cm) Hardness (mg/L as CaCOj) Alkalinity fmg/L as CaCOJ Analyst's Initials FINAL pH D.O. (mg/L) Temperature (C) Conductivity (umhos/cm) Analyst's Initials 1 INITIAL AY 1 DAY 2 DAY 3 DAY 4 DAY 5 DAY 6 DAY 7 COMMENTS 7-8 1 -s H 3 D l T o 3 - 7-8 1S z 5 xs 3 ? 3 2 1 1 l i . 3-S 25 a X 5 T ? a i 33L 33L 31 3 iS 3l i lr (O V lo H i o H i ^ * IO rH LH (Y (oH (ptf O l !e0 5m SUS SLfi. HJy 5 J?is/ SLlV j-Zjj 5/27 k, i if- '^Corr<.cTV-\^MtCntcJ1i Ti 1i 3 34 T3 S (-B> LV 13 L 3 l.o T 5 33 5 A 5EtJ 1 7 1 U "1 1* V <L> L- ^ i,.7- a a s' 311 32.0 SaS S i i t i 6UV SlV CONCENTRATION l O o m 5/<- DAY DAY DAY DAY DAY DAY DAY 7 12 34 56 COMMENTS j pH D.O (mg/L) 7 fl 1 ? 7' 3-? l . l T o 1 - 8 7-8 3 ? 3 ? 3- 1 J 1,2 3 8 Temperature ("C) z-5 iS a as 3 -6 R 5 as Conductivity (umhos/cm) 33L H i 3 16 3 '5 s a i Hardness (mg/L as CaCOJ Alkalinity (mg/L as CaC03) A nalyst's Initials o m SA FINAL pH D.O (mg/L) 3 i q-4 73 TH Tem p eratu re (C) T i l C onductivity (ym hos/cm ) A nalyst's Initials 34? 3LX 5L> SUI N MEMPLAT\lOBENCH\CHRCNICiCHRONCH w p o L 5L&- 5/Za/ 1 -r " M l o 7 L> 3 o 3 .0 G/(,5 L L a i Alo a? 33 3 3 4 3 3 i5 3/7 SUV S tr J 5l 6 7-(, Ll ai 30.S1 SLk - - Revise November 1. 2000 77 smp??y Smilizi not contain TSCA CB1 QoA& IXn^^S'5,- ~Vn ~n- fyfcn^fa/d CcnHol A. FISHER'S EXACT TEST FOR THE DETERMINATION OF SIGNIFICANT DIFFERENCES IN TEST ORGANISM MORTALITY F is h e r's Exact Test NUMBER OF IDEN TIFICATION CONTROL 5 mg/L TOTAL A L IV E 10 10 20 DEAD 0 0 0 TOTAL ANIMALS 10 10 20 C r i t i c a l F i s h e r ' s v a l u e ( 1 0 , 1 0 , 1 0 ) ( a lp 'h a = 0 0 5 ) i s 6 0 b v a l u e i s 10 S ince b is g re a te r th a n 6 0 th e re is no s ig n if ic a n t d iffe r e n c e b e tw e e n CONTROL a n d TREATMENT a t t h e 0 05 l e v e l F is h e r's Exact Test NUMBER OF ID E N T IF IC A T IO N A L IV E DEAD TOTAL ANIMALS CONTROL 10 m g /L 10 0 91 10 10 TOTAL 19 1 20 C r i t i c a l F is h e r 's v a lu e <10,10,1C) !alp h a= 0 05) is S 0 b v a lu e is 9 S in ce b is g re a te r th a n S 0 th e re is no s ig n if ic a n t d iffe r e n c e b e tw e e n CONTROL a n d TREATMENT a t t h e 0 05 l e v e l Olver Laboratories Incorporated 1116 South Main Street Blacksburg, Virginia 2-1060 Phone (540) 552-554S F4.X (540) 552*1715 78 Company Sanitized. Does not contain TSCA CBI Campftf'San ~Vp "ttyg. 54JiAP"fd Carikoj F is h e r's Exact Test NUMBER OF ID E N T IF IC A T IO N CONTROL 25 m g/L + ' TOTAL ALIVE 10 9 19 DEAD 0 1 1 TOTAL ANIMALS 10 10 . 20 C r i t i c a l F is h e r 's v a lu e (1 0 ,1 0 ,1 3 ) (alpha= 0 05) is S 0 b v a lu e is 9 S i n c e b i s g r e a t e r t h a n S 0 m e r e i s no s i g n i f i c a n t d i f f e r e n c e b e tw e e n CONTROL a n d TREATMENT a t t h e 0 05 l e v e l F is h e r's Exact T est NUMBER OF ID E N T IF IC A T IO N CONTROL 50 m g/L ALIVE 10 7 DEAD 0 T TOTAL ANIMALS 10 10 TOTAL 17 3 20 C r i t i c a l F is h e r 's v a lu e (1 0 ,1 3 ,1 0 ) (alph a = 0 05) is 5 0 b v a lu e is 7 S in c e b is g r e a te r th a n S 0 th e re is no s i g n i f i c a n t d iffe r e n c e b e tw e e n CONTROL and TREATMENT a t t h e 0 05 l e v e l 01ver Laboratories Incorporated V y 1116 Smith Mam Street ^ Blacksburg, Virginia 24060 Phone (5*40) 552-5548 PAX (540) 552-1715 79 Company Sanitized. Does not contain TSCA CB! F is h e r's Exact Test NUMBER OF ID E N T IF IC A T IO N A L IV E DEAD TOTAL ANIMALS CONTROL 10 0 i 100 mg/L 73 10 10 TOTAL 17 \ Critical.Fisher's value (10,10,10) !alpha=0 05) is 6 0 b vain Since b is greater than 6 0 there is no significant difference between CONTROL and TREATMENT at the 0 05 level 20 F is h e r's Exact Test NUMBER OF ID E N T IF IC A T IO N CONTROL 500 mg/L TOTAL A L IV E 10 4 14 DEAD 0 6 6 TOTAL ANIMALS 10 10 20 C ritic a l S ince b b e tw e e n F is h e r 's v a lu e (1 0 ,1 0 ,1 0 ) (alcha = 0 05) is 6 0 b v a lu e is 4 is le ss than o r equal to 6 0 th e re is a s ig n ific a n t d iffe re n c e CONTROL a n d TREATMENT a t t h e 0 . 0 5 l e v e l . Olver Laboratories Incorporated Kf 1116 South M ain Street Blacksburg, Virgmta 14060 i>l , - t e nv c 7 z~ <Q n v . c u n cc"> i " i : 80 Company Sanitized. Does not contain TSCA CBl k n q \ H S > S ) - C a m p t v' s n n 4 o tA y u W A C?n~W l ;r o u p i 2 3 4 5 6 Summary o f F is h e r 's E x a c t T e s ts ID E N T IF IC A T IO N CONTROL 5 m g/L 10 m g/L 2 5 mg/ L 50 m g /L 100 m g/L 500 m g/L NUMBER EXPOSED 10 10 10 10 10 10 10 NUMBER DEAD 0 0 1. 1 3 3 S i O lver Laboratories Incorporated 1116 South Mam Street Blacksburg, Virginia 24060 Phone (540) 552-554S FAX (540) 552-1715 81 Company Sanitized. Does not contain TSCA CBt Qo-V<X kna\^b\S- -~Vp ~\Vai tbWxtkM Co^Vroi B. C H I -SQUARE TEST FOR NORMALITY OF DATA T itle F ile . Dupon T o x ic ity -C d u b ia C h ro m c -2 /2 0 /0 1 T ransform - C h i-S quare T e st f o r N o rm a lity NO TR A N S FO R M A TIO N INTERVAL EXPECTED OBSERVED < -l 5 4 0200 4 A c tu a l and E xpected F requencies -1 5 to c -0 5 -0 5 to 0 5 14 5200 14 2 2 .9 2 0 0 27 >0.5 to 1 5 14 5200 12 . >15 4 0200 3 C h i-S q u a re = 1 4412 ( p - v a lu e = 0 8370) ; C r it ic a l C h i-S q u a re = 13 277 ( a lp h a = 0 .0 1 , d f = 4) = 9 488 ( a lp h a = 0 .0 5 , d f = 4) D a t a PASS n o r m a l i t y t e s t ( a l p h a = 0 01) C o n t i n u e a n a l y s i s C. TEST FOR HOMOGENEITY OF VARIANCE - T itle F ile Dupon o cicity-C d u b ia C h ro n ic -2 /2 0 / l T ransform NO TRANSFORMATION B a r t l e t t 's T e st f o r H om ogeneity o f V a ria n ce C a lc u la t e d 31 s t a t i s t i c = 11 0373 (p -v a lu e = 0 0506) D a t a PASS B1 h o m o g e n e i t y t e s t a t 0 01 l e v e l C o n t i n u e a n a l y s i s C r i t i c a l B = 15 0863 = 11 0705 (a lp h a = 0 01, d f = 5) (a lp h a = 0 05, d f = 5) Olver Laboratories Incorporated V 1116 South Main Street Blacksburg, Virginia 24060 Plione (S40) 552-5548 FAX (540) 552-1715 82 Company Sanitized. Does not contain TSCA CUT T^>o-W CorAPO-<\c'0A 4d iWg- 'frW-icaid_0 `iN"Wa\ D. SUMMARY STATISTICS ON REPRODUCTION DATA Title File DuDon Toxicity-C dubia Chronic-2/20/Q1 Transform MC TRANSFORMATION Summarv Statistics on Data TABLE 1 of 2 GRP IDENTIFICATION 1 Control 5 ma/L 3 10 mg/L 4 25 mg/L 5 50 mg/L 6 100 mg/L N 10 10 10 10 10 10 MIN 14 0000 15 0 0 0 0 13.0000 9 0000 10 0000 8.0000 MAX 22 0000 19.0000 21.0000 19 0000 23 0000 22.0000 MEAN 13 0 0 0 0 16 6000 17.1000 13 9000 15.2000 17.2000 Title File Dunon Toxicity-C dnbia Chronic-2/20/01 Transform NO TRANSFORMATION Summary Stati sties on Data TABLE 2 Of 2 GRP IDENTIFICATION 1 Control 2 5 mg/L 3 10 mg/L 4 , 25 mg/L 5 50 mg/L b 100 mg/L VARIANCE 7 7778 2 3778 6 7667 1 0 3222 1 1 9556 14 8444 SD 2 7889 1.1738 2.6013 3 .2128 3 .4577 3.8528 SEM 0 8819 0.3712 0.8226 1.0160 1.0934 1.2184 CV % 15 4937 7 0710 15 .2 1 2 2 23 113 8 2 2 7479 2 2 4003 Olver Laboratories Incorporated V 1115 South M am Street Blacksburg, Virginia 24060 83 Phone (540) 552-5548 FAX (540) 552-1715 Company Sanitized. Does not contain TSCA CB1 f\ocA u,S .C s- E. ANALYSIS OF VARIANCE OF REPRODUCTION DATA Title Dupont File To:ticity-C dubia Chronic-2/2O/Ol Transform A1IOVA Table ~TP ^ W - ,S~VQ. / - y ja fc j ChoVr NO TRANSFORMATION SOURCE Between W i c m n (Error) Total DF 5 54 59 SS 113 9333 477 4000 531 3333 MS 22 7867 8.8407 F 2 5775 (p-value = 0 0366) Critical F = 3 3759 (alpha = 0 01, df = 5,54) ^ = 2 3 3 6 1 (alpha = 0 0 5 , df = 5 , 5 4 ) Since F > Critical F REJECT Ho All equal (alpha = 0 0 5 ) F. DUNNETT'S TEST Title. Dupon File <& Toxicicy-C dubia Chronic-2/20/01 S Transform. NO TRANSFORMATION Dunne11's Test TABLE 1 OF 2 Ho ControlTreatment GROUP IDENTIFICATION TRANSFORMED MEAN MEAN CALCULATED IN SIG ORIGINAL UNITS T STAT 0 05 1 Control 18 .0 0 0 0 18 0 0 0 0 2 5 mg/L 16 6000 16 5000 1 0529 3 10 mg/L l7 1 0 0 0 17 .1 0 0 0 0 6768 4 25 mg/L 13 9000 13 9000 3 0834 * 5 50 mg/L 15 2G00 15 2 0 0 0 2 1057 6 100 mg/L 17 2 0 0 0 17 2 0 0 0 0 o0 1 b Dunne 1 1 critical value = 2 3100 (1 Tailed, alpha = 0 05, df [used] = 5,40) (Actual df = 5,54) Olver Laboratories Incorporated Sf 1116 South M ain Street sS Blacksburg, V irginia 24060 Phone (540) 552-5543 F-VX (540) 552-1715 84 Company Sanitized. Does not contain TSCA CBl t>Q.-Vo f^ncA^ Si-s-- Cciri\P&f\'sr'a 4p JtW- 0> nV c`A Title File Du d o n Dunnett's Test GROUP IDENTIFICATION Transform NO TRANSFORMATION o n to P3 O ABLE 2 ControlTreatment NCM OF REPS MIN SIG DIFF % OF DIFFERENCE (TN ORIG UNITS) CONTROL FROM CONTROL 1 Control 10 5 mg/L 10 3 0715 17 1 1 4000 10 mg/L 10 3.0715 17 1 0 9000 25 mg/L 10 3 .071S 17 1 4 1000 50 mg/L 10 3 0715 17.1 2 8000 100 mg/L 10 3 0716 17.1 0 8000 G. INHIBITION CONCENTRATION ESTIMATE Titl. Dupont -Conyl Toxicity-C dubia C h r o n i c ^ 2 / 2 0 / 0 1 File zonceric Transform. NO TRANSFORMATION GRP IDENTIFICATION MEAN SMOOTHED MEAN CONCENTRATION 1 Control 18 0 0 0 0 18 . o o o o 0 0000 2 5 mg/L IS 6000 IS ..8500 5 .. 0 0 0 0 3 10 mg/L 17 1 0 0 0 I S .. 8 5 0 0 1 0 .. 0 0 0 0 4 25 mg/L 13 ,.9000 1 5 .. 9 2 5 0 25 0 0 0 0 5 50 mg/L 15 . 2 0 0 0 15 9 2 5 0 50 0000 6 100 mg/L 17 2 0 0 0 15 9 2 5 0 100 0000 7 500 mg/L 17 4000 15 . 9 2 5 0 500 0000 estimate with p = 25 is > 500 0 0 0 0 O lvcr Laboratories incorporated ^ U16 South M am Street Blacksburg, V irginia 24060 Phone (540) 552-554S FAX (540) 552-1715 85 Company Sanitized. Does not contain TSCA CBI ----- ---- frnc.\u<.'S- "' "_J " ' -Vo C r^)% ^ pn ^ a n g \ I i a A. FISHER 'S EXACT TEST FOR THE DETERMINATION OF SIGNIFICANT DIFFERENCES IN TEST ORGANISM MORTALITY 11 1 Fisher's Exact Test NUMBER OF IDENTIFICATION DEAD ALIVE TOT.AL ANIMALS CONTROL w/MeOH I 9 5 mg/L 0 10 l , TOTAL 1 19 10 10 20 Critical Fisher's value (10,10,1) (alpha=0.05) is negative no significant difference b value is 0 Fisher's Exact Test nr . NUMBER OF IDENTIFICATION ALIVE CONTROL w/MeOH 10 mg/L 9 9 TOTAL IB DEAD 1 1 2 TOTAL ANIMALS 10 10 20 Critical Fisher's value (10,10,9) (alpha =0.05) is 4.0 . b value a,s 9 Since b is greater than 4 0 there is no significant difference between CONTROL and TREATMENT at the 0 .OS level Otvcr Laboratories Incorporated I I 16 South M a in Street sS Blacksburg, V irg in ia 24060 Phone (540) 552-5548 FAX (540) 552-1715 Company6Sanitized. Does not contain TSCA CBi "f^ O -'V g - Cc. ri\ P o - A -0 a r i ^ r G ^ 6oJ ^U-L CxAt-^ Vng_'VV-ie<.O\ Fisher's Exact Test NUMBER OF IDENTIFICATION ALIVE CONTROL w/MeOH 25 mg/L 9 9 i TOTA.L ie DEAD 1 1 2 TOTAL ANIMALS 10 10 20 Critical Fisher's value (10,10,9) !alpha =0 05) is 4 . 0 b value is 9 Since b is greater tnan 4 0 there is no sigmfleant difference between CONTROL and TREATMENT at the 0 05 level Fisher's Exact Test NUMBER OF IDENTIFICATION ALIVE DEAD TOTAL ANIMALS CONTROL w/MeOH 50 mg/L 9 .7 TOTAL . 15 1 3 4 10 10 20 Critical Fisher's value (10.10,9) (alpha=0 05) is 4 0. b value is 7 Since b is greater than 4 0 there is no significant difrerence between CONTROL and TREATMENT at the 0 05 level Olver Laboratories Incorporated 1116 South M a in Street v\ Blacksburg, Virgim a 24060 Phone (540) 552-554S FAX (540) 552-1715 Company Sanitized. Does not contain T3CA CB1 DaVs- f~r.1n*ciWS*v'-S>-- .C.^*mpcxK-ofxu^itio ~ Corf\v&u\ls. ^oo Q-*kaA roo^y-ic^noi Fisher's Exac t Test NUMBER OF IDENTIFICATION ALIVE DEAD TOTAL ANIMALS CONTROL w/MeOH 9 1 1 0 0 ma/L 73 l 'TOTAL IS 4 10 10 20 Critical Fisher's value (10,10,9) (alpha=0 05) is 4 0 b value is 7 . Since b is greater than 4 0 there is ho significant difference between CONTROL and TREATMENT at the 0.05 level. Fisher's Exact Test NUMBER OF IDENTIFICATION ALIVE DEAD TOTAL ANIMALS CONTROL w/MeOH 500 mg/L 9 4 1 S 10 10 TOTAL 13 7 20 Critical Fisher's value (10,10,9) (alpha= 0 05) is 4.0. b value is 4. Since b is less than or equal to 4 0 there is a significant difference between CONTROL and TREATMENT at the 0.05 level. s? Olver L-aborotones Incorporated 1116 South M am Street & Biackiburg, V irginia 24060 Phone (540) 552-5543 FAX (540) 552-1715 Company Sanitized. Does not contain TSCA CBl 'OQ'Vtx ocxAvVSiS-- ComPzjuf\vn^i "Vo Q>o'Tyo\ l^ v'V^ 5*00 cxt^A-^jt ^ 1?A,aad\ GROUP 1 2 3 4 5 6 Summary of ?isher's Exact Tests IDENTIFICATION NUMBER EXPOSED NUMBER DEAD CONTROL w/MeOH 5 mg/L 10 mg/L 25 mg/L 5 0 mg/L 1 0 0 m g /L 500 mg/L 10 10 10 10 10 10 10 1 0 1 1 3 3 S SIG 0 05 * i Olver Laboratories Incorporated y 1116 South M am Street Blacksburg, Virginia 24060 Phone 1540) 552-5548 FAX (540) 552-1715 89 Company Sanitized. Does not contain TSCA CBl AiAo-Ih^ S --GimoanSAA "V13 Cjn~V,\ \j-a\~W- 5oo AM-- ^.AQtj m g.~i\nQ.o0\ B. CHI-SQUARE TEST FOR NORMALITY OF DATA Title File Dupont Toxicity-C d u m a Chromc-2/20/01 :er Transform Chi-Square Test for Normality NO TRANSFORMATION INTERVAL EXPECTED OBSERVED <-l 5 4 0200 5 Actual and Expected Frequencies -1 5 to <-0.5 -0 5 to 0 5 14 5200 13 22 9200 25 >0 5 to 1 5 > 1 5 14 5200 11 4 0200 3 Chi-Square = 2 6361 (Critical Chi-Square (p-value = 0 6204) 13 277 (alpha = 0 0 1 , df = 4) 9 488 (alpha = 0 05 , df = 4) Data PASS normality test (alpha = 0 01) Continue analysis C. TEST FOR HOMOGENEITY OF VARIANCE Title Dupont File Toxicity-C dubia Chronic-2/20/01 cer Transform NO TRANSFORMATION Bartlett's Test for Homogeneity of Variance Calculated B1 statistic = 20 1697 (p-value = 0 0012) Data FAIL B1 homogeneity test at 0 01 level Try another transformation Critical B 15 0863 (alpha 11 0705 (alpha 0 0 1 , df 0.05, df 5) 5) /A Olver Laboratories Incorporated 1116 South M ain Street Blacksburg, V irginia 2-4060 Phone (540) 552-5548 FAX (540) 552-1715 90 Company Sanitized. Does n o t contain TSCA CB1 D . SUMMARY S T A T IS T IC S ON R EPRO DUCTIO N D ATA Title File wDupont Toxic it' C dubia Chromc-2/20/01 cer Transform NO TRANSFORMATION Summary Statistics on Data TABLE l o f i GRP IDENTIFICATION -> Control w/MeOH 2 5 mg/L 3 10 mg/L 4 25 mg/L 5 50 mg/L 6 100 mg/L N 10 10 10 10 10 10 MIN 0 0000 15 0000 13 0000 9.0000 10 oooo 8.0000 MAX 22 0000 19 0000 21 0000 19 0000 23 0000 22.0000 MEAN 14 3000 16.5000 17 1 0 0 0 13 9000 15 2000 17 2000 Title File Dupont Toxi c1 ty -C dubia Chronlc-2/20/01 *z7/cer Transform: NO TRANSFORMATION Summary Statis ics on Data TABLE 2 Of 2 GRP IDENTIFICATION 1 Control w/MeOH 2 5 mg/L 3 10 mg/L 4. 25 mg/L 5 ` 50 mg/L 6 100 mg/L VARIANCE 36 6778 1 3778 6 7667 1 0 .3222 1 1 9555 14 8444 SD 6 0562 1 1738 2 6013 3 .2128 3 .4577 3 8528 SEM 1 9151 0.3712 0.8226 1 0160 1.0934 1 2184 CV % 42.3512 7 0710 15.2122 23.1138 22.7479 22.4003 Olver Laboratories Incorporated 1116 South M a in Street Blacksburg, V irginia 2-J060 Phone (540) 552-554S FAX (540) 552-17X5 91 Company Sanitized. Does not contain TSCA CBl I3Q-'Va- ^ S - CampoogS^r-, At flrr\v*\S ^ S0 Ml i^Vgc3 VT\ gL'Hio. A g 1 STEEL 's MANY-ONE RANK TEST Title. File GROUP Dupont Toxiclty-C dubia Chronic-2/20/01 2cer Transform NO TRANSFORMATION Steel's Many-One Rank Test - Ho Control Treatment IDENTIFICATION MEAN IN ORIGINAL UNITS RANK SUM CRIT VALUE SIG DF 0 05 1 Control w/MeOH 14 3000 2 5 mg/L 16.6000 119 00 75 00 1 0 . 0 0 3 10 mg/L 17 1 0 0 0 121 00 75 00 1 0 0 0 4 25 mg/L 13.9000 96 00 75 00 1 0 0 0 5 50 mg/L 15 2000 104 50 75.00 1 0 . 0 0 S 100 mg/L 17.2000 122 00 75 00 1 0 . 0 0 Critical values are 1 tailed l k = 5 ) it F. INHIBITION CONCENTRATION ESTIMATE Title File D u p o nt^Bxj Tcxicity-C dubia Chromc-2/20/01 zceric Transform: NO TRANSFORMATION GRP IDENTIFICATION MEAN SMOOTHED MEAN CONCENTRATION 1 Control w/MeOH 14.4000 16 0333 o oooo 2 5 mg/L 16.60 0 0 16 0333 5 0000 3 10 mg/L 17 1000 16 0333 10 0000 4 25 mg/L 13 9000 15.9250 25.0000 5, 50 mg/L 15.2000 15 9250 50.0000 100 mg/L 17.2000 15.9250 100 0000 7 500 mg/L 17 4000 15 9250 500.0000 ICn estimate with p = 25 is > 500.0000 Olver Laboratories Incorporated 1116 South M ain Street Blacksburg, V irginia 24060 Phone (540) 552-5548 F A X (540) 552-1715 92 Company Sanitized. Does not contain TSCA CBi i APPENDIX 8 ACUTE REFERENCE TOXICITY TEST DATA 93 Company Sanitized. Does not contain TSCA CB1 OLVER la b o r a to r ies J . i i _i Company Sanitized. Does not contain TSCA CBt OLVER LABO RATO RIES REFERENCE TOXICITY TEST DATA SUMMARY SHEET PAGE ___ i OF I TESTING MONTH: Cfon toai REFERENCE TOXICANT: C L M o n 'd *. TEST DATEfSI ACUTE TOXICITY TEST RESULTS C erlo d aph n ia Fathead Minnow l/ig- |/ i i lot >/i 1 - ' / | a I o/ CHRONIC TOXICITY TEST RESULTS C e rlo d a p h n ia TEST CONDITIONS TEST ORGANISM AGE DILUTION WATER 1 SOURCE AERATION EPA-MHW OLVER LABS Continuous 1 -VS EPA-MHW Q1..VER LABS Continuous TEST ACCEPTABILITY CONTROL SURVIVAL (90%) loo'/. Ion'/. TEST ORGANISM AGE DILUTION WATER SOURCE AERATION CONTROL SURVIVAL (80%) NO OF CONTROL FEMALES % CONTROL FEMALES WITH 3 BROODS (60%) EPA-MHW OLVER LABS continuous AVE NO YOUNG/SURVIVING FEMALES (15) STATISTICAL RESULTS SURVIVAL IN 100% lcm 95% C I METHOD J2jL o'/. 2.5 3/ l 5.5 5 /l 7 . 1 - 2 - 8 3 / l H-m - (.. i 21L ttkrm ,J5i_A _ ~ k t __ AVE W T/SURV CONTROL (0 25 mg) SURVIVAL IN HIGHEST I JCONC NUMBER OF REPLICATES NUMBER OF ORGANISM/REPLICATE NORMAL DISTRIBUTION? HOMOGENEOUS VARIANCE? NOEC METHOD NOEC SURVIVAL NOEC. REPRODUCTION/GROWTH Fathead Minnow EPA-MHW OLVER LABS continuous G COMMENTS. R itW in C A - W x 'u V j ^ `'+ H i n .. ^ I *\ Company Sanitized. Does not contain TSCA CBl OLVER LA B O R A T O R IE S REFERENCE TOXICITY TEST DATA SUMMARY SHEET PAGE 1 OF I____ TESTING MONTH: Zn,r>l________________ REFERENCE TOXICANT: d 3Vt.riA.fc. 1 TFST DATEfSl ACUTE TOXICITY TEST RESULTS C e rlo d a p h n la Z fn t- z /iu L i Fathead Minnow z / ; t - Z-Ao / d / . CHRONIC TOXICITY T EST RESULTS C e rio d a p h n la Fathead Minnow TFST CONDITIONS TEST ORGANISM AGE DILUTION WATER SOURCE AERATION t H u 04<S EPA-MHW OLVER LABS Conlmuous Z J-A.H5 FPA-MHW OLVER LABS Continuous TEST ORGANISM AGE DILUTION WATER SOURCE AERATION FPA-MHW OLVER LABS continuous EPA-MHW OLVER LABS continuous TEST ACCEPTABILITY CONTROL SURVIVAL (90%) i ooV. lo o / CONTROL SURVIVAL (80%) NO OF CONTROL FEMALES % CONTROL FEMALES WITH 3 BROODS (60%) AVE. NO. YOUNG/SURVIVING FEMALES (15) STATISTICAL RESULTS oUKVIVAL IN TUU/o '-'-'50 QC0/_ p | METHOD ' AVE W T/SURV CONTROL (0 25 mg) o' /. 0 / SURVIVAL IN HIGHEST i 1CONC ? .\ 3lu ^ 1. B - 1 . 5 3 /l II. 1 3 / l / o. Z - /2 oJ/i NUMBER OF REPLICATES NUMBER OF ORGANISM/REPLICATE NORMAL DISTRIBUTION? ip c a m-.r. VH. if HOMOGENEOUS VARIANCE? NOEC METHOD NOEC SURVIVAL NOEC REPRODUCTION/GROWTH SG SG SG COMMENTS: R c-ferLn n -froXv u-P) v~\il-H o lV 'i u n T w M +K <LXf^cHd__V ^ A l N? OLVER L A B O R A T O R IE S REFERENCE TOXICITY TEST DATA SUMMARY SHEET PAGE i O F __ L Company Sanitized. Does not contain TSCA CBI TESTING MONTH: tAcMC-U 2 o p l REFERENCE TOXICANT: fSochurA C V |Uri'4.^.... TEST DATEfSl ACUTE TOXICITY TEST RESULTS C erlodaphnla Fathead Minnow 3 I lb -aU ftlo l 3[zq - ^ h ilo i CHRONIC TOXICITY TEST RESULTS C e rlo d a p h n la TEST CONDITIONS TEST ORGANISM AGE DILUTION WATER SOURCE AERATION U3 cn TEST ACCEPTABILITY CONTROL SURVIVAL (90%) CX.'A Floors FPA-MHW OLVER LABS Continuous I o o '/ 2 EPA-MHW PI VER LABS Continuous oo7. TEST ORGANISM AGE DILUTION WATER SOURCE AERATION CONTROL SURVIVAL (80%) NO OF CONTROL FEMALES % CONTROL FEMALES WITH 3 BROODS (60%) FPA-MHW OLVERLABS continuous AVE NO. YOUNG/SURVIVING FEMALES (15) STATISTICAL RESULTS SURVIVAL IN 100% LC* 95% C ! METHOD 0/ l.(> 3 /l l . i - l . 8 3A. ___ Pv-&b'~ir___ o7 11- H 3 J L lo. fe - 12-1 3Jl AVE. W T/SU pV CONTROL (0 25 mg) SURVIVAL IN HIGHEST JCONC NUMBER OF REPLICATES NUMBER OF ORGANISM1REPLICATE NORMAL DISTRIBUTION'? HOMOGENEOUS VARIANCE? NOEC METHOD NOEC SURVIVAL NOEC RJEPRODUCTION/GROWTH Fathead Minnow EPA-MHW O lVFR LABS continuous COMMENTS: 7T -V\o-y^ rg-ooVA A-- 16-APH-200 I TITLE: Ceriodaphnia dubia Acute Test Reference Toxicant Sodium Chloride Test Date Test Name Mean Mean+2SD Mean-2 S LC50 1 1 /2 0 / 2 0 0 0 01/19/2001 01/19/2001 0 1 /2 2 /2 0 0 1 01/24/2001 02/14/2001 03/16/2001 1.73 2.48 2.48 1.6 8 1.53 2.14 1.55 2 .11 2.23 2.09 1.98 2 .0 1 1 94 3.17 3 10 2.99 2.90 2.84 2.78 1.04 1.36 1.2 0 1.06 1.17 1 10 97 O l v e r L a b o r a t o r ie s . In c Company Sanitized. Does not contain TSC CBI 16-Apr-20Q1 Ceriodaphnia dubia Acute Control Chart Sodium Chloride Reference Toxicant LC50 ( g/L NaCi ) LC50 ------- Mean ------- Mean+2SD ------- Mean-2SD I OLVER LABORATORIES, INC 98 Company Sanitized. Does not contain T SG ACSI % I 6-APR-200 I TITLE: FATHEAD MINNOW ACUTE TEST ___________ Reference Toxicant. Sodium Chloride (o /L )________ Test Date Test Name Mean Mean+2 SD Mean-2SD LC50 1 1 /2 0 / 2 0 0 0 12/18/2000 12/19/2000 12/19/2000 12 /2 0 /2 0 0 0 01/17/2001 02/14/2001 03/29/2001 11.7 9.9 10 8 12 11.4 11 4 1 1.1 11.4 10.80 10.80 11 .1 0 11.16 11.2 0 11.19 11.2 1 13.35 .12.60 13.00 12.82 12.70 12.56 12.49 8.25 9.00 9.20 9.50 9.70 9.81 9.93 O l v e r L a b o r a t o r i e s . In c 99 Company Sanitized. Does not contain TSC CBI 1S-Apr-2001 FATHEAD MINNOW Acute Control Chart Sodium Chloride Reference Toxicant LC50 ( g/L NaCI ) -- LC50 ------- Mean ------- Mean+2SD ------- Mean-2SD OLVER LABORATORIES, INC 1 00 Company Sanitized. Does not contain TSCA CBl i APPENDIX 9 CHRONIC REFERENCE TOXICITY TEST DATA 1 01 Company Sanitized. Does not contain T SC A OBI OLVER laboratories OLVER LABORATORIES REFERENCE TOXICITY TEST DATA SUMMARY SHEET PAGE t OF 102 Company Sanitized. Does no! contain T SC A CBI TESTING MONTH: Z oo REFERENCE TOXICANT: Sodi um C ^ W 'Y e TFST DATEIS! ACUTE TOXICITY TEST RESULTS C erlodaphnla Fathead Minnow TEST CONDITIONS TEST ORGANISM AGE DILUTION WATER SOURCE AERATION EPA-MHW OI-VFR LABS Continuous FPA-MHW OI VER LABS Continuous TEST ACCEPTABILITY CONTROL SURVIVAL (*90%) CHRONIC TOXICITY TEST RESULTS C e rlo d a p h n ia I/ 3 - 1/ 10I o1 TEST ORGANISM AGE DILUTION WATER SOURCE AERATION IB-T-H hfs. EPA-MHW OLVER LABS continuous CONTROL SURVIVAL (*80%) NO OF CONTROL FEMALES % CONTROL FEMALES WITH 3 BROODS (*60%) I uo/. Io I g ci'/. Fathead Minnow '/zz - i/z n/oi UrS- EPA-MHW Ol VFR LABS continuous US / STATISTICAL RESULTS SURVIVAL IN 100% LCyj f 95% C I METHOD AVE NO YOUNG/SURVIVING FEMALES (* 15) AVE W T/SURV CONTROL (*0 25 mg) SURVIVAL IN HIGHEST ( M-o3A-)CONC NUMBER OF REPLICATES NUMBER OF ORGANISM/REPLICATE NORMAL DISTRIBUTION? HOMOGENEOUS VARIANCE? NOEC METHOD NOEC SURVIVAL NOEC REPRODUCTION/GROWTH . O '/. 5 3 ' / Ves JL S-HO <S z-.g.a/u. 0 .7 .S 3//. >0 S Un G 'h i S *in G 'k i S M rti G harwvcVt-i 2 n 3/l 2 o3 /i COMMENTS. Pit-lfOnt-l. -VoM'GC'Vj yts^VV* ujVtc UAvtVM'n ^. I Company Sanitized. Does not contain TSCA CBI OLVER LABORATORIES REFERENCE TOXICITY TEST DATA SUMMARY SHEET PAGE ___L _ 0 F _ J ____ TESTING MONTH: F ^ -W v .Q'Ym Z p p REFERENCE TOXICANT: AOU1C. TOXICIFY TEST RESULTS C erlodaphnla Fathead Minnow IRSI CUNDI I IONS TEST ORGANISM AGE DILUTION WATER SOURCE AERATION oUJ TEST ACCEPTABILITY CONTROL SURVIVAL (90%) EPA-MHW OLVER LABS Continuous EPA-MHW OI VER LABS Continuous STATISTICAL RESULTS SURVIVAL IN 100% TEST ORGANISM AGE DILUTION WATER SOURCE AERATION CONTROL SURVIVAL (S0%) NO OF CONTROL FEMALES % CONTROL FEMALES WITH 3 BROODS (60%) AVE NO YOUNG/SURVIVING FEMALES (15) AVE W T/SURV CONTROL (0 25 mg) SURVIVAL IN HIGHEST ( 3- I 5?,, )CONC NUMBER OF REPLICATES NUMBER OF ORGANISM/REPLICATE NORMAL DISTRIBUTION? HOMOGENEOUS VARIANCE? C e rlo d a p h n la % ln - Z - / / 3 lo I Fathead Minnow z /;z - l-B U5. FPA-MHW OLVER LABS continuous l - M Virs FPA-MHW PI VER LABS continuous top/. IO I Do'/ I d o /. 6 . Cp3 z O / 35 X IQ NOEC REPRODUCTION/GROWTH OLVER LABORATORIES REFERENCE TOXICITY TEST DATA SUMMARY SHEET PAGE ' OF I 104 Company Sanitized. Does not contain TSCA CBI TESTING MONTH: M tw c V i 'l o t , 1 REFERENCE TOXICANT: 5 o J m m I I'S I 0 -M1 (S. ACUIE 1 OXICI fY TEST RESULTS C eriodaphnla Fathead Minnow CHRONIC TOXICITY TEST RESULTS Ceriodaphnla 3/ 15- 3/ 2.1/ 0/ TEST CONDITIONS TEST ORGANISM AGE DILUTION WATER SOURCE AERATION EPA-MHW OLVER LABS Continuous FPA-MHW OLVER LABS Continuous TEST ACCEPTABILITY CONTROL SURVIVAL {2 90%) TEST ORGANISM AGE DILUTION WATER SOURCE AERATION CONTROL SURVIVAL (2 8 0 %) NO OF CONTROL FEMALES % CONTROL FEMALES WITH 3 BROODS (2 6 0 %) ) - e hrs. EPA-MHW Ol VER LABS continuous 1007. ID n o V. Fathead Minnow I--Z H hrs . EPA-MHW O IV FR 1ABS continuous <W STATISTICAL RESULTS SURVIVAL IN 100% LCM 95% C I METHOD COMMENTS: *% AVE NO YOUNG/SURVIVING FEMALES (215) AVE WT /SURV CONTROL (2 O 25 mg) 'g -5 Q., o SURVIVAL IN HIGHEST (H.o /* , )CONC NUMBER OF REPLICATES L NUMBER OF ORGANISM/REPLICATE NORMAL DISTRIBUTION? HOMOGENEOUS VARIANCE? NOEC METHOD NOEC SURVIVAL NOEC R^PRODUCTION/GROWTH is : 07. jo .Vtj. MO frfccl'-S 2 . o 3JL Qi.%. 3A . D .% 1 SJi- 7 3 V. 10 S Vet G It s S MD G Vts. S s K i'i G T-* 3/Ll.-z 3 /l i n-i 3 /l. yV^, v-Ot'VVv "YWg. I -A PR -200 I TITLE: FATHEAD MINNOW CHRONIC-SURVIVAL Test Date 01/04/2001 0 1 /2 2 / 2 0 0 1 01/31/2001 02/05/2001 02/12 /2 0 0 1 03/14/2001 Test Name NOEC 2 2 2 2 1.25 2.5 Mode 2 .0 0 2 .0 0 2 .00 2.0 0 2 .00 Mode/0.5 Mode .5 ________ _ __________ 4.00 4.00 4.00 4.00 4.00 1.0 0 1.0 0 1.0 0 1.0 0 1.0 0 105 O l v e h La b o r a t o r i e s , In c Company Sanitized. Does not contain TSCA CBI 15-Ap r-2001 FATHEAD MINNOW CHRONIC SURVIVAL CONTROL CHART - m - NOEC ------- Mode ------- Mode/0.5 ------- Mode*0.5 - Olver Laboratories, Inc l 06 Company Sanitized. Does no! contain TSCA CB( I S-APR-SO O I TITLE : F A T H E A D MINNOW C H R O N IC -G R O W T H Reference Toxicant: Sodium Chloride (q/L) ______ Test Date Test Name Mode Mode/0.5 Mode 0.5 NOEC _________________ ______________ 01/04/2001 0 1 /2 2 / 2 0 0 1 01/31/2001 02/05/2001 0 2 /12 /2 0 0 1 03/14/2001 2 2 2 2 1.25 1.25 2 .0 0 2 00 2 .0 0 2 .0 0 2 .0 0 4.00 4.00 4.00 4.00 4.00 1 00 1 00 1 00 1.0 0 1.0 0 107 O l v e r La b o r a t o r i e s . In c Company Sanitized. Does not contain TSCA CB1 1 6-Apr-2001 FATHEAD MINNOW CHRONIC GROWTH CONTROL CHART 03 fi "_io-- O-C 5c E I4 CO cn3 o 01112,, z 0 1 /0 4 /2 0 0 1 01/22/2001 NOEC 0 1 /3 1 /2 0 0 1 Mode 0 2 /0 5 /2 0 0 1 ------ 1------ 02/ 12/2001 0 3 /1 4 /2 0 0 1 Mode/0.5 Mode*Q.5 Olver Laboratories, Inc. 108 Company Sanitized. Does not contain TSCA CB1 16-APR-200 1 TITLE: CER10DAPHN1A CHRONIC TEST_SURVIVAL ____________ Reference Toxicant: Sodium Chloride (g/L)_________ Test Date Test Name Mode Mode/0 5 Mode'O 5 NOEC 1 2 /01/2000 12/27/2000 01/03/2001 02/07/2001 03/15/2001 2 1 2.00 2 2.0 0 1.5 2 .0 0 2 2 .0 0 4.00 4.00 4.00 4.00 1.0 0 1.0 0 1.0 0 1.0 0 1 09 Olver Laboratories. Inc Company 'Sanitized. Does no! confalo TSCA CBI 1S-Apr-2001 Olver Laboratories, Inc 11 0 Company Sanitized. Does not contain TSCA OBI ! 6 -APR- 2 0 0 i TITLE: CER10DAPHNIA CHRONIC TEST-Reproduction _____________Reference Toxicant: Sodium Chloride (q/L) ______ __ Test Date Test Name Mode Mode/0.5 Mode' 0.5 12/01/2000 12/27/2000 01/03/2001 02/07/2001 03/15/2001 0 25 0.25 0.25 0.19 0.5 0.25 0.25 0.25 0.25 0.50 0.50 0.50 0.50 0.13 0.13 0.13 0.13 111 O l v e r La b o r a t o r i e s In c Conroany Sanitized. Does not contain TSCA CB1 16-Apr-2001 CER10DAPHN1A CHRONIC REPRODUCTION CONTROL CHART NOEC ( g/L Sodium Chloride ) NOEC ------- Mode ------- Mode/0.5 ------- Mode*0.5 Olver Laboratories, Inc. 11 2 Company Sanitized. Does not contain TSCA CB! APPENDIX 10 DILUTION WATER QUALITY ANALYSES DATA 113 Company Sanitized. Does not contain TSC A CB! OLVER L A B O R A T O R IE S s? * 4 & O LVERLABORATORIES Consulting Engineers . Environmental Laboratories 1116 South Main Street Blacksburg, Virginia 24060 Client Sheet No.: Date: Client: Source: Shipping information: 0004151 Job No.: 30001 May 8,2000 Date Received: 4/12/00 Olver Laboratories incorporated Blacksburg, Virginia Delivered to Olver Laboratones Incorporated by Olver Personnel Sample No.: Date Collected: Time Collected: Description: 123511 4/12/00 9 45 a m and 3:00 p m. EPA Moderately Hard Dilution Water Analysts pH (Laboratory) (EPA 150 1) Alkalinity as CaC03 (EPA 310 1) Conductivity (EPA 120.1 ) Total Cyanide (EPA 335 2) Ammonia as N (SM 4500 NH3,F) Nitrate as N (ERA 352.1 ) Nitrite as N (EPA 354 1) Hardness as CaC03(EPA 200 7) Total Phenols (EPA 420 1) MDL = M inim um Detection Limit N/A = Not Applicable ND = Not Detectable Result 8 09 60 mg/L 317 imhos/cm ND ND ND ND 100 mg/L ND MM, N/A 10 mg/L . 1 0 pmhos/cm 0 005 mg/L 0.1 mg/L 0 1 mg/L 001 mg/L 1 mg/L 0 005 mg/L Date/Time Analyzed 4/12/00, 7 45 pm. 4/20/00, 11 00 a.m 5/02/00,10 45 a m 4/20/00, 8 15am 4/17/00, 5 00 p m. 4/14/00, 3 00 pm. 4/14/00, 1 30 p m. 4/18/00, 5 00 p m 4/24/00, 1 10 pm. Analyst SAH ACC AOO DF SAH BCW SAH HT DF All tests according to Standard Methods for the Examination of Water and Wastewater. 18th Edition, Te?t Methods for Evaluating Solid Waste fPhvsical/Chemican. 2nd and 3rd Editions, and Methods for the Chemical A nalysis of Water and Wastes, EPA By ---------------------Bnt Ritchey Q Laboratory Manager Unless otherwise indicated, this report sets forth the results of our analysis of samples delrvered lo our laboratory and shall nol be construed to be a representation by ver Laboratories Incorporated as to the source or method of procuring such samples All reports are submitted as the confidential property of clients and authonralton or pub ication of any statements contained in our reports is reserved pending our wntten approval Blacksburg, VA (540) 552-6974 114 Page 1 of 6 N SDA T A\LAB\30C301\CLNTSHT\0004151 Company Sanitized. Does not contain TSCA CBl OLVER l a b o r a t o r ie s Client Sheet No Client Date 0004151 Olver Laboratories Incorporated May 8, 2000 Sample No.: Date Collected: Time Collected: Description: 123511 4/12/00 9 45 a.m and 3:00 p m. EPA Moderately Hard Dilution Water Analysis Total Aluminum (EPA 202 2) Dissolved Aluminum (EPA 202 2) Total Arsenic (EPA 200 9) Dissolved Arsenic (EPA 200 9) Total Cadmium (EPA 200 9) Dissolved Cadmium (EPA 200 9) Total Chromium III (EPA 200 9-SM 3500 Cr,D) Dissolved Chromium III (EPA 200.9-SM 3500 Cr,D) Total Hexavalent Chromium (SM 3500 Cr,D) Dissolved Hexavalent Chromium (SM 3500 CrtD) Total Cobalt (EPA 200 9) Dissolved Cobalt (EPA 200 9) Total Copper (EPA 200 9) D is s o lv e d C o p p e r (EPA 2 0 0 9) Total Iron (EPA 235 2) Dissolved Iron (EPA 236 2) Total Lead (EPA 200 9) Dissolved Lead (EPA 200.9) Total Mercury (EPA 245 1) Dissolved Mercury (EPA 245.1) Total Nickel (EPA 200 9) Dissolved Nickel (EPA 200.9) Total Selenium (EPA 200 9) Dissolved Selenium (EPA 200 9) Total Silver (EPA 200.9) Dissolved Silver (EPA 200.9) Total Zinc (EPA 200 7) Dissolved Zmc'(EPA 200 7) Pnonty Pollutant Organics- Acid Compounds (EPA 625): 2-Chlorophenol 2.4- Dichlorophenol 2.4- Dimethylphenol 4.6- Dinitro-o-cresol 2.4- Dmitrophenol 2-Nitrophenol 4-Nitrophenol p-Chloro-m-cresol Pentachlorophenol Phenol 2.4.6- Tnchlorophenol Result 0 005 mg/L ND ND ND ND ND ND ND ND ND ND ND ND ND 0 006 mg/L 0 006 mg/L ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND MP.L 0 003 mg/L 0 Q03 mg/L 0 001 mg/L 0 001 mg/L 0 0001 mg/L 0 0001 mg/L 0 001 mg/L 0 001 mg/L 0 005 mg/L 0 005 mg/L 0 001 mg/L 0 001 mg/L 0 001 mg/L 0 001 mg/L 0 001 mg/L 0 001 mg/L 0 001 mg/L 0 001 mg/L 0 0002 mg/L 0 0002 mg/L 0 001 mg/L 0 001 mg/L 0 002 mg/L 0 002 mg/L 0 0002 mg/L 0 0002 mg/L 0 005 mg/L 0 005 mg/L 10 Ag/L 10 ig/L 10 aq/l 10 A94- 50 Ag/L 10 A9/L 50 A9/L 20 figlL 50 A9/L 10 A9/L 10 aq/l Date/Time Analyzed 5/02/00, 12.00 p m 5/02/00, 12 00 p m 4/25/00, 2:00 p m 4/25/00; 2.00 p m 4/20/00; 9.30 a m 4/20/00; 9 30 a m 4/20/00, 4 00 p m 4/20/00, 4 00 p m 4/13/00,TOT pm 4/13/00,1 30 p m 4/26/00, 3 00 p m 4/26/00, 3 00 p m 4/18/00, 9 00pm 4/1B/00; 9 00 p m 5/03/00; 12 00 p m 5/03/00; 12 00 p m 5/01/00; 2 00 pm 5/01/00; 2 00 pm 4/21/00; 9 00 a m 4/21/00; 9 00 p m 4/18/00; 7 30 a m 4/18/00; 7 30 a m 4/17/00; 11.45 a m 4/17/00, 11 45 a m 4/18/00; 5 00 p m. 4/18/00; 5 00 pm 4/22/00,11.-30 a m 4/22/00; 11.30 a m 4/2B/00;7 56 a m Analyst HT HT HT HT BN BN HT HT SAH SAH HT HT HT/BN HT/BN HT HT HT HT BN BN BN BN BN BN HT HT BN BN JSL Page 2 of 6 N \DATA\LAB\30001\CLNTSHT\0004151 115 ' Company Sanitized. Does not contain TSCA CBI OLVER LABORATORIES Client Sheet No Client Date 0004151 Olver Laboratories Incorporated May 8, 2000 Sample No.: Date Collected: Time Collected: Description: 123511 4/12700 9 45 a m and 3 00 p m EPA Moderately Hard Dilution Water Analysis Pnonty Pollutant Organics (continued) Base/Neutral Compounds (EPA 625) Acenaphthene Acenaphthylene Anthracene Benzidine i Benzo(a)anthracene Benzo(a)pyrene 3,4-Benzofluoranthene Benzo(g,h.i)perylene Benzo(k)fluoranthene Bis(2-chloroethoxy)methane Bis(2-chloroethyl)ether Bis(2-chloroisopropyl)ether Bis(2-ethylhexyl )phthala te 4-Bromophenyl Phenyl Ether Butyl Benzyl Phthalate 2-Chloronaphthalene -4-Chlorophenyl Phenyl Ether Chrysene , Dibenzo(a,h)anthracene 1,2-Dichlorobenzene 1,3-Dichlorobenzene 1,4-Dichlorobenzene 3,3'-Dichlorobenzidine Diethyl Phthalate Dimethyl Phthalate Di-n-Butyl Phthalate 2,4-Dinitrotoluene 2,6-Dinitrotoluene Di-n-Octyl Phthalate 1,2-Diphenylhydrazine Fluoranthene Fluorene Hexachlorobenzene Result ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND MDL 10 Fg/L 10 Ag/L 10 Fg/L 10 u g l l 10 Fg/L 10 Fg/L 10 Fg/L 10 f g/L 10 Fg/L 10 Fg/L 10 FgA10 f g/L 10 Fg/L 10 Fg/b 10 Fg/t 10 Fg/t 10 Fg/L 10 Fg/i 10 Fg/L 10 Fg/L 10 Fg/L 10 Fg/L 20 Fg/L 10 Fg/L 10 Fg/L 10 f g/L 10 Fg/L 10 Fg/L 10 Fg/L 10 Fg/L 10 Fg/L 10 Fg/L 10 Fg/L Date/Time Analyzed 4/28/00, 7 56 a m Analyst JSL Page 3 of 6 N \DATA\LABV30001ICLNTSHT\0004151 116 Company Sanitized. Does not contain TSCA CBI OLVER l a b o r a t o r ie s Client Sheet No Client Date 0004151 Olver Laboratones Incorporated May 8, 2000 Sample No.: Date Collected: Time Collected: Description: 123511 4/12/00 9-45 a m. and 3:00 p m. EPA Moderately Hard Dilution Water Analysis Result Base/Neutral Compounds (EPA 625} (continued). Hexachlorobutadiene Hexachlorocydopentadiene Hexachloroethane lndeno( 1,2,3-cd jpyrene Isophorone^ Naphthalene Nitrobenzene N-Nitrbso-dimethylamine N-Nitroso-di-n-propylamine N-Nitroso-diphenyiamine Phenanthrene Pyrene 1,2,4-Tnchlorobenzene ND ND ND ND ND ND ND ND ND ND ND ND ND MDL 10 ^gIL 10 pg/L 10 pig/L 10 pg/L 10 Aig/L 10 ijqIL 10 figIL 10 figfL 10 f/g/L 10 pg/L 10 Aig/L 10 ig/L 10 Aig/L DatefTme Analyzed 4/28/00, 7 56 a m Analyst JSL Page 4 of 6 N \DATA\LAB\30001 \CLNTSKh0004151 1 17 Company Sanitized. Does not contain TSCACB1 OLVER la b o r a t o r ie s Client Sheet No Client Date 8004151 Olver Laboratories Incorporated May 8, 2000 Sample No.: Date Collected: Time Collected: Description: 123511 4/12/00 9'45 a m and 3 00 p.m. EPA Moderately Hard Dilution Water Analysis Volatile C o m p o u n d s (EPA 624)- Acrolein A crylom tnle Benzene Bromodichlbromethane Bromoform Bromome'thane Carbon Tetrachlonde Chlorobenzene Chloroethane 2 -Chloroethy( Vinyl Ether Chloroform Chloromethane Dibromochioromethane 1.1- Dichloraethane 1.2- Dichloroethane 1.1- Dichloraethene trans-1,2-Dichloroethene 1.2-Dichloropropane ci^-1,3-Dichlorapropene trans-1,3-Dichloropropene Ethylbenzene Methylene Chlonde sym-Tetrachloroethane Tetrachloroethene Toluene 1.1.1-Tnchloroethane 1.1.2-Tnchloroethane Tnchloroethene Tnchiorofluorometha ne Vinyl Chlonde Result ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND Mm. 10 ug/L 10 pg/L 5 pg/L 5 pg/L 5 pg/L 10 g/L 10 pg/L 5 pg/L 10 pg/L 5 pg/L 5 pg/L 10 pg/L 5 pg/L 10 pg/L 5 ng/L 10 pg/L 10 pg/L 5 /g/L 5 xg/L 5 pg/L 5 pg/L 5 pg/L 5 pg/L 5 pg/L 5 pg/L 10 pg/L 5 pg/L 10 ug/L 10 pg/L 10 pg/L Date/Time Analyzed 4/13/00. 4 06 p m Analyst BP Page 5 of 6 N\DATa4aBV50001\CLNTSHH0004151 118 Company Sanitized. Does not contain TSCACB! OLVER la b o r a to r ie s Client Sheet No ci,ent Date Sample No.: i Date Collected: ; Time Collected: i Description: Analysis Pesticides (EPA 608) Aldnn alpha-BHC beta-BHC delta-BHC gamma-BHC Chlordane . 4,4'-DDD ` 4,4'-DDE 4.4'-DDT Dieldnn Endosulfan I Endosulfan II Endosulfan Sulfate Endnn Endnn Aldehyde Heptachlor Heptachlor Epoxide Toxaphene PCBs (EPA 6Q8) PCB-1016 PCB-1221 PCB-1232 PCB-1242 PCB-1248 PCB-1254 PCB-1260 0004151 Olver Laboratories Incorporated May 8, 2000 123511 4/12/00 9:45 a.m and 3 00 p m. EPA Moderately Hard Dilution Water Result ND ND ND ND ND . ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND MfiL 1 Ag/L 1 Ag/L 1 Ag/L 1 Ag/L 1 Ag/L 1 Ag/L 1 Ag/L 1 Ag/L 1 Ag/L 1 ^g/L 1 Ag/L 1 Ag/L 1 Ag/L 1 Ag/L 1 Ag/L 1 Ag/L 1 Ag/L 1 Ag/L 50 Ag/L 50 Ag/L 50 Ag/L 50 Ag/L 50 Ag/L 50 Ag/L 50 Ag/L Date/Time Analyzed 4/21/00. 9 26 p m Analyst SD 4/21/00. 9 26 p m SD Page 6 of 6 1 19 N \DATA\LABV3000 UCLNTSHTtOOOd 151 Company Sanitized. Does not contain TSCA CBI / .} Si c h ain of Custody record .< Consulting Engineers and Environmental Laboratories Q i w p p 1116 South Main Street Blacksburg, Virginia 24060 lXborat^ S Telephone: (540) 552-6974 FAX: (540) 552-1715 Client:_______ Giver laboratories. Incorporated Company Contact: Bioassav Laboratory_______I-------------------------Address: T .. 111 6 South Main Street. Blacksburg. V A 2406Q. * Client should complete ill information requested lojhe nghl and in the unshaded areas below, DO HOT WRITE IN THE SHADED AREAS Telephone:_______ (540) 552-6974 ---------------------------------- -- ttl%J ViJttJ- u!<luu't " U p*||jUS AUtKlUIOg Sahft&ed. Does not contain TSCA CBI y Pl 1\/F R CHAIN OF CUSTODY RECORD Consulting Engineers and Environmental Laboratories 1116 South Main Street Blacksburg, Virginia 24060 Telephone: (540) 552-6974 FAX: (540) 552-1715 Client., Diver I ,abnmtnries. Incorporated, Company Contact:_Bioa.ssny Laboratory Address;_____ --------1--1--1-6---South' 'M' ai`n nS`tr-eet. p inr-Kshnrp. VA 24060- I APPENDIX 11 CHEMICAL ANALYSES OF BRINE SHRIMP AND YCT FOOD MIXTURES 1 22 Company Sanitized. Does not contain TSCA CB1 OLVER L A B O R A T O R IE S 1300 Blue Spruce Drive, Suite C Fort Collins, Colorado 80524 Toll Free: 800/331-5916 Tel: 9 7 0 / 4 8 4 - 5 0 9 1 F a x : 9 7 0 / 4 8 4 - 2 5 1 4 SALMON STARTER #1 38- 4763- 91-50 PROCESS DATE: 07/ 26/00 GUARANTEED ANALYSIS Crude Protein, Min . .......................... 55 0% Crude Fat, Min....... ................................15.0% Crude Fiber, Max..... i .................................2 0% Toxic Metals ajid Pesticide Analysis (Note: This analysis is on Lot 3/16/00) Perform ed by Energy Labs, Billings, MT A lum inum Arsenic C ad m iu m C hrom ium C o b alt Copper Iron Lead M ercury Nickel Silver Zinc Total Metals Detection Limit "g/g 5 5 1 5 5 5 5 5 1 5 5 5 Result "g/g 20 <5 <1 <5 <5 9 347 <5 <1 <5 <5 103 FPA Methods 8081: Orssnochlorme Pesticides & 8082. PCBTs Analys s Report Compound* Result Compound* RESU LT ug/g A ldrin alpha-BHC beta-BHC delta-BHC gamma-BHC (Lindane) alp h a -C h lo rd a n e 2 amma-ChIordane 4,4' -D D D 4.4' -D D E 4,4' -D D T D ieid rin Endosulfan I Endosulfan Q Endosulfan sulfate Endrin <0.10 Endrin ketone <0.10 H ep tach lo r <0.10 Heptachlor eponde <0.10 M ethozvchlor <0.10 C hlordane (technical) <0.10 Toxapbene <0.10 Aroclor-1016 <0.20 Aroclor-1221 <0.20 Aroclor-1232 <0.20 Aroclor-1242 <0.20 Aroclor-1248 <0.10 Arocior-1254 <0.20 - Aroclor-1260 <0.20 Aroclor-1262 <0.20 Aroclor-1268 <0.20 <0.10 <0.10 <1.0 <1.0 <10 <2.0 <4.0 <2.0 <2.0 <2.0 <2.0 <2.0 <2.0 <2.0 E ndrin aldehyde <0.20 Compound analyzed for but not detected. INGREDIENTS v ct, r Fish Meal, Soy Flour, Com Gluten Meal, Blood Meal, Fish Oil, Liquid Fish Solubles, Torula Dried Yeast, Brewers Yeast, Soy LecUmn, Lignm Sulfonate, L-Ascorbyl-2-Polypbospbate (Vitamin C), Cholme Chloride, Ethoxyqum (preservative), Canthaxanthin (piggienting agent). Vitamin B12 Supplement, Niacin, Calcium Pantothenate, Riboflavin, Pyndoxme Hydrochloride, Vitamin A Acetate, D-Acuvatcd Animal Sterol (source of Vitamin D3), Thiamine Mononitrate, Folic Acid, Biotin, dl-Alpha Tocopherol Acetate (source of Vitamin E), Menadione (Vitamin K), Zinc Sulfate, Copper Sulfate, Manganous Sulfate, Ethylenediarrune Dihydroiodide, Cobalt Carbonate, Ferrous Sulfate, Calcium Carbonate MANUFACTURED BY: ZEIGLER BROS., INC. P.O. BOX 95, GARDNERS, PA 17324 Aquatic BioSystems, Inc Quality Research Organisms 123 Company Sanitized. Does not contain TSCA CB1 1300 Blue Spruce Drive, Suite C Fort Collins, Colorado 80524 Toll Free: 800/331-5916 Tel: 970/484-5091 Fax:970/484-2514 YTC TOTAL SOLIDS MEASUREMENT (Methodfrom EPA/505/8-89-002a) YTC Process Date: Average Total Solids 12/4/00: Best if used by 04/30/01 1760 mg/1 ingredient TOt Numbers _- Pines International Wheat Grass WG98S00090; Zeigler Salmon Starter#!: 38-4763-9150, Fleischmanns Yeast- G-3 Analyzed Metals A lu m in u m Arsenic Cadmium i Chromium ' Conner Iron Lead M ercury Nickel Silver Zinc EPA Required Toxic Metals Report Limits Results (msfL) Compounds 0.1 0.005 <0.1 <0.005 Aldrin alpha-BHC 0.001 <0.001 beta-BHC 0.01 <0.01 delta-BHC 0.01 0.01 gamma-BHC fLindane) 0.03 0.18 alpha-Chlordaue 0.01 <0.01 g am m a-C hlordane 0.001 <0.001 4,4' -D D D 0.01 <0.01 4.4' - DDE 0.005 <0.005 4,4' -DD T 0.01 0.42 Dieldrin Endosulfan I Endosullan H Endosulfan sulfate Endrin Endrin aldehyde Endrin ketone Heptachlor Heptachlor epoxide M ethozychlor Chlordane (technical) Toxaphene Aroclor-1016 Aroclor-1221 Arodor-1232 ArocIor-1242 Aroclor-1248 Arodor-1254 Aroclor-1260 ArocIor-1262 Aroclor-1268 Results (ug/L) <2.0 <2.0 <2.0 <2.0 <2.0 <2.0 <2.0 <4.0 <4.0 <4.0 <4.0 <2.0 <4.0 <4.0 <4.0 <4.0 <4.0 <2.0 <2.0 <20 <20 <200 <40 <80 <40 <40 <40 <40 <40 <40 <40. Qualifier U -U U u u .u u u u u u u u u u u u u u u u u u u u u u u u u U - Indicates compound was analyzed for but not detected ""Testing performed by Energy Labs, Billings, Montana Aquatic BioSystems, Inc Quality Research Organisms Company SaAffed. Does not contain TSC CBl OLVER Consulting Engineers Environmental Laboratories laboratories 1116 South Main Street Blacksburg, Virginia 24060 Client Sheet No.: 0005275 Job No.: 60001 Date: July 11,2000 Date Received: 5/25/00 Client: Olver LaboratoriesIncorporated Source: Blacksburg, Virginia Shipping information: Delivered to Olver Laboratories Incorporated by Olver Personnel Sample No.: Time Collected: Date Collected: Description: Analysis Total Aluminum (EPA 202.2) Total Arsenic (EPA 206 2) Total Cadmium (EPA 213 2) Total Chromium (EPA 218.2) Total Cobalt (EPA 219.2) Total Copper (EPA 220 2) Total Iron (EPA 200.7) Total Lead (EPA 239 2) Total Mercury (EPA 245.1) Total Nickel (EPA 200 9) Total Silver (EPA 272 2) Total Zinc (EPA 200.7) 124686 3:45 p m. 5/25/00 Tetramin Flakes (Lot No. 121599) Result MEL Analyzed Analyst 350 ND 0.0125 1 05 0.425 13.3 905 0 275 ND 13 0.055 82 3 mg/kg as received mg/kg as received mg/kg as received mg/kg as received mg/kg as received mg/kg as received mg/kg as received mg/kg as received mg/kg as received" mg/kg as received 31 2 0.15 0 005 0.15 . 0.05 05 0 35 0.05 0.25 0.05 0 01 05 mg/kg as received* mg/kg as received mg/kg as received mg/kg as received mg/kg as received mg/kg as received* mg/kg as received mg/kg as received* mg/kg as received mg/kg as received mg/kg as received mg/kg as received 6/27/00; 8 00 a m. 7/01/00; 10.00 a.m. 6/19/00; 11.30 a.m. 7/10/00; 1 30 p.m. 6/29/00; 1.00 p m. 6/14/00; 3.00 p m. 6/22/00; 2.00 p m. 6/23/00; 2.00 p m. 7/05/00; 2:00 p m 7/05/00; 2:00 p.m 6/27/00; 3-00 p m. 6/27/00; 8:00 a m AMT BN ' AMT BN HT HT HT HT HT HT/BN HT AMT MDL = Minimum Detection Limit ND = Not Detectable * Sample required dilution: MDL was raised accordingly. ** Due to low spike recovery, the Method of Standard Additions was used to analyze this sample. All tests according to Standard Methods for the Examination of Water and Wastewater. 18th Edition, Test Methods for Evaluating Solid Waste iPhvsical/ChemiGall. 2nd and 3rd Editions, and Methods for the Chemical Analysis of Water and Wastes. EPA. By Brit Ritchey Laboratory Manag U nless otherwise indicated, thus report sets forth the results of our analysis of samples delivered to our laboratory and shall not be construed lo be a representation by Olver Laboratories Incorporated a s to the source or method of procuring such samples. Ail reports are submitted as the confidential property of clients and authorization for publication of any statements contained in our reports is reserved pending our written approval Blacksburg, VA (540) 552-6974 125 Page 1 of 4 P \DATAIBIO\60001\CINTSHTI0005275 Company Sanitized. Does not contain TSCA CBI OLVER LABORATORIES Client Sheet No Client Date , Sample No.: Time Collected: Date Collected: Description: Analysis Pesticides {EPA 608)' - Aldnn alpha-BHC beta-BHC delta-BHC gamma-BHC i Chlordane 4,4'-DDD 4,4'-DDE 4,4'-DDT Dieldnn Endosulfan I Endosulfan II Endosulfan Sulfate Endnn Endnn Aldehyde Heptachlor . Heptachlor Epoxide Toxaphene PCBs (EPA 608): PCB-1016 PCB-1221 PCB-1232 PCB-1242 PCB-1248 PCB-1254 PCB-1260 0005275 Olver Laboratories Incorporated July 11, 2000 124686 3:45 p.m. 5/25/00 Tetramin Flakes (Lot No. 121599) Bssu ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND MOL 5 Aig/kg as received 5 iig/kg as received 5 pig/kg as received 5 Aig/kg as received 5 Aig/kg as received 50 g/kg as received 5 figi\g as received 5 g/kg as received 5 pg/kg as received 5 /jg/kg as received 5 #jg/kg as received 5 g/kg as received 5 Aig/kg as received 5 Aig/kg as received 5 pg/kg as received 5 Aig/kg as received 5 g/kg as received 50 Aig/kg as received 50 fig/kg as received 50 Aig/kg as received 50 ^g/kg as received 50 g/kg as received 50 pg/kg as received 50 pg/kg as received 50 figfkg as received Date/Time Analysed 6/06/00; 5.56 a m. 6/06/00, 5:56 a.m Analyst asm/pmw ASM/PMW Page 2 of 4 126 P \DATAVBlO\600Q1\CLNTSH'n0005275 Company Sanitized. Does not contain TSCA CBl OLVER l a b o r a t o r ie s Client Sheet No Client Date 0005275 Olver Laboratories Incorporated July 11,2000 Sample No.: Time Collected: Date Collected: Description: 124687 3:45 p.m. 5/25/00 TYC (Lot No. 51900) Analysis Total Aluminum (EPA 202.2) Total Arsenic (EPA 206.2) Total Cadmium (EPA 213.2) Total Chromium (EPA 200.9) Total Cobalt (EPA 219.2) Total Copper (EP/k 2202.) Total Iron (EPA 200.7) Total Lead (EPA 239.2) Total Mercury (EPA 245.1) Total Nickel (EPA 200 9) Total Silver (EPA 272 2) Total Zinc (EPA 200.7) Pesticides (EPA 608): Aldnn alpha-BHC ' beta-BHC delta-BHC {jamma-SHC Chlordane 4.4'-DDD 4,4'-DDE 4,4'-DDT Dieldnn Endosulfan I Endosulfan ll Endosulfan Sulfate Endnn Endnn Aldehyde Heptachlor Heptachlor Epoxide Toxaphene PCBs (EPA 608): PCB-1016 PCB-1221 PCB-1232 PCB-1242 PCB-1248 PCB-1254 PCB-1260 Result 0.118 mg/L 0.22 mg/L'* NO 0.004 mg/L ND 0 054 mg/L 0.372 mg/L 0.012 mg/L ND 0.004 mg/L ND 0.521 mg/L ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND MEL Date/Time Analyzed Analyst 0 025 mg/L* 0.15 mg/L* 0.0001 mg/L 0001 mg/L 0.001 mg/L 0.001 mg/L 0.007 mg/L 0.1 mg/L' 0.25 mg/L 0.001 mg/L 0.0002 mg/L 0 005 mg/L 5 zg/kg as received 5 zg/kg as received 5 zg/kg as received 5 zg/kg as received 5 zg/kg as received 50 zg/kg as received 5 zg/kg as received 5 zg/kg as received 5 zg/kg as received 5 zg/kg as received 5 zg/kg as received 5 g/kg as received 5 zg/kg as received 5 zg/kg as received 5 zg/kg as received 5 zg/kg as received 5 zg/kg as received 50 zg/kg as received 50 /jg/kg as received 50 zg/kg as received 50 zg/kg as received 50 Azg/kg as received 50 /zg/kg as received 50 /zg/kg as received 50 /zg/kg as received 6/27/00; 8:00 a.m 7/01/00; 10:00 a m. 6/19/00; 11:30 am. 7/07/00; 11.30 am. 6/29/00. 1:00 p.m. 6/14/00; 3:00 p.m. 6/22/00; 2:00 p.m. 6/23/00; 2:00 p m. 6/26/00; 10.00 a m. 7/05/00; 2:00 p m. 6/27/00; 3.00 p m. 6/27/00; 8:00 a m. 6/06/00; 6.24 a m. 6/06/00; 6.24 a m. 'A* AMT BN AMT BN HT HT . HT HT AMT HT/BN HT AMT ASM/PMW ASM/PMW * Sample required dilution; MDL was raised accordingly. ** Due to low spike recovery, the Method of Standard Additions was used to analyze this sample Page 3 of 4 127 P \OATA\BiO\6Q001\CLNTSHT\0005275 Company Sanitized. Does not contain TSCACBI OLVER LABORATORIES Client Sheet No Client Date 0005275 Olver Laboratories Incorporated July 11, 2000 Sample No.: Time Collected: Date Collected: Description: 124688 5:00 p.m. 5/25/00 Brine Shrimp Nauplii (Lot No. 4400) Analysts Total Aluminum (EPA 202.2) Total Arsenic (EPA 206.2) Total Cadmium (EPA 213 2) Total Chromium (EPA 200.9) Total Cobalt (EPA219.2) Total Copper (EPA 220 2) Total Iron (EPA 200.7) Total L e a d (EPA 239 2) Total Mercury (EPA 245 1) Total Nickel (EPA 200.9) Total Silver (EPA 272.2) Total Zinc (EPA 200.7) Pesticides (EPA 608): Aldnn alpha-BHC beta-BHC - " detta43HC gamma-BHC _ Chlordane 4.4 - ODD 4,4'-DDE 4.4- DDT Dieldrin Endosulfan I Endosulfan II Endosulfan Sulfate Endnn Endnn Aldehyde Heptachlor Heptachlor Epoxide Toxaphene PCBs (EPA 608). PCB-1016 PCS-1221 PCB-1232 PCB-1242 PCB-1248 PCB-1254 PCB-1260 Result 0.007 0.08 ND 0 001 ND 0 015 1.04 ND ND 0.003 ND 0 069 mg/L mg/L** mg/L mg/L mg/L mg/L mg/L ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND MDL Date/Time Analyzed ' Analyst 0.005 0.15 0.0001 0.001 0.001 0 001 0 007 0.1 0 25 0.001 0.0002 0 005 mg/L mg/L* mg/L mg/L mg/L mg/L mg/L mg/L* mg/L mg/L mg/L mg/L ' 5 g/kg as received 5 g/kg as received 5 ud/kq as received 5 g/kg as received 5 g/kg as received 50 g/kg as received 5 g/kg as received 5 j.g/kg as received 5 fj.g/kg as received 5 g/kg as received 5 g/kg as received 5 g/kg as received 5 xg/kg as received 5 g/kg as received 5 g/kg as received 5 /g/kg as received 5 g/kg as received 50 u/kd as received 50 /g/kg as received 50 /g/kg as received 50 /g/kg as received 50 /g/kg as received 50 /g/kg as received 50 /g/kg as received 50 /g/kg as received 6/27/00; 8 00 a.m. 7/01/00; 10.00 a.m 6/19/00,11:30 a.m. 7/07/00; 11:30 a.m. 6/29/00, 1.00 p.m. 6/14/00. 3 0 p.m. 6/22/00, 2:00 p.m. 6/23/00. 2.00 p m 6/26/00; 10:00 a m 7/05/00, 2-00 p m 6/27/00. 3 00 p.m 6/27/00; 8:00 a m 6/06/00; 6:53 a m. 6/06/00, 6 53 a.m AMT BN AMT BN HT HT HT HT AMT HT/BN HT AMT ASM/PMW ASM/PMW * Sample required dilution; MDL was raised accordingly. ** Due to low spike recovery, the Method of Standard Additions was used to analyze this sample. Page 4 of 4 128 P \OATA\BIOU50001\CLNT5HT10005275 Company Sanitized. Does not contain TSCA CB1 ) Auti k V CHAIN OF CUSTODY RECORD S Consulting Engineers and Enviionmenlal Laboratories Q | w p p 1116 South Main Street Blacksburg, Virginia 24060 l a b o r a t o r ie s Telephone: (540) 552-6974 PAX: (540) 552-1715 * Client ihuuld cmplele sil information requested to (he right ami in the unshaded areas below DO NOT WRIT IN D lC SIIADHU AKUAS * Sample] w ill be discarded or relumed lo the client two weeks after (he analytical report has been nulled, unless prior irfiig c n ic M i have been made Client: Olvic-r L abor^T ori^s X uC . Company Contact: 5>ioo.->sqM L-a,bnoykirjj - (Smi Address:_____ ~ - _____________________________ T e le p h o n e :_______ Purchase Order No., C o m p o s ite ( / ) # o r C o n ta in e rs c s in c n .S 3 JuUi lo o o o \ O lv c r S a m p le 10 H p ii S a m p le L o c a llo n (i c , in d u c ili, m u ra li 001, M W I, ele ) D a le C o lle citd Tim e C o lle citd S a m ple Type C o nta iner I ype /J d ! /Jo 'L ' T ^ ir e s m io F ta K c S L o -t i z is n n ^ Z 5 j 2 M 's F o p - -D--------- pf --m------ 6 o u r C t P T *vc_ fe a J, P re ie rva llo n W o n t. eL3t. A n a ly s e r t u q u e sIc d O T o - M IAe-V<LK-. BA / A3 A h A S ,c r, c d .c u ,C o , P c, p b ,u r,7 .n . i/ 1 P L cA L l A j p C f t S ^ " m c lA vo A G ,0 < ? 3 1 2- W fe> 7 7 " ' r * '/ /JO T TC - Food M ix P u rC L d+. S I T o d 5 h 5 o o 2^6 -----------o\--m f\& A t. MA K lo n . Tb-p.1 N s T A \i. m .A n e - " ! f t ! , A 5 , C r , C d ( C u . C o , p t , f A s J d J iT L A 1 p * y H c . ( <**>./D -- % { n i c - i h o c ) Gd o ? 3 '-s S d B n o i 5 onVip Ln+ K J o u tp li/ -- 5 [V 5 )c o c ro o 5 p h -i f\& A&~ ^A W on* U -'' / 1 T b-W N K'C +'cAS.* H\ # .I, f K i . C r . C i C u , C o , p ii , Z r f B i y A ' _i'd s j C M ic tU o d 6 q 8 ^ S u m p lc i(s ) (S g n a lu re ) 4 L0 V il itc ln iq u is h c d B y* (S ig n n lu :) A A U / ild i Itc lin c |tii.s lic d C fy^ ( S ig i'iiilu ic ) R e lin q u is h e d B y : (S ig n n lu ic ) Dale 1mn. R e c e i v e d B y ( S i g n a t u r e ) Date Time R e e l e d B y : ( S i g n a t u r e ) 1 Dale lim e R e c e iv e d B y : (S ig n a tu re ) 1 S p e c ia l In s tru c tio n s | 6 e . iW 'u J r t u r < ir A r p r s s ii u S . d A Y ] Dale %% Date lim e i'3 n Time T e m p e ra tu re U jio n rc c c ip l in lo ll = , S am ples tra n sp o rte d o n ice? Yes M e th o d o f S h ip m e n t. Hu 1 Dale lime C o m m e n ts C jf i l O V'J. **i**t*w * - ul