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VlR. - 0 7 3 / BIODEGRADATION (301 E) TEST SUBSTANCE Identity: A mixture containing perfluorooctanesulfonate, which may also be referred to as PFOS, FC-95, or as a component of FC-203A or of FC-203 NFP. (1-Octanesulfonic acid) (CAS # 2795-39-3). Remarks: The 3M production lot number was not noted. The test sample is FC-203 NFP Current information indicates it is a mixture of 1.34% PFOS, 25% diethylene glycol butyl ether, 67.85% water, 2.66 % Sultone foamer, 3% sodium octyl sulfate, 0.1% sodium lauryl sulfate, and 0.05% tolyltriazole. The following summary applies to a mixture with incompletely characterized concentrations o f impurities. Data may not accurately reflect degradation potential of the fluorochemical component o f the test sample. METHOD____________________________________________________ Method: Modified OECD Screening Test, OECD 301E, with DOC Analysis, 1981 version. Test type: Ready Biodegradability GLP: No Year Completed: 1982 Analytical monitoring: Dissolved organic carbon (DOC) Statistical methods: Results were determined by calculation of the % DOC removal and graphic interpretation. Test organism source: A 50:50 mix of soil extract and secondary effluent. The secondary effluent was the supernatant from an activated sludge aeration basin at the Metro Wastewater Treatment Plant, St. Paul, MN, while the soil was from the City of White Bear Lake, Ramsey County, MN. Test condition: Dilution water: Deionized water Mineral Nutrient Medium: Nutrient medium per OECD 301E method (1981). Initial pH 7.0. Reference and test solution preparation: The test material was prepared by dissolving 153 mg in two liters of mineral nutrient medium. This solution gives a final test concentration of 20 mg DOC/L. The reference substance, sodium benzoate, was prepared by dissolving 30.3 mg in one liter of mineral nutrient medium. This solution gives a final test concentration of 20 mg DOC/L. Test vessels: Not given. Incubation conditions: Constant dark conditions Temperature: 23.5 - 24C Agitation: Continuously Number of concentrations: 1 plus sodium benzoate (reference substance) and blank, ail in duplicate. 000310 Inoculum condition on te s t in itia tio n : Not given . Element Basis: Decrease in dissolved organic carbon compared to the blanks. Test substance fla sk con dition s: Not given. RESULTS__________________________ _________________________ Nominal concentrations: Blank control, sodium benzoate at ~20 mg DOC/L and at ~20 mg DOC/L plus HgCL2 (inhibited), test material at ~20 mg DOC/L and at -2 0 mg DOC/L plus HgCh, all in duplicate. Element values: 27-day Degradation = 76.7% duplicate 1 and 81.3% duplicate 2. Mean value = 79% Remarks: Testing was conducted on the mixture as described in the Test Substance Remarks field. The values reported apply to that mixture and not the fluorochemical proportion alone. CONCLUSIONS_______________________________________________ The FC-203 NFP % degradation based on the mean DOC removal value was 79 after 27 days. Subm itter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 DATA QUALITY_______________________________________________ Reliability: Klimisch ranking = 2. This study meets the criteria for quality testing. However, the sample purity was not properly characterized and the study lacks analytical confirmation of the amount of fluorochemical proportion in the solution. REFERENCES________________________________________________ The studies were conducted by the 3M Company, Environmental Laboratory, St. Paul, MN, Lab Request number 8483, 1982. OTHER______________________________________________________ Last changed: 6/28/00 000911 3E0 Form 6 7 4 7 -1 1-A 1 TECHNICAL REPORT SUMMARY TO: TECHNICAL COMMUNICATIONS CENTER - 201-2CN Date 6/30/8C (Important --I f report Is printed on both sides o f paper, send two copies to TCC.) Division Environmental Laboratory (EE & PC) bept. Number 0535 P ro je c t Project Num ber Commercial Chemicals Division 9970012600 Report Title Report Number Biodegradation of "LIGHT WATER" Products in OECD Test-6/80 TO 040 John A. Pignato - Commercial Chemicals Division - 236-2A (01) Author(s) Employee Number(s) Eric A. Reiner - Environmental Lab (EE&PC) - 21-BW (63 : 47816 Notebook Reference No. of Pages Including Coversheet None - See 3M Environmental Lab Request No. 5541S 31 SECURITY ES Open Closed 3M CHEMICAL ^ REGISTRY " New Chemicals Reported Yes H No KEYWORDS: (Select terms from 3 M Thesaurus. Suggest other applicable terms.) Environment al Laboratory (EE & PC) CUR R EN T OBJECTIVE: To use the internationally recognized OECD Screening Test with DOC analysis to show that "LIGHT WATER" products are highly biodegradable. AFFF TOC R E P O R T ABS TR A C T: (2 0 0 -2 5 0 words) This abstract information is distributed by the Technical Communications Center to alert 3M'ers to Company R & D . This study used the "Modified OECD Screening Test with DOC Analysis" and supplemental parallel sterile controls to conclusively demonstrate the extensive biodegradability of "LIGHT WATER" Brand AFFF products: FC-203, FC-206, and FC-3017. In 14 days, the dissolved organic carbon (DOC) levels of FC--206 degraded by 90% and FC-3017 was 94% degraded. FC-203 showed 93% DOC degradation in 21 days. The parallel sterile controls proved that this DOC loss was not due to chemical or physical processes such as adsorption, volatilization, or precipitation of the paren_t material. - Inform ation Liraaiisson Initials: XMQ- 000912 -2- BIODEGRADATION OF "LIGHT WATER" PRODUCTS IN OECD TEST INTRODUCTION The 3M Environmental Laboratory chose to attempt to demonstrate the biodegradability of "LIGHT WATER" products using the OECD screening method because the test has wide international acceptance, and the Environmental Lab has had experience using the OECD test as a participant in an international ring test. These results will complement the existing BOD data that show these products to have a high degree of biodegradability. The OECD test is run at 20-25C and it measures only dissolved organic carbon. For these water-miscible "LIGHT WATER" products, which are not expected to volatilize, precipitate, or be adsorbed during testing, the OECD test is an appropriate method for measuring % total degradation. The TOC analysis method even measures the perfluorinated portion of these products. METHODS AND MATERIALS Methods and Conditions - Wade A. Scheil performed this testing following the September 19, 1979, version of the Modified OECD Screening Test with DOC Analysis(l). A copy of this method is attached (Appendix 1). Reductions in the scale of the test were necessary to adapt it to available shaking equipment. Five hundred-ml Erlenmeyer flasks replaced 2-liter flasks, 250 ml of inoculated nutrient solution replaced 900 ml, and the sample size was 25, not 30 ml. As in the prescribed procedure, the analyst used only the last 10 ml of sample filtrate for DOC analysis. A calibrated chart recorder monitored the temperature which stayed within the 20-25C range during the 28-day test, except for a 3-4 hr. period when it reached 25.5C. The temperature was most frequently near the high end of the range (23.5-24C). Chemicals - All chemicals were reagent grade unless otherwise noted^ The 3M "LIGHT WATER" products used were samples of commercial material of Antwerp manufacture. Their label identified them as FC-203 NFP, FC-3017 Lot 2303, and FC-206 (FM 3824) Lot 2330 10/79. The hydroquinone used as the calibration compound was Aldrich reagent grade hydroquinone 98.5%, Lot 100147. Four chemical supply houses were contacted in an attempt to obtain the 99.5% pure hydroquinone prescribed by the Modified OECD Screening Test, but this purity is apparenty not readiy available in the USA. We expect that this reduced purity will have no signficant effect on results. The impurities have no apparent inhibitory effect on microorganisms and their presence could make only a trivial change in TOC measurements. 000913 -3- Water used in the preparation of all solutions, except the inoculum, was St. Paul city water passed through a carbon bed, macroporous anionic resin bed, and 2 mixed bed deionizers, and then filtered through a 0.2-um filter. This water was also used to make up losses to evaporation. Stocks of water collected at the start of the experiment ensured consistent water quality. In preparing nutrient solutions, 26.4 g of anhydrous Na2HP04 replaced the prescribed 33.4 g of NH2HPO42H2O, 36.3 g of CaCl2'2H20 replaced 27.5 g CaCl2. These replacements yielded solutions and concentrations identical to those required by the OECD Method. The optional yeast extract solution was used in place of the vitamin solution (1.6.1.2(f)). The 100 mg of Fe-chelate used in the trace element solution consisted of equimolar amounts of FeCl3 and EDTA (30 mg FeCl3 and 70 mg EDTA). Test Concentrations - DOC measurements of sample stock dilutions served as the basis for adjusting initial test concentrations to approximately 40 mg of carbon per liter. This is the highest concentration in the range recommended by the OECD test. Use of this high initial concentration increased the sensitivity of % DOC removal measurements. The low toxicity of "LIGHT WATER" products to microorganisms made significant inhibition at this concentration unlikely. Adjustment of hydroquinone, the calibration compound, to 20 mg of carbon per liter was done by weight based on its known carbon concentration of 65.4%. Two blank controls, instead of 1, were utilized in making blank DOC corrections. Inoculum - The inoculum was 50-50 mixture prepared according to steps 1.6.2.1 and 1.6.2.2 o.f the OECD test using fresh soil from E. A. Reiner's garden and the supernatant of a sample from an activated sludge aeration basin at the St. Paul Metro Plant. The filter paper used was WhatmanR 54, and the water for soil extraction was chlorine-free well water. Sterile Controls - Replicate vessels containing 400 mg/1 HgCl2 served as sterile controls for each test material and the calibration ~ compound. Handling of these sterile controls was identical to the handling of the viable cultures. They had the same innoculum and sampling frequency, but the analyst only made DOC measurements on the 0- and 28-day samples. Sample Preservation - The sample preservation method used was that prescribed by the TOC manufacturer(4). The method involves adding 1 drop of concentrated HC1 to the 10 ml filtered samples, bringing the sample to <pH 2, and storing the samples under refrigeration in vials with aluminum foil-lined caps. The method is an effective preservation method. The manufacturer indicates that the method can stabilize calibration solutions made from potassium hydrogen phthalate, a readily biodegradable material, for several months. 000914 -4- Since the acidification in this preservation method was also a necessary step in the TOC analysis protocol, its use was the most practical and allowed elimination of the HgCl2 preservation technique described in the OECD method. All TOC analyses were made within a month of the preservation of the samples. Instruments and equipment - The organic carbon analyzer used was a Dohrman DC-52A. Its sensitivity limit is between 1 and 2 mg of carbon per liter. The stoppers for the reaction flasks were clean, porous, plastic foam plugs. Gelman 0.2 um membrane filters, (Part No. 64814) boiled 3 times and stored in deionized water, served to filter samples for DOC analysis. Glassware cleaning involved soaking in chromic acid cleaning solution (ChromergeR ) followed by 6 deionized water rinses. RESULTS AND DISCUSSION Table 1 summarizes the results of this study. Appendices 1 and 2 contain the actual data sheets and plots of the degradation as a function of time. All 3 "LIGHT WATER" AFFF products degraded nearly completely. TABLE 1 Percent Degradation of Hydroquinone and "LIGHT WATER" AFFF Products FC-203, FC-206, and FC-3017 With Time in Modified OECD Screening Test % Degradation at Day: Product 7 14 21 27 28 FC-203 13 85 93 91 FC-206 23 90 94 93 FC-3017 37 94 96 96 Hydro- 89 92 97 94 quinone 93 92 95 93 In the case of the highly water soluble "LIGHT WATER" products, it is very unlikely that physical means such as adsorption, volatilization, or precipitation caused the loss of soluble TOC (DOC). This is substantiated by the relatively high oxygen demand observed in BOD tests of the 3M Environmental Laboratory (FC-203 BOD5/COD = 0.5, ~ FC-206 BOD5/COD =0.5). The sterile control data in Table 2 provide further substantial evidence that the soluble TOC loss from the test samples containing "LIGHT WATER" products is not due to adsorption, volatilization, or precipitation. These samples were handled identically to the test samples except that they contained HgCl2 to prevent microbial growth. 000915 -5- At the end of the 28-day test period, they still contained nearly all the initial DOC. Thus loss of soluble TOC by these physical modes was not a major factor, at least for nonmetabolized "LIGHT WATER" components. This control doesn't prove that physical processes did not remove "LIGHT WATER" metabolites in the test runs, since no metabolism occurred in these sterile controls, but the catabolic* formation of less water soluble materials is unlikely because catabolic products are usually more polar and smaller. TABLE 2 DOC Loss from Sterile Controls Product % DOC Remaining at Day 28 FC-203 FC-206 FC-3017 Hydroquinone 91.3 94.2 88.1 77.5 An off-white precipitate formed in the hydroquinone sterile control on day 0 prior to filtering for DOC analysis. The precipitate was slightly brownish, as was the solution in the hydroquinone sterile control after 21 days. This suggests that hydroquinone is not stable, at least in the presence of HgCl2, throughout the course of the 28-day OECD experiment. This apparent tendency of hydroquinone to spontaneously form insoluble humus-like material makes it an inappropriate control compound for the OECD test. Its partial precipitation with HgCl2 also casts some doubts about the appropriateness of using the HgCl2 preservation procedure in the OECD method. CONCLUSION The present study conclusively demonstrates that "LIGHT WATER" products, FC-203, FC-206, and FC-3017, are nearly completely degraded in 21 days under the conditions of the modified OECD Screening Test, REFERENCES (1) Organization for Economic Co-operation and Development Chemicals Testing Program Expert Group on Degradation/Accumulation, Dec., 1979, Test Guideline for the Modified OECD Screening Test with DOC Analysis (Level I) (H. G. Nosier) Revision of Sept. 19, 1979. (2) Dohrman DC-52A Operating Manual, 4th Ed., 1978, p. 3-1. ~' Appendices: 1 - OECD Test Guidelines (Sept. 19, 1979) 2 - Data Sheets 3 - Graphs * Catabolism is biologically facilitated breakdown to less complex molecules. 000316 5 APPENDIX 1 Tokyo, December 1st, 197^ C 118/79/Int. OECD - Chemicals Testing Programme Expert Group C, Degradation/Accumulation Mbdified OECD Screening Test with DOC Analysis 000917 Test Guideline C 118/79/Int. Test Guideline for the Modified OECD Screening Test with DOC Analysis Date of last revision: Sept. 19,1979 Level I test for ready biodegradability 1. Prerequisites It has to be known whether the test material is soluble in the concentration range employed in the test (corresponding to 5 - 40 mg D0C/1). 2. Guidance Information Knowledge of the bacterial toxicity or inhibitory properties of the test material is not unequivocally required but constitutes useful information for the conduction of the test. 3. Qualifying Statements The method is suited for the measurement of the aerobic ultimate biodegradability of water soluble, non-volatile organic compounds. It is unsuited for the biodegradabiiity evaluation of mixtures. 000918 Sept. 19. 1979 Modified OECD Screening Test with DOC Analysis Preamble It has to be realized that the following procedure for the modified OECD Screening Test has to be regarded in some points as provisional since se veral important features such as the calibration compound and the new test duration of 28 days are completely untried yet. However, since the test constitutes a modification the official, widely practised and well accepted OECD Screening Test for the biodegradability evaluation of surfac tants there should exist a good prospect for success. 000919 September 19 1979 OECD Chemicals Testing Programme Test Guideline for the Modified OECD Screening Test with DOC Analysis 0. The test procedure constitutes a modification of the OECD Screening Test (OECD Environment Directorate, Proposed Method for the Determination of the Biode gradability of Surfactants Used in Synthetic Deter gents, Paris 1976, and council directive of Nov. 22, 1973, on the approximation of the laws of the member states relating to methods of testing the biodegrada bility of anionic surfactants (73/^05/EEC), Official Journal of the European Communities No. M 3^7/53 of Dec. 17, 1973) for the application of the dissolved organic carbon (DOC)analysis. 1. Method 1.1 Introduction: Purpose, scope, relevance, and applica- tion of test and explanation of limits. The purpose of the method is the measurement of the ultimate biodegradability of water soluble, non volatile organic compounds in an aerobic, aqueous medium at a starting test concentration corresponding to 5 - ^0 mg DOC/1 ( In order to avoid inhibitory effects it is in the investigator's own interest 2 000920 to choose as low a starting concentration as his analytical capability permits ) 1.2 Definitions and units 1.2.1 Definition of biodegradability D= t where Ct - C J x 100 - Cbl. D.W = degradation in.percent DOC-removal at time t CQ s starting DOC concentration of the culture medium (mg DOC/1) C fc = DOC concentration of the culture medium at time t (mg DOC/1) Cbi= starting DOC concentration of the 0 blank (mg DOC/1) C DOC concentration of the blank at time t (mg DOC/1) 1.2.2 Units The degradation is stated as the percentage DOC-removal within 28 days with respect to the test material ( % DOC-removal ) -3- 000921 3- 1.3 Reference compounds 1.3.1 Calibration compound The calibration compound used in this test is hydroquinone at a concentration corresponding to 20 mg DOC/1. Hydroquinone has to exhibit a DOC-removal o f ^ 6 0 % within 28 days, otherwise the test is regarded as invalid. 1 11 The principle of the method A predetermined amount of the compound is dissol ved in an inorganic medium (mineral nutrient solu tion, fortified with a trace element and essential vitamin solution), providing a concentration corres ponding to 5 - AO mg DOC/1. The solution is inocu lated with a small number of microorganisms from a mixed population and aerated at 293 ~ 298. (20 - 25C) in the dark or at least in diffuse light only. The degradation is followed by DOC analysis over a 28 day period. The procedure is checked by means of a standard (hydroquinone). A control with inoculation but without either test material or standard is run parallel for the deter mination of DOC blanks. 1.5 Quality criteria 1.5.1 Reproducibility The reproducibility of the method is appropriate for a screening test which has solely an accep tance but no rejective function. 000922 A 1*5.2 Sensitivity The sensitivity of the method is largely deter mined by the sensitivity limit of the organic carbon analysis which is 0.5 mg C/l at the present state of the art. 1.5.3 Specificity, applicability Applicable for the biodegradability evaluation of water soluble, non - volatile organic compounds. 1.5.4 Possibility of standardization The test version- with specific analyses -for anionic and nonionic surfactants is standardized as "OECD Screening Test". 1.5.5 Possibility of automation Parts of the test, e.g., the analysis,can be automated, although hardly the total procedure. The procedure is, though, well suited for being operated with whole series of test materials. 1.5.6 Costs ( in 1978 Swiss Francs ) 1.5.6.1 Equipment Glassware ,-2 0 0 0 shaking machine 6000 - 20000 Carbon analyzer 42000,- Miscellaneous (pH meter, balance provision for air dor.ditioning) 5000,- - 5- 000923 5 1.5.6.2 Person - hours 10 1.5.6.3 Approximate total cost per test 750,- - 1000,(investments assumed to be amortized) 1.6 Description of the method 1.6.1 Reagents and materials 1.6.1.1 Deionized water Deionized or distilled water free of toxic substances (copper in particular), for general use as a solvent. Water which has been deioni zed by distillation or ion exchange is suitable. A high purity of this test water is necessary in view of the DOC analyses in the concentra tion range of 0 - *0 mg/1. The contaminations result from' inherent impurities but also from the ion exchange resins and microbial devel opments (bacteria, algae under the influence of light etc). Only one water charge must be used for one test series which is to be controlled beforehand by DOC analysis. If necessary, suitable water may be gained by UV irradiation or other means. 1.6.1.2 Nutrient solution Mix 1 ml each of the following solutions (a) to (f) and make up to a volume of 1 1 with water 1.6.1.1 6 000924 6 (a) XH2P04 A.R. k 2h p o 4 A.R. Na2HP04 . 2 H20 n h 4c i A.R. A.R. 8.5 g 21.75S 33.4 g 20 0 S in 1000 ml of water 1.6.1.1 the pH value should be 7.2 (b) 22.5 g of MgSOjj . 7 H20 A.R. dissolved in 1000 ml of water (3.3.1) (c) 27.5 S of CaCl2 A.R. dissolved in 1000 ml of water (3.3.1) (d) 0.25 g of FeClj . 6H20 A.R. dissolved in 1000 ml of water (3.3.1) This solution is prepared freshly immediately before use. (e) Trace element solution MnSOjj . 4 H20 H 3B 0 3 ZnS04 . 7 H20 (NH4 )6Mo ?0 24 39.9 mg (30.23 mg MnSOj. . HjO) 57,2 mg 42.8 mg 34.7 mg (36.85 mg (NH4)6Mo ?0 24.4H20) Fe - chelate (FeClj,EDTA) water 1.6.1.1 100 mg 1000 ml Sterilisation of the trace element stock solution at 393 (X) (120C), 2 atm., 20 min. - 7 000925 7 (f ) Vitamin solution Biotin 0.2 mg Nicotinic acid 2.0 mg Thiamine 1.0 mg p-Aminobenzoic acid 1.0 mg Pantothenic acid 1.0 mg Pyridoxamine 5.0 mg Cyanocobalamine 2.0 mg Folic acid 5.0 mg water 1.6.1.1 100 ml The solution is filtered sterile (0.2 ;um). Instead of solution 1.6.1.2 (f) 15 mg of yeast extraxt may be used per 100 ml of water 1.6.1.1. 1.6.1.3 Biodegradability standard Hydroquinone 99,5 % DAB Erg. B. 6 1.6.1.A Mercuric chloride solution 1 per cent of H g C ^ in water 1.6.1.5 Shaking machine accomodating 2 ltr. Erlenmeyer flasks either with automatic tempera ture control or used in a conrtant temperature room at 293 - 298 0 0 (20 - 25C) 1.6.1.6 Marrow neck - 2 ltr. Erlenmeyer flasks. (Creased flasks are recommended) The flasks must be care fully cleaned with, e.g., alcoholic hydrochloric fluted- - 8- 00092G - 3- e use, rinsed and dried in order to avoid nation with residues from previous tests, -lasks also have to be cleaned before their .rst use since they may be contaminated, 1.6.1.7 Membrane filtration apparatus 1.6.1.8 Membrane filters 0,2 /an 1.6.1.9 Carbon analyzer 1.6.2 Inoculation Either of the following t-hree alternatives may? be used .is inoculum or a composite sample thereof. 1.6.2.1 Inoiulu^ from secondary effluent The inoculum is gained preferentially from a secondary effluent of good quality collcted from a treatment plant dealing with a predominantly dorrestic sewage. The effluent must be kept under aerobic conditions in the period between sampling and use. To prepare the inoculum the sample is filtered through a coarse filter, the first 200 ml >eing discarded. The filtrate is kept aerobic until ised. The inoculum must be used on the day of collecion. 1.6.2.2 Inoculum from soil 100 g of soil (fertile, not sterile) are suspended in 1000 ml of chlorine-free drinking water (soils with an extremely large content of clay, sand or organic carbon are unsuited). After stirring the suspension is allowed to settle for 30 minutes. - 9 000927  - 9- The supernatant is filtered through a coarse filter paper, the first 200 ml being discarded. The filtrate is aerated immediately and until use. The inoculum must be used on the day of collection. 1.6.2.3 Inoculum from a surface water An inoculum is drawn from a suitable surface water. The sample is filtered through a coarse paper, the first 2oo ml being discarded. The filtrate is kept aerobic until used. The inoculum must be used on the day of collection. 1.6.2.4 Composite inoculum Equal volumes of the 3 inoculum samples are united, mixed well, and the final inoculum drawn from this mixture. The suitability of the inoculum i3 checked by means of the standard hydroquinone. 1.6.3 Conduction of the test 1.6.3.1 Procedure The test materials are evaluated simultaneously in duplicates together with the standard (1.6.1.3) and a control test with inoculation but without either test or standard material for the determination of DOC blanks. The standard material has to attain - 60 % DOC re moval within 28 days at a starring concentration corresponding to 20 mg DOC/1. If <60 % DOC removal are achieved the whole series has to be discarded +) +) This limit is based on present experience with the 19 day version of the test. A revision of this limit or even of the standard might have to be considered after the accumulation of experien ce with the new 28 day version of the test. 10 0 0 0 9 2 8 -10 A stock solution of the te3t material in water (1.6.1.1) is prepared. So much of this stock solution is added to the nutrient solution (1.6.1.2) that a carbon concentration of 5 - ^0 mg DOC/1 is attained. The starting concentration of the standard hydroquinone is, though, 20 mg DOC/1. Two reaction vessels (1.6.1.5) are each filled with 900 ml of the nutrient solution and inocula ted with 0,5 ml/1 of the inoculum (1.6.2). The opening of the vessel is covered with, e.g., alumi num foil in such a way "that the exchange of air between the flask and the surrounding atmosphere is not unduly impeded (Cotton wool is unsuited because of the DOC analysis). The vessels are then inserted in the shaking machine. The tempe rature of 293 -298 K ( 20 -25C) must be maintained unchanged during the test, and the vessels should be shielded from light. The air should be free of pollutants and toxic materials (chlorinated sol vents etc). In the course of the biodegradation test the DOC concentrations are determined in duplicate ( 1 . 6 . 2 ) at the beginning (day 0), and on the 27. and 28. day. Three additional analyses have to be performed 11 0009.^9 f t -/U - 11 - in rather regular time intervals ( ~*7., "14., and '>'21. day) The analyses are registered in the attached form sheet and evaluated. Only the necessary volumes of culture medium may be drawn for each determination; however, they have to be large enough for the membrane filtration or centri fugation preceeding the carbon determination. The latter requires differing volumes for the different instruments. Evaporation losses of the culture medium are to be made up by adding water (1.6.1.1) in the required amounts. The culture medium is to be mixed well before withdrawing a sample. Material adhering to the wall of the vessel has to be dissolved or suspended before sampling. The membrane filtration or centrifugation has to be done immediately. The filtered or centrifuged samples,have to be analyzed on the same day, otherwise they must be preserved with 0,05 ml of the HgClg solution (1.6.1.4) for each 10ml of nutrient medium or by storing them at 2 - 4C, The biodegradability test is valid provided the standard exhibits a degradation rate within the specified range. The test can be finished before the 28. day if complete mineralization is accomplished. All steps require great care and cleanliness of the vessels, pipettes etc. but not sterility. 12 000930 12 1.6.3.2 Calculation of results The degradation at the time t is calculated from the determinations of the DOC concentra tions at the beginning (CQ ) and the time t (Ct ) according to D t x loo where D t = degradation in per cent at time t CQ = measured starting DOC concentration of the inoculated culture medium (mg DOC/1) C^ = DOC concentration of the culture medium at time t (mg DCC/1) C^i = starting DOC blank of the mineral nutrient solution with inoculation but without test material (mg DOC/1) C. , blt = DOC blank of the mineral nutrient solution with inoculation but without test material at the time t (mg DOC/1) The degradation rates are calculated to the nearest 0,1 %. The means of the D t values are calculated and reported to the nearest full per cent. Results 13 000931 ending in 0,5 are rounded up to the nearest whole number. The course of the degradation test is followed graphically in a diagram as shown in the attached example. The results are reported on the attached data sheet. The results of the degradation test are valid if the condition is met that in the same test series the standard yields ^ 60 % DOC-removal. ' 1.6.4 Analytical means 1.6.4.1 Membrane filter 0;2/m, 25 mm 0 (1.6.1.6). Pre paration of the filters: membrane filters are impregnated with surfactants for hydrophilizaticn. Thus each filter contains up to several mg of soluble carbon which would interfere in the biode gradability determinations. Therefore the filters are purified from surfactants and other soluble organic interferences by boiling them 3 times 1 hr each in deionized water. These filters may be stored in water (1.6.1.1) for at least one week. Other membrane filters are suitable if it is assured that they neither release carbon nor adsorb the compound in the filtration step. If the samples are centrifuged, this has to be done _2 at 40 000 m sec ( 4000 g) for 15 minutes, preferably in a refrigerated centrifuge, in any case < 4oC. (Remark: the differentiation T0C:D0C by centrifuga tion at very low concentrations does not seem to work well since either not all bacteria are removed or carbon as part of the bacterial plasma is redissolved. At higher test concentrations ( ^ 10 mg C/l) and the same small inoculation the centrifugation error seems to be comparatively small ). 000932 Form Sheet for the Modified OECD Screening Test -xp. no.: )ate of start of test: Test / standard material: rheoretlcal test cone.: Inoculum: 'arbon analyzer: ---------- mg DOC/1 BEST COPY AVAILABLE Controls: Stock solution of the test material { 1000 mg/1, dilution .../1000 ml of nutrient solution) TOC* 1 DOC** mg/1 B: Carbon determinations: Culture medium Flask no Analyses Mineral nutrient solution with test material and with inoculum Mineral nutrient solution without test material but with Inoculum 1 ' al a2 al + a2 B1 2 < Ct > 2 bl b2 b1 + b, 2 " 2 ( ct ) Blank C1 c2 C1 + c2 *3 2 < ch1> Theor. DCK - concentrations after x aays cone. mg/1 mg/1 0 CC0 >. -.7 . v -14 1- 2 1 1 27- 1 28 / 1 1 / /i '/ / A / / -1 C : Evaluation of raw data: DOC - concentrations minus blanks Flask no m. - m. 1 D. - -i-r;-- -- . 100 1 "l *2 " 2 Do2 - -=-=m--2 - * 100 % DOC r.emoval after x days 7 14 21 1 27 i 28 o ccso -Co---- mean DB ---1--+j--D-2 . for day x WM JW And SUV la jju u KKMfrt. 0( 40 H 1 1 > n * th 1.6.4.2 The DOC measurement The sample withdrawn from the culture medium (about 30 ml) is centrifuged or membrane filtered immediately in the filtration apparatus (1.6.1.6) using the membrane filters prepared acc. to 1.6,4.1. The first 20 ml of the filtrate are discarded'. The DOC concentration is determined twice in the remaining filtrate (about 10 ml) by means of the TOC/DOC instrument (1.6.1.8). If the filtrate cannot be analyzed on the same day it has to be conserved acc. to 1.6.3.1. The DOC measurements (mgC/1) obtained 'are registered on the'attached data sheet and the DOC concentrations of the culture medium and of the blanks calculated for each sampling time. 000934 APPENDIX 2 3M Environmental L aboratory Oata Sheet -r e s u lts o f the M odified OECD Screening T e s t- Lab Request No.; 55*1 s Date o f S ta rt of Test; 4 - W - f t o * A nalyst: Wade A. Schell Test M aterial ; W T W E R .P FC-9_o?T", M F P Standard M a te ria l; hydroqulnone, 98.5%, Lot 100147. A ldrich Theoretical DOC of Test M a te ria l; ( MOT C ^L C u l A t C D Measured TOC' of Test M a te ria l: 14-2 j OOP mg TOC/kg Inoculum: s o il and non-chlorlnated secondary e fflu e n t fran a municipal wastewater treatment p lant___________ Carbon Analyzer: Ooh'rmann DC-5A Total Organic Carbon Analyzer A. Determination of TOC^ of Test M a te ria l; A stock solution o f the te s t m aterial was prepared by d ilu tin g 1 1 7 0 mg to a f in a l volume of 5 0 0 ml with deionized water. cone, te s t matertal TOC In stock solution stock solution mg/1 mg/1 TOC test material mg/kg This re s u lt was used to c alc u la te the necessary amount o f te s t m aterial to prepare a c u ltu re medium o f 40 mg/1 DOC' 23 40 332- I4 Z , 000 BEST COPY AVAILABLE B Carbon Determinations: 2 Culture medium Flask no. Mineral nutrient solution wlth test material and w lth Inoculum 1 2 Mineral nutrient solution without test material but with Inoeu1urn Blank 1 Blank 2 . Evaluation o f Raw Data: Cone, o f te s t Calculated DOC m aterial In of test m aterial fla s k , mg/1 In fla s k , mg/1 4 0 .0 J 4* ee.a^ ct , " n 282. tj-O .O b , + b , . . . bn Ct*j " n 1 c di + C*l2 -- -- / DOC Anal yses at *a3 ac bi Jy b3 bl br Cl C- d, A - DOC - cone, af t e r X days Incubiitlo n , m<i / i 0 (c0) 7 14 21 27 28 3 7 .0 a . / ~ p rr 3 .Z 6 .0 6 .2 4 --8 7 -S' 4-,2. ^ I h i -s V .o 3,V.e Vt J 37. 31. 32.1 > .l fe>T ..s . r ..... 5^ 2 .8 ' ..O / */ 4*1 3. Z r-o 6 .2 . 7 2,-S 2 .8 .? Z -6 4 l-b , I1'-L9 yr /S ' / Q> bX lCblO) 1*4 52..0 0 ./ - .Z -o / 0 ./ 0 1.^ - o . | (o> 0 0-X o-r 0 .4 0 `i 0.6 o-H 2 >4 / r 09 A2 / /. 0 A3 l'Z 2 -8 0-9 0 . o .l 0.1 0 .S " . rt.ft ?./ -o .1 - 0.1 X 6 -0 ./ 0.6 0 Flask no. 1 2 mean Degrada :lon - % )0C remov>1 a ft e r >c da^s Incubation 14 21 27 .S ' 11.8 13.0 2o. \ l7.o 41. 13 ^3 ^1 n See attached section 1 .6 .3 .2 fo r the*12 formula used to c alc u late degradation. Results o f blank n o .l and no. 2 were averaged fo r each day x . The average values were used In the c alc u latio n s . cb1j + ^bl2 (from above) Cbiave -- l---- 1. The te s t m aterial ts completely soluble In w ater. Therefore, the TOC DOC. 2 . DOC analyses performed more than twice on the same sample were run fo r q u a lity assurance p u rp o s e ^ q q 0 3 5 3M Environmental L aboratory Oata Sheet re s u lts o f the M o d ified OECD Screening T e s t- BEST COPY AVAILABLE Lab Request N o .; 55^*1 S Oate o f S ta rt o f Test: 4- - 11- Sd_________ A nalyst: Wade A. Schell Test M a te ria l; amtuJCRP. r r - . r * - i s ? s L o r z ssq, to/rt Standard M a te ria l; hydroqulnone. 98.SK. Lot 1001k7, A ldrich Theoretical DOC o f Test M a te ria l: f NOT cfi-t~Cnuk-re.b) Measured TOC* of Test M a te ria l: 9 3 ,9 0 0 mg TOC/kg Inoculum: s o il and non-chiorInated secondary e fflu e n t frowa municipal wastewater treatment plant Carbon Analyzer: Doh'rmann OC-j>lA Total Organic Carbon Analyzer A. Determination of TOC* of Test M aterial; A stock solution of the te s t m aterial was prepared by d ilu tin g /jO&O mg to a f in a l volume o f 5~Q0 ml w ith deionized water cone, te s t m aterial TOC In stock solution stock solution mg/1 mg/1 TX test material mg/kg This re s u lt was used to c alcu late the necessary amount of te s t m aterial to prepare a c u ltu re medium of kO mg/1 OOC** Z,!ZO B. Carbon Determinations; 2 Culture medium Flask no. Mineral nu trien t solution wlth test material and wlth Inoculum 1 2 Mineral n u trien t solution without test material but with Inoculum Blank 1 Blank 2 Evaluation of Raw Data: Cone, of te s t m aterial In fla s k , mg/ 1 ................-- I-- Calculated D X 1 of test m aterial In fla s k , mg/1 4ZG io .o aj + a j . . .an t t]" n 4 o ,o b, + b2 . . . bn Vn OX Anal yses ai aa3t .. 5 D X - conce af t e r x days Incubiitlo n , me/ I 0 (c0) 7 Ik 21 27 28 V 2 .3 J/,0 VI-7 a r .3 . / 3 -6 3. S' 3 .V 3.V 3 .O V.s3 /0 4 o , o 3 1,0 r - 7 Z-(o 3 .V 3 -^ bi ' t h . 3 b? v / . s b3 bi 5 V /.S 30.7 30.1 So.% 'i-T S-3 3 -* 3-0 _ / 2.(2 Vz/ 3 . 2. 3 .6 3 .i 3*6 3J c i I. / . e - .... 0<( '.y 0 .1 0 S' / -S~ 0 .7 O '? 0./ 0 .1 . / TW /S" -&-Z 0,9 A 2. O./ ! d, / i> - O . f 0 - 1 /& 0,7 - o . f d? A 2. 0 . t 0 , 6 , !>0 0 .8 -- -0 , ! ccb, 2- _V _ "212 l.f- O -H /3 l -O . 1 /w -o .l O-H A 2 >.6. & Flask no. 1 2 mean Degrada : Ion - % I X removii l a ft e r c da^s Incubation Ik 21 27 2 3 .3 f a . ? 9 /i/ 93J 7 /.V 9 V . / ?2.3 3 7o n }l 72. See attached section 1 .6 .3 .2 fo r the formula used to c alc u la te degradation. Results o f blank n o .1 and no. 2 were averaged fo r each day x . The average values were used In the calcu latio n s. r Cb1 j + Cb12 (from above) Cb1ave -------5---------- 1. The te s t m aterial Is completely soluble In w ater. Therefore, the TOC DOC, 2 . DOC analyses performed more than twice on the same sample were run fo r q u a lity assurance purposes. A V A IL A B L E3M Environm ental Laboratory Data Sheet D EC T f ' n O V A \ / A i i a m ir- ilts o f the M odified OECD Screening T e s t- DCO I l ; U r i Lab Request N o .: 5541 S Date o f S ta rt o f T es t; 4 - - l l - f t o A nalyst; Wade A. Schell Test M a te ria l: A^TVitltP. Standard M a te ria l; hydroqulnone. 98,5%. Lot 100147. Aldrich Theoretical DOC o f Test M a te ria l; /AJOT g A ic u L A T S fiJ Measured TOC' of Test M a te ria l; 197.0OO mg TOC/kg Inoculum; s o li and non-chlorlnated secondary e fflu e n t fro sa municipal wastewater treatment plant Carbon Analyzer; Dohrmann 0C-52A Total Organic Carbon Analyzer A. Determination of TOC^ o f Test M a te ria l; A stock solutio n of the te s t m aterial was prepared by d ilu tin g ,2 * 4 ^ mg to a fin a l volume of &__jn1. with deionized w ater. cone, te s t m aterial TOC In stock solution stock solution mg/l mg/l TOC test material mg/kg This re s u lt was used to c alcu late the necessary amount of te s t m aterial to prepare a culture medium o f 40 mg/1 DOC** 1 ,4 4 0 411 l^ZjO O O B Carbon Determ inations; C ulture medium Flask no. Mineral n u trien t solution wlth test material and wl t h Inoculum i 2 Mineral n u trien t solution without test material but with Inoculum Blank 1 Blank 2 Evaluation of Raw Data: Cone, o f te s t C alculated DOC m aterial tn o f te s t m aterial fla s k , mg/1 In fla s k , mg/1 Zo% fo .o d| ^ tj" &2 * * *an n 2oZ o b , + b , . . . bn c tj n c ! + c2 Cb l f n 1 "7 DOC Anal yses at a, a3 A .... aF DOC - cone, o (c0) 7 5 /.Z V o -* 3o.3 af t e r x days Incubiitlo n , me/ I 14 21 27 28 a .y a-r 3 .1 X- M Z*5" / o f l - l $ o >2 2 . 4 3.o 2 S J'S i>i u s . - i >2..... -3. S'. W .4 3 , if 3 /9 /.? / 7 X . ) 2 . 2. 2.<-i b3 bl 3 y . v 11, Z 3.6 2 .0 I . C l..... / ( o . ; o , a i . r 0 , 1 0 . 1 .C- -o.w o. r 0.9 0. t o , ( lCb l0) lS " d. ).d - 0 . 1 do X C>. I 0 .4 o .i o , c> /.X I. 6 1.0 o.r o .% O, fl 0,1 - 1 -a ,, cb l2 - _ _ _ 0 0>4 /. 3. 0 1(o - 0 - 1.1 - 0 ,1 o . H | h x 0 . 6 o Flask no. i 2 mean Degradaitlon - % )0C removi>1 a fte r ; da^s Incubation 7 14 21 27 33 . X !, 0 IS S 6 .2 . iZx\ 37 1 4 U % -r 94 lC Sea attached section 1 .6 .3 .2 fo r the formula used to c alc u late degradation. Results o f blank n o .l and no. 2 were averaged for each day x . The average values were used In the calculations. - Cb1| + Cbl2 (from above) Cb!ave ------ 5---------- 1. The te s t m a te ria l Is completely soluble In w a te r. Therefore, the TOC DOC. 2 . DOC analyses performed more than twice on the same sample were run fo r q u a lity assurance purposes. 000937 3M Environm ental Laboratory Data Sheet -r e s u lts o f the Hod I fle d OECO Screening T e s t- BEST COPY AVAILABLE Lab Request N o .: 55^1 S Oate o f S ta rt of Test: 4 -- II --<S*> A nalyst; Wade A. Schell_______________ Test M aterial; Standard H a ta r la l; hydroqulnone. 98.5%. Lot 1001^7. A ldrich Theoretical DOC o f Test H a ta r la l; 6S.4-a> C CA uTC A R&OM A SSur^ B s> t o B e o lu jJl E o Pc-a N 'C CA Rta>j\ Measured TOC* of Test H a ta r la l; mg TOC/kq Inoculum; s o il and non-chlorlnated secondary e fflu e n t frowa municipal wastewater treatment plant Carbon Analyzer; Pohrmann DC-52A T o ta l Organic Carbon Analyzer A. Determination of TOC^ o f Test M a te ria l; A stock solution of the te s t m aterial was prepared by d ilu tin g with deIonized w ater. mg to a f in a l volume o f ml cone, te s t m aterial TOC In stock solution stock solution mg/1 mg/1 TOC test material mg/kg This re s u lt was used to c alc u la te the necessary amount o f te s t m aterial to prepare a c ultu re medium o f b0 mg/1 DOC' 2 B. Carbon Determinations; Culture medium Flask no* Mineral n u trien t solution wlth test material and wlth Inoculum 1 2 Mineral n u trien t solution wlthout test material but wlth Inoculum Blank 1 Blank 2 . Evaluation of Raw Data: eVALUArtotJ t>F cALt8**TtcJ COMPOUND- STAKIDARD M A T e ttrA t- A s o v e . Cone, of te s t m aterial In f la s k , mg/1 1 C alcu lated DOC of test material In f la s k , mg/1 3 0 .6 ZO.O a j Hh 62 e 3^ ct j" n 30. G ZO.o b , + b, . . . bn Vn ,, _ C 1 + C2 b'l n 1 Ccb,2w _d 1_+ _^*12 DOC Anal yses ai a, *3 aF ... b> _b _ b3 bi b5r CT c. d] DOC - cone, aft e r x days Incubiitlo n , me1/1 o (c0) 7 \k 21 27 28 i l \ ! 2-3 2 .0 Z .V A3 A7 / .3 1.7 A Z ^ 3 3-3 /.<? A O AG>.% ia.> /7 '3 /7. /e .z 2 .0 2- o -r d / . A S' *4A6 2 .7 s' AX ) . <p Asr /A hi o -e o .e 17.0 hi A 3- 0-) -o -v A8 O' 2or 0.B hr 0.4 AS" h ,/'X (CblO) /*/ -o. z -O .l 0 os O.J _ .<+ t-2 it fe /.o o.<+ .Z hi 0 .9 a,../ 5*8 d .y 0. ) OS o .v O . - o .l -o ./ -O.) .H - 0 . , C. Ubll.ve c. ^-- + `--" b'l. _ / y - o .) / . % O.(o 0 Flask no. 1 2 mean Degrada tlon - % 1>0C removeil a ft e r 1 da^s Incubation % (*.% 42S 21 4 o .i> 27 n .7 f/.2 - 11.7 i l . o /02X 441 W J 4 l 41 44 13 See attached section 1 .6 .3 .2 fo r the formula used to c alcu late degradation. Results o f blank n o .l and no. 2-were averaged fo r each day x . The average values were used In the calculations _ Cb1j + Cbl2 (from above) C*ave -------J---------- 1. The te s t m aterial Is completely soluble In w a te r. Th erefore, the TOC DOC. 2 . DOC analyses performed more than twice on the same sample were run fo r q u a lity assurance purpQ Q Q < ^ g I 100% 90% - --------------- --------------------- f -. -.---------------- 1-1-------------------- rr 8o%: 70%: Uce1 T T i T T T i a I 5c%: i iri i 7 4o%: Ua<taisc-_- 3o% = 20%F i l J)T i .. CO CO 3H Environmental Laboratory 0EC0 Modified Screening Test w ith DOC A n alysis A n a ly s t: Wade A. Scheil Date o f S ta rt of Test: 4-11-1980 Lab Request No.: 5541 S Test M a te ria l: AM Tw RP^ fC-su>3 8 F P 1 _[ _^ J 1 -- Jj ! .1 J. I I T 1I | }I h a -------:--------- 2f NUM9ER OF DAYS INCUBATED vnt APPENDIX 3 000940 3M Envlronrental Laboratory OECD Modified Screening Test w ith DOC A nalysis A n alyst: Wade A. Schell Date of S ta rt o f T es t: 4-11-1980 Lab Request N o.: 5541 S Test M aterial; A N TW E R P ; F C -^ O tT j LO T-2 3 o? ~"|------------------ NUM5ER OF DAYS INCUBATED i --t- '1i i 4 i 000941 000942 3M Envlronnental Laboratory OECD Modified Screening Test w ith DOC Analysis A n aly st; Wade A. Schell Date of S tart of Test; *-11-1980 Lab Request No.; 55**1 S Test Material; HYPROQUllfolJe "j 1 L 4 t svv t r September 19., 1979 > OECO Chemicals Testing Programme Test Quideline for the Modified OECD Screening Test with DOC Analysis I1 0. The test procedure constitutes a modification of the OECD Screening Test (OECD Environment Directorate, Proposed Method for the Determination of the Biode gradability of Surfactants Used in Synthetic.Deter gents, Paris 1976, and council directive of Nov. 22, 1973, on the approximation of the laws of the member states relating to methods of testing the biodegrada bility of anionic surfactants (73M05/EEC), Official Journal of the European Communities No. *i 3*17/53 of Dec. 17, 1973) for the application of the dissolved organic carbon (DOC )analysis. 1. Method 1.1 Introduction; Purpose, scope, relevance, and applica tion of test and explanation of limits. The purpose of the method is the measurement of the ultimate biodegradability of water soluble, non volatile organic compounds in an aerobic, aqueous medium at a starting test concentration corresponding to 5 - *<0 mg DOC/1 ( In order to avoid inhibitory effects it is in the investigator's own interest *i - 2 -I I 0009 3m Environmental Laboratory Oata Sheet - r e s u lt s of tha Modi fia d OCCO Scraanlng T e s t- BEST COPY AVAILABLE Lab Raque*t N o.; 55AI S Data of S ta rt of T a t; 4 - \ \ -ft'o * A n a ly s t: Wade .................. Tast M atarla MFP Standard M a te ria l; hydroqulnona. 96.S 1. Lot T h e o re tic a l DiOC o f f a s t H a ta ria I ; f tM 6-r c a l c i a l a t C d 3 Measured TOC^ of Tost rHwawtai r*lma l ^ T C x i / k g Inoculum: so li anid n o n -c h i o r in a ta d secondary a f f lu a n t fre n a m unicipal wastewater tra a ta a n t p la n t Carbon A nalyzer: 0ohrmenn 0C-52A T o ta l O rg a n ic C a rb o n /A nalyzer 1001^7. A ld ric h A. Oaterm I natio n of TOC* o f Tast H a ta r la l: A stock s o lu tio n o f tha ta s t m a te ria l was prepared by d ilu t in g 1 1 7 0 mg to a f i n a l volume o f 5 0 0 ml with deionized water cone, te s t m a te ria l In stock solution mg/1 TOC stock solution mg/1 TOC test m aterial 9/kg This r e s u lt was used to c a lc u la te tha necessary amount o f ta s t m a te ria l to prepare a c u ltu re medium o f bO mg/1 OOC' 340 33^ IH-Xjooo B 2 Carbon D eterm in atio n s: C ultu re medium Flask no. Mineral n utrien t solution wlth i test m aterial and w lth i Inoculum 1 2 Mineral nutrient! solution without te s t m aterial but with Inoculum Blank 1 Blank 2 . E valuation of Raw Data: Cone, o f te s t m aterial In f la s k , mg/1 -------------------------- 1-- C a lc u la te d DOC of test m aterial In f la s k , mg/1 DOC A n a l yses OOC - cone, af t e r x days Incubiit 1on, mel / l o (c0) 7 1U 21 27 28 81 4 0 .0 i at _ J 2 __ 4 0 - 6 _J3__ _______ *5 3 7 .0 T p rr S ea 1 .fi fi.O 7 S' 4 -4 4 -/ V ./ H2.Z-1 l ct i " 2 "n n H I - 5 3 7 .4 1 . 4 5 -4 4 1 2. 32. ! fo.o "T-- y /.y ...2 - a 3 2 1 . . s r ..... 2 . 0 3.Z H .TO E T y. 2. b. + b, . . . b ct 2" n 3 V/<b 2> 7 .0 <o.O 24 {.Z 1 , _ c l + C2 Cb l , n i ci M 0>l > 4 . - .<* o-z o.ir /sr _ d , _ _ <6 : 4 /X '.Z -O.f 0 ./_ 04 0.1 0 .6 /r M " T o r o. 1 _j 2j h i 0. h i "57*5 - 0 / o -c C - V d* C2 -- H-- /Y uve. * \ 4 0 >4 A 3 -o.| 1 o 4 1 l`Z . (s ' , 04 t Flask no. i 2 mean Degrada tlon - % )0C removi l a f t e r c da^s Incubation \k 21 27 . >.Z S 3 1 3 .0 2o. \ %c>.\ V . o 4 /.0 4 3 .0 13 <?3 3 Sea attachad sectton 1 .6 .3 .2 fo r the form ula usad to c a lc le te degredatlo n . R esulta o f blank no.1 and noT 2'were everaged fo r each day x . The average vales were usad In tha c a lc u la tlo n s . r Cb l | + ^ b l2 (from above) "'ave -- J---- 1. The te s t m a te ria l Is com pletely so lu b le In w a te r. T h e re fo re , the TOC OOC. .2 DOC analyses performed more than tw ice on the same sample were run fo r q u a lity assurance purposes. 000944 3M Environmental Laboratory OECD Modified Screening Test with DOC Analysis A n aly st: Wade A. Scheil Date of Start of Test: 4-11-1980 Lab Request No.: 5541 S 000945 3M Environmental Laboratory Data Stoat re s u lt o f the M odified OCCO Screening T e s t- BEST COPY AVAILABLE Lab Request Wo.; 55A| S Oats of Start of Test; 4-11-^ Analyst; Wade A. Schell_________ _ Test Material:AisiTVjCItP. t U - j ^ T Y o T - V S o ^ Standard Material; hydrogulnone, 9*. Lot >001b7. Aldrich Theoretical DOC of Test Material; CNQT CAu<LuuAT6fi!> Measured TOC' of Test Material; 1XtC O O *8 TOC/kq Inoculum; soil and pon-chlorlnatad secondary affluent froaa municipal wastewater treatment plant--------- Carbon Anolvxer; Oohrmann 0C-52A Total Organic Carbon Analyzer A. Determination of TOC* of Teat Material; A stock solution of tha teat material was prepared by diluting 1,2-4 S' mo to a final volume of with deionised water ail cone, test material TOC TOC In stock solution Stock solution test material mg/1 mg/1 g/kg This result was used to calculate tha necessary amount of test matsrlal to prepare a culture medium of bO mg/1 DOC' 1,440 *71 rfZjO I 2 Carbon Determinations; Culture medium Flask no. Mineral nutrient solution wlth test material and wlth Inoculum 1 2 Mineral nutrient solution wlthout test material but with Inoculum Blank 1 Blank 2 Evaluation of Raw Data: Cone, of test Calculated DOC1 material In of test material flask, mg/1 in flask, mg/1 Zo% Ho, o al + a2 n Lt|" n 20% J.0.0 b, + b2 ... bn *'t2" n DOC DOC - cone, aftar x days Incubiitlon, m;|/1 Anal o (c0) 7 lb 21 27 28 yses at s......w r f r - v aL 3/.2 20- .r_ 3? X-% h! i.z. Z>S- 2,o /*. f. /,/ 30.$ 2 . 4 2S Z'O /f b2 bj bl _ b5 3 4/.X 35" 3-9 j.i 1.7 A, / 2.Z A V M l,(* 2 . ? 2 . 0 Cl /<{ 0> 2 t.f 0,1 0,1 V `O.w o. r 0, 1 o.i ----------- 1 I.S- - Q , Z />2 , r 0,1 d,__ 1,6 - o.i o. ) f . i O.V . -, I -- d9 'a. o, 1 o,0> /.o o , k - - 0 ` b!2 h 2 al qye 1-4 0-4 ),4 -o,i O . H 1. S />2 0, (o 0.6 -0 . Flask no. i 2 mean Deg7radaLion1b- % )0C removiil 21 after 27 ! daj| Incubation 33. X iff I f 2 7C,. 2. 52,1- 92i I 1S.2 % .s* 14. i 3 7 15 U 1<o See attached section 1.6.3.2 for the formula used to calculate degradation. Results of blank no.I and no. 2~were averaged for each day x. The average values were used in the calculations, pCb,#v. *-"-bl-jj-+-^-b-1-2 (from above) 1. The test material Is completely soluble In water. Therefore, the TOC - DOC. 2. DOC analyses performed more than twice on the same sample were run for quality assurance purposes. 000946 000947 3m Environmental Laboratory Data Shaot r a t u lt o f tha M o d ifia i OECD Scraanlng T a a t- BEST COPY AVAILABLE Lab Request Ho.: SS^I S Data of Start of Taat; 4 - - l l - & d Analyst ; Wads A. Scholl_____________ Test M a ta rla l: AMTyJLRP. L o r z ilo , /q/ tt standard H a ta r la l: hydrogulnono. 9 6,5 1. Lot 100147. A ldrich Tbaoratlcal DOC of Teat Hatar 1ilV v q T <Lftt-C-Ui,X-r 0) Maaturad TOC' of Taat H a ta rla l; a.PO mg TOC/ka Inoculum: t o ll and oon-chlorjnatad aacondary a fflu a n t fros> municipal wastewater treatment p lant___________ Carbon Analvzar; Dohrmenn OC-52A Total Organic Carbon Analyser A. DatarmlnatIon of TOC* of Taat H a ta rla l; A stock solution of tha ta s t a a ta rla l was praparad by d ilu tin g fjQ & O mo to a f in a l volume of S"0O wl with da Ion I sad watar. ' cone, test material TOC In stock solution stock solution mg/l mg/l TOC test matarlal g/kg This ra a u lt was uaad to c alc u lata tha nacassary amount o f tast m atarlal to proparo a c ultu ra madlum o f bO mg/1 DOC'* Z,tZ0 /? ? a 2Carbon Oatarmlnatloni; Culture medium Flask no. Mineral nutrient solution wlth test material and wlth Inoculum 1 2 Mineral nutrient solution wlthout test material but with Inoculum Blank 1 Blank 2 Evaluation of Raw Data: Cone, of te s t Calculated OOC* material tn o f te s t m aterial fla s k , mg/l In fla s k , mg/l q tc . Vo . o l + 2 **n Ct , " n ^zc> V0 ,0 b, + b, . . . bn Ct 2" n r C1 + C2 Cb l T n 1---------------------- ----------- -----cb, - d>+ b,2 n C DOC Ana1> ysas ai ,? , 1 fi b; b2 bbii - b5r DOC - cone, af t a r X days Incubiit Ion, m<l / l o (c^ 7 1b 21 27 28 3 /,o W l7 3/. o 6< / 'S -Q> 3 ,S' 3 'H 3.V 3 .0 4l;oS' 42.0 3)>o 42.3 " F T V /,3 30-7 r.7 .r 3 /3 3 ' to 3.V 3 /0 .f t V // 3 'Z 3 .5 " 2- 3- to 3 0 ,% 3.*/ 3 .t 3 ` t J./ ci C, 1. 1 0< f O' 2. -O 'V O S ' /S " O ./ 0, / O ./ >.rl .s ~ / 2, o . . fe<J. / . -0 .1 d] r f t r O'/ 06.. /* t>to /o >. V .. --o0., (Cb10^ / 0 .y /'3 0,6 --o. -O '! A2 01 o Flask no. i 2 mean % Degrade tlon - )0C remov 1 a fte r i da^s Incubation 1b 21 27 23.3 U ' 93, / 23, r \X<(o IV ./ h .i <23 1 o ) 3 1 2 - Sea attached tactio n 1 .6 .3 .2 fo r tha formula used to calcu lata degradation. Results of blank no.1 and no.~2 ware averaged fo r each day x . Tha average values were used In the calcu latio n s. r ^ b lj * ^ b lj (from above) CHav. -- 5---- 1. The test material Is completely soluble In w ater. Therefore, the TOC > DOC. 2 . DOC analyses performed more than twice on the same sample were run fo r q u a lity assurance purposes. 000948 000949 3M Environmental Laboratory Data Sheet BEST COPY AVAILABLE -re s u lts o f the M odified OCCO Screening T e s t- Lab Request No.; 5541 Date of S ta rt of te s t: 4 - l l - K O Analyst ; Wade A. Schell Test M aterial; Standard M aterial: hydroqulnone. 9 6 . . Lot 1001b7. Aldrich Theoretical DOC o f Test Materla i: Measured TOrCI1 of Test M a te ria l; t A u . CAR&3M wtagi TiwO.C>/kg ur*Bi> TO 8 6 JOLuftLC ORftAA/UL C A R & o N j Inoculum: sol 1 and oon-chlorlnatad secondary e fflu e n t rosa m m lslm L mss tawater treatment aient Carbon Analyzer; Dohnaann DC-52A Total Organic Carbon A< nalyzer A. Determination of TOC* of Test M a te ria l: A stock solution of the test Material was prepared by diluting with deionized water mg to a fin a l veluna of 1 cone, te s t m aterial TOC In stock solution stock solution mg/1 mg/1 TOC test material *g/kg This result was used to calculate the necessary amount of test m aterial to prepare a culture medium of bo mg/1 DOC' 2 I . Carbon Determinations: 1 /A C H A T E t>F eA u & A A rto t) c o m p o u n d - see standard MATAtAt- ABO VC Culture medium Flask no* Mineral nutrient solution wlth test material and wlth Inoculum 1 2 Mineral nutrient solution wlthout test material but wlth Inoculum Blank 1 Blank 2 Evaluation of Raw Data: Cone, of test Calculated DOC1 material In of test material f la s k , mg/1 In f l a s k , mg/1 30.6 zo.o l + a2 ,an ct)" n 30. G ZO.O b 1 + b,* e b Lt2 n , _ C 1 + C2 Cb l , n 1 DOC Anal ysas 1 a, a .... c DOC - cone, aft a r x days Incubiitlon, mil/l 0 (Co) 7 1b 21 27 28 17,1 2-3 / .3 1.7 2 .0 1.7. 2 .4 / 3 A 7 /<7 h o J8.4- Z. 3 <7- /0. / 7* 3 bi /7. b7 /C.2 b3 bl b5 n .o Cl h i e,, M . ^Cb l 0 / ` S' d. ! t do .... 2.0 o -r 06 A 2- o>) -0 .V -O 'l - o.l .) /*b r/ hi A8 o<x. Q .r 0 .4 o, 4 . 2 ,7 OS" J-2. o.& h s* o.q /2 I.i J. 0 / /S" IV 1 .4 AV 0 ,9 d). ) 5 .8 0 ./ o- / OS o.v - O ./ O. ' - o .t cb.'2, - d , *n d2 - e* + -- bj;-- 1.4 0 _ 1-9 -o.i 0 .9 .y J.J O.b - 0 . /.% 0. b 0 Flask no. 1 2 mean Degrada tlon - % >0C removiil a fte r 1 da^s Incubation lb 21 27 7/,7 ^ 2 .r ?3.7 7/-0 / U 2 . 6 7 2. 77 ?/i2- w .i 13 See attached section 1 .6.3.2 fo r the*12 formula used to calculate degradation. Results of blank no.1 and no. 2 were averaged for each day x . The average values were used In the calculations **bl | + ^bl2 (from above) cb i , v, " ------ j ---------- 1. The te s t m aterial ts completely soluble In w ater. Therefore, the TOC DOC. 2 . DOC analyses performed more than twice on the same sample were run for q u ality assurance purposes. 000950 3M Envi ronrrental Laboratory OECD Modified Screening Test with 00C Analysis Analyst: Wade A. Scheil Date of Start of Test: **-11-1980 Lab Request No.: >5**1 S 1 I \ 000951 FORM10420-lfWO SAMPLE DESCRIPTION BEST COPY AVAILABLE L .& S S H I -S' File: Page No. / ENVIRONMENTAL ENGR. LAB - WORK SHEET Date: Analyst: .S f Hrs.: ___________________________ 71<SG^ - ECK & /^ O T s li^ iS a C )_____ ^ i Tv\, ^A^pAA^kJZctTY^ `--------------- j i , a) _^ y iL ^ K ru ^ . aJa^ M F y uszi^ ,__F W -J b I k . j b - 3>,o 7 ___ - ~ 7 % ~ ~ ^*77& Vu-cXt/try^ iZi2)-- (7 I ^*ZFxO lls-Olos jju^ kL .--- 71-n/LAZ^C-n'-Nh S M s ' ~ A32r -/-^) L^JLO^j js*4/ss<>*<sL AjUTOA' ajlAlaJ AsyvFXg^C /uJm a!^ -^ / * 6 / 2 ( ? f a C t "2. y tt ^ l. -.. ^ f / v g U T'ixi h ^ ^ r..,---------------------------------------:-- J L __- - f.- ..- ^..r -..T.T--...--...- ....w......... -- ~ II f -- n r - f ^ - t V ^ n v ' y Qsr~t flm -yvSxC^T-X/tf't&FltSs,,\J ^ kL_.*L*>y ..**?. s i + ^. ^SLASCZJ^ d j__J)~r^c7ZsO<;tct0'S . /'L*?, y ^ A o ^ L -,- ~JjX < n u fip v 1,0 b a? (JL #Vv J J & ^i /`' 'pury^esi. * ^ s -**pp t. ____ ydAA frrryA- f jfr: >(6A<&MZL.l **___ ? c rzs \t h J L J t. `i /f J ^ . .2A )/ t, ! n\ -- -- 2.__ a ^ ^ r r v ^ u Y ^ JL aj^ { 2 ) ___________ i^ h n ^ A^T- v 5 r ^ V J76l -- -A , ---------------------------- --- -- -- -- /\i- jr^a- ^ <acY c L l~ r-~ i * ' ot >4 * /fyy\Ajt>ir<iAsfcL 1/v^TM A ^/rF ) , j t (o Z z ST^ ~~~ / Cp 7.* ) i^ ^ c P rli_?j2 j^T~^ ^ F t c s u ^ ' ~ & <y<f j1jL A '1 oe t~ u < r jg s y ^ d a ^ - O y ----ill'3 ^ siVAts &*.9jJ s b L .&i& \? l \~(<2-L (/(/ Revieved by: 000952 P O ftM I0 2 0 I-P W O L U * STS'Y/ _ x BEST COPY AVAILABLE File: Page No. r S ENVIRONMENTAL ENGR. LAB - WORK SHEET SAMPLE DESCRIPTION fltr tu ^ - [\ld )> D & C < L:VULiH Date:____________________ Analyst: . f\r_ Hrs.: ____________________ Ai.__ j^_MAr.-'S. (.H r i i ' %_ tW : 7,. 7 f V - ! ? - & > ,) A/ -----kxkk,--------.-.-.-.-.-.-.-.-.-.-.-.-.-.-.-.-o m J 2 ..__________________________________ #. _r_>i/_\! --* j| -- </^> /^ VT - 2^/ - fs=*r-:o..)/ y Lr'vuv.s "U. &lYXjjJ\-AJ, AW y~>^ ~f a S L # A J rfa J fA >r?v. __ 4 _. an dL*______________________________________________ ^VI /Xa^- K (V-2. 5~% J ^__.ia-/y.y./.v .% ^ .:>v> .( a $- --- * c ^ n ^ jL .i -/-___ ~ 2.1_____________ r Q2- r -Qi__ ^ J . '' >0^ t u t A f^ ^ rr- ^tDs^. JZ sL x L ^ fjA ^ tu n ^ ^ m A fti L __ / ./CJtb1JL A r 'm "1kcr'>^ ^-vv A M ^ A A - 4 - 3 y ''U $ 1s.>y j x *# u__il d jrfL *.. Lt& z \ A M 4 J .J i ,% $JL aS uA J JU. A _ -Jx.^u, /r ^ tonrrnJn) j t l-LL __b A ^ T r^A jo J O n C /\- ^ (U XflCu . / - / ^ S 'Z j^ T r b ^ u^ r ^ U > > f jU & j & t VT J ^ kA i L s J j^ _t/^hr j^ ra ^ v u ^ ^ ,____ V j l ^ " * '-- - ' Reviewed by: 000953 FORM tO20-i-FW O SAMPLE DESCRIPTION BB Et SlT UCOU Pr YY AAVVAAIILL AA BB LL EE File: J t o f r No. IS ENVIRONMENTAL ENGR. LAB - WORK SHEET v. ' "aJr 3 ^ 5 Date: S - Z 3 - 1 Analyst: J. 9 Sc Hrs.: _________________ )1tu on y y tfi- o c < o JO r b I f u r i L < r > s ~ j ; r v - ^ ' - )S) j*x u H ~vso^m XttiJIT C y ^ t r ^ Le. c riF triu ^ -a ^ . &Gy*svY^4ry^s .wA S '- `-'o <& <W$7` il \j^ ju , \A*JL$ AAjn&Si- ( l im ) , in a ^c v *J _____ *dt Kl^ ^\L/fjA^ Ac k5f. AA *e>fi/. -^AS#OPt\- i ATTii>i>a>^J Jr-'SV\A*:~^y3ur\ ^AJf7ctJ^JTFVV^I ' 77m . _Ajc 7t>U*-e^tl. ______iAAS7Q&- /r> CjaA ZuJ ^ L . iAJ-OXt /<' "TL, sL^ 'Cj^(r&<r<s>i Y'/otsyj yv^JA'W >u j U ) ^ryn t u A^._- ~f^< 4-W j^Z --------------------------------------------- Ixsec-Csy^L. r>i 3 ^ * * 4 A j*<uluU * ( 44- g ~fvv._ y -J J jz& Hi_PoA+p"^^^<S'" "-Trf_\4~J'CSO */ ^ ^ / jo^j-', 1 Z F jz c/ut Lostj _ -- 3 V>Kj F* C l $ amr^cP 7 Q l- DT A U-<J-d. h . a ik cj lltj&Arlj-JSJl a*S3j&~ AjH & L . //CbT-.V---'1g^/V^J~^ /(>C*-^Arf->H".*t*t.-- <'3. fi^ ^ X tn >vj o tyvH f1 iAst^LB^di L?t AAsj- ((b) 'i^yy^u^F -- iZ-- H *,t.',---- /*2. jFforr'O'J-M/rrv -- "XjL AJ-<^rr-4>LA/^M A-12^-^Lrtt_'Qr'HOQ- A S .J lf -*L SI QJ5~t O uL^'aJFc^\ tx x ^ ^ fc y -d {H&A l'Sln^ej ~f*Pp A_stjr<^L* _QotdH._ ~ A t * y ^ -4nJ> ' 4- fd n n M '______________________ ;___ J - ttu iy r^ .v\/ A > A..^7*Jt"o 0^F ~&"~ry~"j>>4 cfj / c^ J/M/-iru ^'KjJU/uryy^ > ,/ ^ W 4 ^ A ^ U k ^u ~/^yf. Aya,, /< <*d^LL4*-d. sty- C ^ r^ rA y ^ ray-X^.^ r^rro Reviewed by: -- 000954 BEST COPY AVAILABLE L-ll File: d^ctge"No. ENVIRONMENTAL ENGR. LAB - WORK SHEET <rr^/ s H r j S' f SAMPLE DESCRIPTION /'m- Date: Analyst: U J 4 S Hrs.: _______________ ____ .. /- , . " L ivJL-zLc4A^UvA# L ' 0- S d 'is J ? {j ^ A a jls y a A s & /` iv . , jj j E>t /> //a . & A sh*A' ^>i"rsMi'TjSAy+^ Tj <~z/ /T\Jk A ^/v^s>Cy?pA / Jt+ '/^"V-^ ^... ^ 'IM A < L ^ ( f 1>(e> <! <) > J A--t, C^-vT - y jl f f /O ^ Y ^ y ^ y/S H A , r f-T \~ A * r * & <*^^+1/1 n 'rlM T& A y -F * dLbQ-C^6X J ^ C c ^ e J-ZTxaS J L ^ i - C i t ^ X t2 ^ . h *4 < L ~ y J b / A f r \ j Qsv\d^ 10 v '~b* ^ c, d_ -AAd-icLA*, _________________________________ L -- t?CT^I /jy \ & ^4 g^ - J ( C } k ^dA _^__A_______-f_a___._______ ^ -Jbr\ < ^ v __y~^g_^2i U d . / & > Q ^ v T < ~h 4.2__ s___ T l ^ __'^V^y~p^pioj /u. M./!/\.e* / * * ____^ sitfyV L _o le \/* .Jj&^ ..^ /U ^ IA J lX ^ A M vxjt tv^ %4n S irru iX ^ __a^klS/rr? .ssuC A ____________ <Afl_A ,yy^. TOd l j ^ ^ r t r c a ^ y jjt Atsaxu A & u d td ^ A f t . A r i ^ ^ r A ^/;/ ^ "" AiiuwJi 6W. ^k)LA ,^^X^rzau 4 ^ 7 W /f^ XU714- "/nr^ UAILv^. z/ffta-a'. l^t f r*>\frvi Q-*>2^ Qp&-\$,'Z^yya ) Vi<3^V/c'^ H 2.A. t p, 5 ~ i Reviewed by: 000955 r O t t M tO < 2 0 - |- P W O BEST COPY AVAILABLE S'5'V/ File: Page No. ENVIRONMENTAL ENGR. LAB - WORK SHEET SAMPLE DESCRIPTION Da,.: Analyst: O O . Hr$.: __________________ ~ 66c() '-a \ JL^k 1 2 - ,____ L A /llA & tu n i i M ^ u / rr^ { r ^ /-&. ________CM &h S v t . Yt J L ,, Ma, U & A ,juJ s , MaC.I-y .-n/aa JJj ,___ 7 ^ x t a*. /^yyi^A>r^A> ypr ^y^U A A x. J & h c A - L^o -7 *jJ b A -f ___< c U jl VuH,,, /K s Q u S i* rv<A. _____ _d|ti /S) vMe 'ir t2 A ^ < * A jl^ l^ X a^t y ^ IM A a u X a ,* . 5 V > aJ s-& \ /'Urn $ ,S v l f '^~> ^ U l. jts A 7\t>. 2 1 , 7^iL JX) ^ r t * < u r*k \jr% 6 - A r? ^ 'v v ^ Q v .^ 0 .^ > J r ... ^ f.1 ^-<V^ ~- pyy^Q &0Us\ - * R jL & vu tX a, 'S ' S'-aJ q P g -ii ir 'b P C - >*< / A P A Y -0 z w -is q X > C . "Rji vA/s+jt*s^q Jf 28<w ^ "1^ / '; i l <* /- 3 ''fc -id ) % ? } *ft-1 2 - 3 (F c -y > n ) ti T l ] ` Ji-<' 3 - 3 ( fC -2 d6 ) , % \\ \c s ^ / 3 1 t 'A if f `tJAMnrrJ r fy -- y -- -------------- .7 I M W - L - I - D oa - , 3 f 3^*7 > 7 / 0 i'0 ( ^ k j ^ l d X 'x/9 . <20 I ^ i V / . o - /v; ' 0 0 < / * / i , 0 { t-2 / / y . t J 15. t ii>7 0 ^ ,<t Z A l y 0 : ^ . X ^ o _________ T T f T f f ^ , 1 ' ____________ ^ L L ii i -. - . { f l , - ' O') to 0 O-C--.---R---&--r-v--'---d--u-s--v--^^/y^ i _ ( D > a* D C 4 0>jLs*M o dou^ . (C 5 C X - M l - 5 5 c 4 / 9 Reviewed by: 0U95 FORM10420 IPWO BEST COPY AVAILABLE File: p # No. ENVIRONMENTAL ENGR. LAB - WORK SHEET '' I^ I SAMPLE DESCRIPTION Date: ...( 0 7 _ Analyst: U J . Q ,^r C j u C Hrs.: ______________________ C _ So /. TO C - ti yfA ^ v p <^c> ^ /A n - ( d l^ U , ~h> A J i ________/^iy p s/^ L sC s p jju IC C fa"'A 4 ^ v # V < v t c < r v O 1 Pa j t c u /^ iA A U ij r f t J t ; , /ru s C 1 *^ b A ^ t i d p * & i i j & ca f tjr & J l ^/7djLLS lV jJ/iJj4\ / y T & A i- { I* & - X 'V \ Js 1A-^> *V 4 O bV ^ K tr i ./ w = ^ A a L . - //-&/ 1/ - 2 ) V/g /.oo -v >utA .A H J-C Z ; L ^ itS s r jU L - nruA & u^rA sL .^ r S u t is y p O p d -^ Mn //yY i'isMA Jj rrvUc.^s^jl'^^ ^sfitkKuA.- 2 SO ^r*-& ^ W ^ r f ~THt aAe4m_(2, S0 4 /,. j s \ s*i U y A - ^ 'S g ^ k c J . 4A OOAL /\M W K O ^ r^ . r & 4 ) a i^ u ^ ^ l _____________________________ L________ ( j t ^ n a yCtiAA~tA>j^ F C ' 2 0 Z U f f i J T Q C ____L4 ~ . , O P Q . : r e j ^ a r ^ .J jL -------------------------------------------------------------------------------------------------------------- 4 /O^v^ C< r ivrv>^ 7~^^- y )po/?^ c^IiL^ looo ^ ^ 0,Q*%2- g|iF d * ^ 3 roc Ma K, su~-. - J p z J A rjU hiA /^ FC- ^ a O . t oT -. no 3 (j`12,oeo1^Tac./A-, n--y-.~) ^ da^yyjl-L ..-. ^ Oyv*-^ "10C y Koo foo AOrt-p -i, y I QPQ ^ ___ l ^l j odo w^ '-xi_ i.qo^fc ~ 0 . 2 0 2 ^ F C - 3017 k.^-3 _ i'^v^v^a F - 2. L ( P r A - - \ % W ' ) l r 3 * x n . l O h l S%^a iCtVar^y>-^L^ 40 yvv^-T?)<C y L o j i ^ U y ;j >.4i&j Fc-ao( h ^ d i/la iu -n r ^ j L !>` `irftC ' -- ^ <L<x2/^rvv< - 'TOC. Reviewed by: 003S7 nOmq- . O 3 0 e r 5 . 6 w p ie 0 - ^ (< Co n t r o l C&l a k j K> c -l C-J. && A C -3 CAt L \ B M r TfO^ Co/'APou.fJli -(, v - j. A& A Y -3 S^ta Pl -M t-/ (-1 a f-* >0C as*^*-&<^ajL4* A*. A <as*^ Luqj- Pa . S*w Pu5 * -12. x - i A x-*3 . 'SlhrWf\.t *^7 3-1 3-2. A& A 3 -3 T ^ t Q * , * ! _6 ^ " O j ^ M ^ 2-1 , 2 i 2J. ^ ^ M v -U *. DOd 1 G^<-^^^i<r^X/S"-rvv^l4- -- ^0 tfb Oi^w^ixA- <sr\ c U t^ i^ a A ^ - I ^ f^ y ^ > ( P ' - P K/i2j|? 'h w ^ c l^ LS / V' ^ --- 77 77 c^ A ^ v ^ f i jLfrvJ ^^yyQA^ro^-K. f AJ piLs\S TC . BEST COPY AVAILABLE 000958 FO RM I OCZO't'FW O BEST COPY AVAILABLE File: <<gage No. S4-i S ENVIRONMENTAL ENGR. LAB - WORK SHEET SAMPLE DESCRIPTION ( VdC Date: S- V ~ * Analyst: U* . ^ Hrs.: __________________ F C -U l fay 7) Ts - /.yv JP * f * j 1- 3 7-V - ( - q- q " ! y lo t o - G <S *7 r I- m,<- i v - ZD. I % MC^J '3*7. ^ c -^>3 /vj /- .y-o.y Ho*i y /oo c S 3 8 /, "\ 8f. f ^ / i- Z L - 1Sc too 2. /7. 2- J - Zo? 'V O i>'tS - 1 1- L 5 -l' 1 y/ao__- .s O Vo-./ i ________ L ^13*7_____________________ ______________ k>- , 1 f ~ ^>7 ; yg/ 2.._._-_7=J/__X___J__o__^_________I____n__.__c_ V________________ _______ _____ 1 0 1 1 c fc * lo V ,} b-f , - -, n . / v / o 0r 1* b 3 % ^ Vo/ -- > 7/V . 4 . 2 -o .c .^ )?tou *. 7/. Vfl.i ___ Dj. J -. IJ - 2 s - 0 j '/a I - J.g-o Vol y ion -- g 93V- j ! Reviewed by: 000959 FORM I0420-9 PWO BEST COPY AVAILABLE File: PageNo. **^^ ^ ENVIRONMENTAL ENGR. LAB - WORK SHEET SAMPLE DESCRIPTION - ( *- /~A * *i rC-3617 '`V ) ( OC AWL 11 " ' .. P i , -- , t - ^0.% ~ ( - 0 . 0 c Ar / oo - U - I.H -- - 39.*7 Date: S ~ Z 2 - ________ Analyst: O. Q &. k>^-Q \ Hrs.: ------------------------------------3 <2<3>Cl^7 'l (3 -)^ _________ Pa > /" i ^/ n * - r-./) b 8 - /.V */= Ho.H S J.-'/, )t, r / 1 - 2-W'O.V y./DO - ^.0*7 1 -- 1------J---------------------------------------------------------------------- L $1-7 ^____________________ { ^ ____________________ O/ -~ r i- 3.^-.V ^/dO C. 1^* J r C '\*n p /- ' i . O ' h t j y/&0 > *7, 'S 31) Di - ) /- 5*7 J 2 ,9 - A2 ~" v */>n ^_______ Vo.Y - %% fc-ii7 r -t u hri- 1 X'*0~ ^ .7 j f % *% /- i%o-o,tr]X/^or %'$*!* ) L ^O'V J FC'ion \J % , -- r < - /,r-<>7 V/dO ~ %'Ml L 3%7 J r>, - r i- 3,a-._. jy /i t w.tf) LJ Reviewed by: ' 000960 FORM 10I20-CFWO BEST COPY AVAILABLE File: Page No. ENVIRONMENTAL ENQR. LAB - WORK SHEET SAMPLE DESCRIPTION C jJltu JU iX i'0^' H ihk--- .1^4- ~f .('`L).~)y ---------- 7) L v;, *-/.</ J ^ Date:__'____L _I_-__S__o________ Analyst: & S* P Hrs.: _____________________ wefrjJ ? 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