Document Vj5BVQVo69oL4q6q0E2Va94qg

AR226-2619 2003-DuET-?? DRAFT AR226-2619 Distribution on last page DuPont Engineering Technologies Wastewater Group Brandywine DuPont Company Carbon Adsorption Isotherm Evaluation for Perfluorooctanoic Acid (PFOA) In Samples From Chambers Works Wastewater Treatment Facility Final Report Work Done By: Stephen Constable, Lynn DeKleva, Barbara Larsen, Stan Bachmura, R. K. Bell, Mark Richmond, Steve Breske Report Written By: Stephen Constable Previous Related Validation o f Liquid Chromatography (LC) Analysis with Tandem Reports: Mass Spectrometry (MS/MS) o f Perfluorooctanoic Acid (PFOA) In Samples From Chambers Works Wastewater Treatment Facility, Analysis o f Perfluorooctanoic Acid (PFOA) In Samples From The Chambers Works Wastewater Treatment Facility Project Code: Period Covered: 06/2003-09/2003 Notebook Numbers: E93384FC Date of Issue: 5/31/04 Reviewed by: Maria Angelo, Steve Breske, Mark Richmond, Irene Legeic, Bob Reich, Paul Jann, Charlie Zarzecki, Bill Berti, John Gannon, Mary Kaiser, Carl Camp Approved by: N/A Information in this report is proprietary and should be handled according to the designated Proprietary Information Protection (PIP) classification listed below. Abstract : Carbon adsorption isotherms were determined for synthetic salt solution, primary clarifier effluent, primary clarifier underflow and mixed secondary/tertiary aerator solid samples taken from the Chambers Works wastewater treatment system. These tests show that the powdered activated carbon used by Chambers Works, primary clarifier and the combined aerator solids adsorb PFOA. Keywords carbon adsorption isotherms, perflurooctanoic acid (PFOA)l [Enter PIP Class] l MM/DD/YYYY 1997-SBU-?? Table of Contents TABLE OF CONTENTS---------------------------------------------------------------------------------------------------2 Introdu ction a n d O b je c t iv e s............................................................................................................................................ 3 Sum m a ry and C o n c lu sio n s................................................................................................................................................. 3 T he isotherm tests show ed that the virgin PAC used by th e CW SET system is capable of ADSORPTION OF P FO A IN PRIMARY CLARIFIER EFFLUENT OR IN A SYNTHETIC WASTEWATER SIMULATING TERTIARY S E T EFFLUENT. THE SET M LSS AND PRIMARY CLARIFIER UNDERFLOW SAMPLES ALSO SHOW SIMILAR BEHAVIOR, THOUGH IN THESE EXPERIMENTS THEY HAD A LOWER CAPACITY ON A UNIT DRY WEIGHT BASIS FOR P FO A ADSORPTION THAN VIRGIN P A C ................................................................................... 3 P a ten t Sit u a t io n ..................................................................................................................................................................... 3 P r o g r a m ...................................................................................................................................................................................... 3 P ublication St a t u s .................................................................................................................................................................3 P er so n n el....................................................................................................................................................................................4 Safety and W a ste D ispo sa l ................................................................................................................................................4 Enviro nm ental C o n sid e r a t io n s...................................................................................................................................... 4 A ck now ledgm en t.................................................................................................................................................................... 4 Sig n a tu res...................................................................................................................................................................................4 Test S ubstance........................................................................................................................................................ 6 Reagents and Solvents..........................................................................................................................................................** Analytical protocols:.........................................................................................................................................-.................. Experimental Protocol:......................................................................................................................................................... 8 Application Information........................................................................................................................................................ 8 Test System............................................................................................................................................................................. D iscussion of Re su l t s.......................................................................................................................................................... 12 R e f e r e n c e s ............................................................................................................................................................................... 16 APPENDICES.................................................................................................................................................. 17 A ppen d ix A: Sug g ested P rotocol F o r Sa m p l in g .....................................................................................................17 A ppendix B: Liquid C hromatography and Liquid Chrom atography T andem M ass Spectrometry fo r P erfluorooctanoic A cid (PFO A ) Q u an titation............................................................................................. 17 A ppen d ix C: Isotherm T est R esults fo r R o u n d 1 and R e t e s t in g .................................................................... 17 DISTRIBUTION FOR COMPANY PROGRESS REPORTS..................................................................... 18 [Enter PIP Class] 2 MM/DD/YYYY 1997-SBU-?? Carbon Adsorption Isotherm Evaluation for Perfluorooctanoic Acid (PFOA) In Samples From Chambers Works Wastewater Treatment Facility Final report Introduction and Objectives Perfluorooctanoic Acid (PFOA) is a compound used for the production o f fluoropolymers in DuPont. PFOA containing wastewaters are discharged to the Chambers Works (CW) site wastewater treatment system, which is operated by Secure Environmental Treatment (SET). To better understand the fate o f PFOA in the CW treatment system, a series of carbon adsorption isotherm tests were performed. The tests used a sample o f the same virgin powdered activated carbon (PAC, i.e.Calgon WPX-D) that SET uses in the site treatment system spiked into either synthetic wastewater effluent or an actual sample of SET primary clarifier effluent. In addition, isotherms were separately developed for the high solids containing primary clarifier underflow and mixed liquor suspended solids (MLSS) samples taken from CW secondary and tertiary aeration basins. Summary and Conclusions The isotherm tests showed that the virgin PAC used by the CW SET system is capable of adsorption o f PFOA in primary clarifier effluent or in a synthetic wastewater simulating tertiary SET effluent. The SET MLSS and primary clarifier underflow samples also show similar behavior, though in these experiments they had a lower capacity on a unit dry weight basis for PFOA adsorption than virgin PAC. Patent Situation N/A Program The program is described below. Publication Status N/A3 , [Enter PIP Class] 3 MM/DD/YYYY 1997-SBU-?? Personnel Name(s) Location(s) Stephen Constable Lynn DeKIeva Barbara Larsen R. K. Bell Steve Breske Stan Bachmura B9248 G300/208 E228/120A DCSE-CW B8432 Safety and Waste Disposai N/A Environmental Considerations N/A A ckn o w ledg m en t Signatures Signature(s) of the author(s) should appear here. Period(s) of Assignment [Enter PIP Class] 4 MM/DD/YYYY 1997-SBU-?? E xperim ental Description o f the Chambers Works Wastewater Treatment System and Rationale Behind Sample Matrices Used in This Study The CW site treatment operations o f interest to this work consist o f influent neutralization using lime, primary gravity clarification and removal o f solids and powder activated carbon (PAC) assisted biological treatment (PACT) in secondary and tertiary polishing units prior to discharge o f treated effluent to the Delaware River (after mixing with other site waters). Figure 1 shows the unit operations and sampling spots of interest to the work discussed in this report. Figure 1: Chambers Works Non-Hazardous Treatment System and Sampling Spots Discharge to River [Enter PIP Class] | To Belt | Press ------- Dewatering 5 MM/DD/YYYY 1997-SBU-?? Test Substance Name: Synonyms: Active substance: CAS Name: CAS Number: Supplier: Product Number: Lot Number: Molecular Formula: Formula Weight: Concentration of a.s., nominal: Certificate o f Analysis Date: Solubility: Appearance: Ammonium perfluorooctanoate Ammonium pentadecafluorooctanoate; Ammonium perfluorocaprylate; DS 101; Fluorad FC 143; Perflurorooctanoic acid ammonium salt; Unidyne DS 101 Octanoic acid, pentadecafluoro-, ammonium salt Octanoic acid, pentadecafluoro-, ammonium salt 3825-26-1 Fluka Chemical Company 1001 West St. Paul Milwaukee, WI 53233 USA 77262 421207/1 24501 C8H4F 15N 0 2 431.1 g/mole > 98.0% 24-Jan-01 0.1 g/ml White Powder Reagents and Solvents All chemicals and solvents were o f reagent grade or purer and were purchased from the following suppliers: Calcium chloride dihydrate (Mallinckrodt); Sodium sulfate (Baker); Sodium hydroxide (Ricca Chemical); Hydrochloric acid (Baker) Methanol used for extractions (Burdick & Jackson), Methanol HPLC grade (EM Science), and Ammonium Acetate ACS grade (EM Science). [Enter PIP Class] 6 MM/DD/YYYY 1997-SBU-?? Test Materials Lab experiments were devised to determine the adsorption behavior o f PFOA according to the operational practices and in the wastewater matrices common to the SET system: 1. PAC is added to the SET system at both the primary clarifier effluent and in tertiary influent, with the split varying according to the seasons, treatment efficiency and other factors. Therefore, one isotherm test case used filtered primary clarifier effluent. Given that PFOA may be present in any effluent sample taken from the SET system and given that the PFOA concentration could not be determined prior to testing, a synthetic salt sample was prepared for isotherm testing so as to simulate the wastewater matrix found in the tertiary influent but without background PFOA present. This synthetic wastewater was prepared by spiking the major cations and anions found in the SET effluent into distilled water along with a known addition of PFOA. 2. The CW SET system is a complex treatment system, where PAC is co-mingled with activated sludge for enhanced removal. In order to gain some insights into PFOA fate in such a system, a series o f isotherm tests were devised where PFOA was spiked to a mixture o f secondary and tertiary solids. In addition, PFOA was spiked to primary solids to gain insights into PFOA partitioning in primary clarification. Distilled water was used to dilute some of the primary and secondary/tertiary samples so that a wide range o f final solution PFOA concentrations could be obtained. Samples o f primary clarifier underflow, primary clarifier effluent, secondary aeration mixed liquor suspended solid (MLSS) and tertiary MLSS samples, and virgin powdered activated carbon (PAC Calgon WPX-D) were taken from the CW treatment plant system for use in the study. The primary clarifier underflow sample from primary clarifier CF-64 and the MLSS samples from Spot 627 (secondary treatment) and Spot 628 (tertiary treatment) were grab samples collected on May 27,2003 and refrigerated until use. The Primary clarifier effluent (CF-64) was a 24-hr composite sample collected from 529 spot on May 29,2003 and refrigerated until use. The virgin Powdered Activated Carbon (PAC) was obtained from DuPont Secure Environmental Treatment (SET) and was stored at room temperature. All samples were collected in accordance with the principles explained in Appendix A. Test solutions were prepared as follows: The salt solution was prepared by dissolving calcium chloride (1400mg/L) and sodium sulfate (1250 mg/L) in deionized water. Hydrochloric acid and/or sodium hydroxide were used to adjust the final pH o f the solution to 7-7.8 The primary clarifier effluent was centrifuged for 10 minutes at 6000 RPM (Sorvall RC-5 HS-4 Rotor) and supernatants filtered (Pall Gelman 4190) prior to use. A mixed MLSS sample for isotherm testing was prepared by combining secondary and tertiary MLSS samples at a ratio o f 3:1 in order to simulate the ratio o f tertiary to secondary solids in the CW system (tertiary solids are wasted to secondary and [Enter PIP Class] 7 MM/DD/YYYY 1997-SBU-?? secondary is wasted to the belt presses for dewatering prior to landfilling dewatered cake on site). Analytical protocols: To determine soluble parameters, samples were centrifuged for 10 minutes at 6000 RPM (Sorvall RC-5 HS-4 Rotor) and supernatants filtered (Pall Gelman 4190) prior to analysis. Total PFOA was determined by sonicating the sample with equal parts methanol for 1-hr. Analytical samples were refrigerated or frozen until analysis. The total solids and total suspended solids o f the primary underflow and MLSS samples were determined according to protocols outlined in Standard Methods for the Examination of W ater and Wastewater, 20th Edition. (1998) American Public Health Association, Washington, DC. PFOA was analyzed per the procedures described in Appendix B. Experimental Protocol: Application Information The test substance was administered from a 1000 mg/L stock solution in deionized water (Bamstead E-Pure Water Purification system) prepared in a polypropylene volumetric flask (Nalgene 4000-0050). The stock solution was prepared the day o f testing and stored at room temperature until use. Test System The test system employed in this study consisted o f individually capped 50-mL polypropylene conical tubes (Falcon BD 35 2070), uniquely identified, containing the salt solution, primary clarifier effluent, primary clarifier underflow or MLSS samples. The tubes were mixed using an end-over-end rotator (Glas-Col Rotator Model 099A RD4512) at 30-35 RPM at an ambient temperature o f 19-25C. The temperature was monitored using a Dickson THDx Temperature recorder, which had a resolution of 0.5 C and accuracy o f +/-1 C. Following incubation, the samples were centrifuged for 10 minutes at 6000 RPM (Sorvall RC-5 HS-4 Rotor) and supernatants were transferred to 50-mL polypropylene tubes using a disposable pipette (VWR 53283 706). Aliquots (5mL) o f the supernatants were filtered (Pall Gelman 4190) in 14-mL polypropylene tubes (Falcon 35 2059) using a 10-mL disposable syringe (BD 309695). Samples were diluted (if required) and submitted for analysis in polypropylene vials (Agilent 5182-0567) sealed with a natural rubber crimp seal (Agilent 5182-1210). Analytical samples were refrigerated or frozen until analysis. [Enter PIP Class] 8 MM/DD/YYYY 1997-SBU-?? For determining total PFOA concentrations in select samples, PFOA was extracted by sonicating well mixed aliquots with methanol for one hour. Samples were filtered (Pall Gelman 4190), diluted (if required) and submitted for analysis. Isotherm R ound 1 Testing: Salt Solution and Prim ary C larifier Effluent PAC material was weighed directly into 50-ml polypropylene conical tubes, according to the study outline presented in Table 1, and 50-ml o f salt solution or primary clarifier effluent was added. The test substance was added from a stock solution to the test vessels to achieve a target test concentration o f 15 mg/L. Control tubes (test substance in salt solution or filtered effluent without PAC), solution blanks and PAC blanks were prepared and processed with the adsorption samples. The test vessels were placed on the end-over-end rotator at 30-35 RPM at ambient room temperature. After 48 hours at ambient temperature, the tubes were centrifuged for 15 minutes at 6000 RPM (Sorvall RC-5B refrigerated centrifuge, HS-4 rotor). The supernatants were transferred to 50-mL polypropylene tubes, aliquots were filtered and submitted for determination of the test compound. T able 1: Salt Solution and Prim ary Clarifier Effluent Isotherm Test M atrix Target Target PFOA PAC spike W t Cone Sample Description 8 mg/1 PAC addition Control 4.3 0 Control 00 Spiked PFOA PAC addition 0.025 15 Spiked PFOA PAC addition Unspiked PFOA PAC addition / Desorb Control 0.28 15 0.28 0 Spiked PFOA PAC addition 0.55 15 Spiked PFOA PAC addition 0.75 15 Spiked PFOA PAC addition 1.7 15 Spiked PFOA PAC addition 4.3 15 [Enter PIP Class] 9 MM/DD/YYYY 1997-SBU-?? z / iin u i Isotherm Repeat Testing: Salt Solution and Primary Clarifier Effluent The PAC isotherm, as described the preceding section, was repeated for primary clarfier effluent and salt solution with the following modifications: A test solution was prepared by spiking the test compound (from a stock solution) to the desired test concentration o f 15 mg/L into the salt solution or primary clarifier effluent. A 50-ml aliquot o f the test solution was added to test system. The PAC test weights were expanded according to the study outline in Table 2. Table 2:Salt solution and Primary clarifier effluent Isotherm Re-test Matrix Sample Description PAC addition Control Control Spiked PFOA Control Spiked PFOA PAC addition Spiked PFOA PAC addition Spiked PFOA PAC addition Spiked PFOA PAC addition Unspiked PFOA PAC addition Spiked PFOA PAC addition Spiked PFOA PAC addition Spiked PFOA PAC addition Spiked PFOA PAC addition Spiked PFOA PAC addition PAC (g) 4.3 PFOA (ppm) 0 00 0 15 0.025 15 0.05 15 0.1 15 0.28 15 0.28 0 0.55 15 0.75 15 1.7 15 4.3 15 0.005 15 Test M atrix Salt Solution and Primary Clarifier Effluent Salt Solution and Primary Clarifier Effluent Salt Solution and Primary Clarifier Effluent Salt Solution and Primary Clarifier Effluent Salt Solution and Primary Clarifier Effluent Salt Solution and Primary Clarifier Effluent Salt Solution and Primary Clarifier Effluent Salt Solution and Primary Clarifier Effluent Salt Solution and Primary Clarifier Effluent Salt Solution and Primary Clarifier Effluent Salt Solution and Primary Clarifier Effluent Salt Solution and Primary Clarifier Effluent Salt Solution only [Enter PIP Class] 10 MM/DD/YYYY 1997-SBU-?? Isotherm R ound 1 Testing: Prim ary Solids Aliquots (50-ml) o f the primary clarifier underflow solids, primary clarifier underflow solids diluted with distilled water or distilled water alone were added to 50-ml polypropylene conical tubes and the test compound was added from a stock solution according to the study outline shown in Table 3. The test vessels were placed on the end-over-end rotator at 30-35 RPM at ambient room temperature. After 48 hours at ambient temperature, the tubes were centrifuged for 15 minutes at 6000 RPM (Sorvall RC-5B refrigerated centrifuge, HS-4 rotor). The supernatants were transferred to 50-mL polypropylene tubes, aliquots were filtered and submitted for determination o f the test compound. Table 3: Primary Clarifier Underflow And Mixed MLSS Solids Isotherm Test Matrix Aliquot # Parts sludge Control Spiked Control Lowest PFOA concentration Sludge Low PFOA concentration Sludge Sludge Only Spiked Sludge Spiked Sludge Spiked Sludge 0 0 1 2 1 1 1 1 Parts distilled w ater 1 1 2 1 0 0 0 0 COI spike (PPm) none 1 none none none 0.5 0.75 1 Isotherm Round 1 Testing: M ixed MLSS Isotherm testing The secondary and tertiary MLSS samples were combined at a ratio o f 3:1, respectively. Aliquots (50-ml) o f the Mixed solids, mixed MLSS solids diluted with distilled water or distilled water alone were added to 50-ml polypropylene conical tubes and the test compound was added from a stock solution according to the study outline in Table 3. The test vessels were placed on the end-over-end rotator at 30-35 RPM at ambient room temperature. After 48 hours at ambient temperature, the tubes were centrifuged for 15 minutes at 6000 RPM (Sorvall RC-5B refrigerated centrifuge, HS-4 rotor). The supernatants were transferred to 50-mL polypropylene tubes, aliquots were filtered and submitted for determination o f the test compound. [Enter PIP Class] n MM/DD/YYYY 1997-SBU-?? J ljt J Isotherm Repeat Testing: Primary Clarifier Underflow and Mixed Secondary/Tertiary Solids Isotherm testing was repeated for the primary clarifier underflow and mixed secondary and tertiary MLSS samples according to the revised test conditions shown in Table 4 below: Table 4: Primary Clarifier Underflow And Mixed MLSS Solids Isotherm Repeat Test Matrix Sample Description Spiked Control Unspiked sludge Control Spiked Sludge Test Spiked Sludge Test Spiked Sludge Test Spiked Sludge Test Spiked Sludge Test Unspiked diluted Sludge Test Parts Sludge 0 1 1 1 1 1 1 1 Parts DI H20 1 0 0 0 0 0 0 1 Test Cone (ppm) 1 0 0.1 0.25 0.5 0.75 1 0 Discussion of Results The analytical results o f the isotherm testing for all matrices are included in Appendix C as Tables C l and C2 for the synthetic salt and filtered primary clarifier effluent wastewater matrices, respectively. Analytical results for the primary clarifier underflow and mixed secondary/tertiary solids are included as Table C3. Table C4 shows the total and soluble PFOA results and computed extraction efficiencies for the high solids (i.e. primary clarifier underflow and secondary/tertiary solids) samples used in this study. Isotherm graphs were developed by determining the total amount of PFOA adsorbed to the solids per unit dry weight of solid (PAC, primary clarifier underflow or secondary/tertiary solid) for each test condition's equilibrium soluble PFOA concentration. Graph 1 shows the isotherms for the filtered primary clarifier effluent and synthetic salt solutions while Graph 2 shows the isotherms for the primary clarifier underflow and mixed secondary/tertiary solids, respectively. Graph 3 shows the isotherms for the primary clarifier underflow and mixed secondary/tertiary solids after correcting for extraction efficiency. Graph 4 shows the results for all tested matrices. On a unit dry solids basis, PFOA adsorption appears to be highest in synthetic salt, followed closely by primary clarifier effluent; it is less well adsorbed by PACT and least well adsorbed by primary clarifier solids in these tests. [Enter PIP Class] 12 MM/DD/YYYY 1997-SBU-?? Graph 1: Sorption ofP F O A from Spiked Filtered Prim ary E ffluent EQUILIBRIUM LOADING, mg PFOA/g PAG [Enter PIP Class] 13 MM/DD/YYYY 1997-SBU-?? JL /J.1^ JLX JL Graph 2: Sorption of PFOA onto Primary and Combined Secondary/Tertiary Solids SOL 1ASE PFOA LOADING, mg/g [Enter PIP Class] 14 MM/DD/YYYY 1997-SBU-?? Gfcaph3: Sorption o f PFOA onto Primary and Combined Secondaiy/Tertiaiy Solids JD PHASE PFOA LOADING, mg/g [Enter PIP Class] 15 MM/DD/YYYY 1997-SBU-?? i/J IU T X i | Graph 4: Sorption ofPFO A onW PX -D PAC for Filtered Primary Effluent and, Synthetic Salt Solution and on 2/3 MLSS or Primaiy Clarifier Underflow EQUILIBRIUM LOADING, mg PFOA/g PAG or mg PFOA/g PACT References N/A [Enter PIP Class] 16 MM/DD/YYYY 1997-SBU-?? JW JLX Y -LM . JL Appendices Appendix A: Suggested Protocol For Sampling Appendix B: Liquid Chromatography and Liquid Chromatography Tandem Mass Spectrometry for Perfluorooctanoic Acid (PFOA) Quantitation Appendix C: Isotherm Test Results for Round 1 and Retesting [Enter PIP Class] 17 MM/DD/YYYY 1997-SBU-?? X/XV/11 X Distribution for Company Progress Reports Copy of Reports Sent To: Author(s): Additional recipients: Documentation Clerk: Director(s): Associate Director(s): Supervisors): Manager(s): Manager-Patent Section: CR&D Technical Records Center: [Enter PIP Class] 18 MM/DD/YYYY 1997-SBU-?? x /J L n i x Appendix C: Isotherm Test Results for Round 1 and Retesting Table Cl: PFOA and Total Suspended Solids Test Resultsfor the Synthetic Salt Solution _______ Sample Description PAC dose (g) Soluble P F O A -lst Test ug/l Soluble PFOA Repeat Test Result ug/l Soluble PFOA Repeat Test Desorb ug/l Unspiked Salt Solution Control 1 4.3 <LOQ Unspiked Salt Solution Control 2 0 <LOQ Salt Solution Control w/ 15 ppm Nominal spike 0 21388 Salt Solution PAC addition Desorb Control 0.28 <LOQ Salt Solution PAC addition Control 15 ppm Spiked Salt Solution PAC addition 0.005 0.025 4s 5 53.9 12 2(i 15 ppm Spiked Salt Solution PAC addition 0.05 1 44 15 ppm Spiked Salt Solution PAC addition 0.1 "LOQ 15 ppm Spiked Salt Solution PAC addition 0.28 <LOQ i ng 0) Unspiked Salt Solution PAC addition Control 15 ppm Spiked Salt Solution PAC addition 15 ppm Spiked Salt Solution PAC addition 0.28 0.55 0.75 <LOQ <LOQ <LOQ OS 15 ppm Spiked Salt Solution PAC addition 1.7 <LOQ 15 ppm Spiked Salt Solution PAC addition 4.3 <LOQ [Enter PIP Class] l MM/DD/YYYY 1997-SBU-?? 1/ i i / l I JL Table C2: PFOA and Total Suspended Solids Test Resultsfor the Primary Clarifier Effluent Sample Description Unspiked PAC addition Filtered Primary Effluent Control Unspiked Filtered Primary Effluent Control 15 ppm spiked Filtered Primary Effluent Control Unspiked PAC addition Filtered Primary Effluent Desorb Control 15 ppm spiked PAC addition Filtered Primary Effluent Control 15 ppm spiked PAC addition Filtered Primary Effluent Control 15 ppm spiked PAC addition Filtered Primary Effluent Control 15 ppm spiked PAC addition Filtered Primary Effluent Control Unspiked PAC addition Filtered Primary Effluent Control 15 ppm spiked PAC addition Filtered Primary Effluent Control 15 ppm spiked PAC addition Filtered Primary Effluent Control 15 ppm spiked PAC addition Filtered Primary Effluent Control 15 ppm spiked PAC addition Filtered Primary Effluent Control PAC Dose (g) 4.3 0 0 0.28 0.025 0.05 0.1 0.28 0.28 0.55 0.75 1.7 4.3 Soluble PFOA-lst Test ug/1 <LOQ 69 <LOQ 13400 522 <LOQ 163 Soluble PFOA Soluble Repeat . l ' I O \ It t Repeat Test Result Desorb ug/1 ug/1 18345 VS2 0 65 mg 25 <LOQ <LOQ <LOQ [Enter PIP Class] 2 MM/DD/YYYY 1997-SBU-?? 1/11/11 X Table C3 PFOA and Total Suspended Solids Test Resultsfor the Primary Clarifier Underflow and Mixed Secondary/Tertiary MLSS Samples Sample Description Primary Solids Control 1 Total Suspended Solids-lst Test g/1 Soluble Total (O l Soluble Suspended Repeat COI-lst Solids- Test Total Test Repeat Test Result COI Test ug/1 g/i ug/1 "g71 <LOQ Primary Solids 1 ppm Spiked Control 1:2 Primary Solids: water dilution 1:2 Primary Solids: water dilution Primary Solids only Primary Solids w/ 0.5 ppm nominal spike Primary Solids w/ 0.75 ppm nominal spike Primary Solids w /1 ppm nominal spike Mixed Secondary/Tertiary Solids Control Mixed Secondary/Tertiary Solids Control w /1 ppm nominal spike 1:2 Mixed Secondary/Tertiary SoIids:water dilution 1:2 Mixed Secondary/Tertiary Solids:water dilution Mixed Secondary/Tertiary Solids only Mixed Secondary/Tertiary Solids w/ 0.5 ppm nominal spike Mixed Secondary/Tertiary Solids w/ 0.75 ppm nominal spike Mixed Secondary/Tertiary Solids w/ 1 ppm nominal spike 140 11.9 <LOQ 159 188 180 275 375 805 <LOQ <LOQ 89 113 136 173 220 597 1841 J32 4607 317 338 1451 12 2 841 488 452 [Enter PIP Class] 3 MM/DD/YYYY 1997-SBU-?? Table C4: Analytical Results For High Solids Samples Sample Spike Soluble PFOA Total PFOA recovered Extraction pg/L pg/L PFOA Efficiency H20 Control Primary Undeflow Primary Spike Secondary MLSS Secondary Spike Tertiary MLSS Tertiary Spike Mixed MLSS Mixed Spike 2342 1110 1251 380 1347 408 2002 398 1447 2461 4607 6688 843 2829 848 2834 841 2679 2081 1987 1986 1838 85% 81% 81% 75% [Enter PIP Class] 4 MM/DD/YYYY 1997-SBU-??