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Home My WebLink AboutNC0001422_ATT 5 - Speciation - J15060247F2_2015080513339 Hagers Ferry Road Huntersville, NC 28078-7929 McGuire Nuclear Complex - MG03A2 Phone: 980-875-5245 Fax: 980-875-4349 Order Summary Report Analytical Laboratory Order Number: J15060247 Project Name:SUTTON - AB GW ASSESSMENT SPECIATION Lab Contact:Peggy Kendall Date:7/1/2015 Customer Address: Customer Name(s):Perry Waldrep, Tim Hunsucker, Kathy Webb, John Toepfer Phone: Report Authorized By: (Signature) Program Comments: Please contact the Program Manager (Peggy Kendall) with any questions regarding this report. Data Flags & Calculations: Any analytical tests or individual analytes within a test flagged with a Qualifier indicate a deviation from the method quality system or quality control requirement. The qualifier description is found at the end of the Certificate of Analysis (sample results) under the qualifiers heading. All results are reported on a dry weight basis unless otherwise noted. Subcontracted data included on the Duke Certificate of Analysis is to be used as information only. Certified vendor results can be found in the subcontracted lab final report. Duke Energy Analytical Laboratory subcontracts analyses to other vendor laboratories that have been qualified by Duke Energy to perform these analyses except where noted. Data Package: This data package includes analytical results that are applicable only to the samples described in this narrative. An estimation of the uncertainty of measurement for the results in the report is available upon request. This report shall not be reproduced, except in full, without the written consent of the Analytical Laboratory. Please contact the Analytical laboratory with any questions. The order of individual sections within this report is as follows: Job Summary Report, Sample Identification, Technical Validation of Data Package, Analytical Laboratory Certificate of Analysis, Analytical Laboratory QC Reports, Sub-contracted Laboratory Results, Customer Specific Data Sheets, Reports & Documentation, Customer Database Entries, Test Case Narratives, Chain of Custody (COC) Certification: The Analytical Laboratory holds the following State Certifications : North Carolina (DENR) Certificate #248, South Carolina (DHEC) Laboratory ID # 99005. Contact the Analytical Laboratory for definitive information about the certification status of specific methods. Peggy Kendall Page 1 of 36 Sample ID's & Descriptions: Sample ID Plant/Station Collection Date and Time Collected By Sample Description 2015017803 Sutton 04-Jun-15 11:37 AM Synterra AW-5D 2015017804 Sutton 04-Jun-15 1:47 PM Synterra SMW-6C 2015017805 Sutton 04-Jun-15 3:06 PM Synterra SMW-3C 2015017806 Sutton 04-Jun-15 4:05 PM Synterra SMW-3B 2015017807 Sutton 04-Jun-15 3:55 PM Synterra ABMW-1S 2015017808 Sutton 04-Jun-15 11:26 AM Synterra ABMW-2S 2015017809 Sutton 04-Jun-15 10:33 AM Synterra ABMW-2D 2015017810 Sutton 04-Jun-15 12:19 PM Synterra AW-9D 2015017811 Sutton 04-Jun-15 1:02 PM Synterra AW-9C 2015017812 Sutton 04-Jun-15 2:02 PM Synterra AW-9B 10 Total Samples Page 2 of 36 COC and .pdf report are in agreement with sample totals and analyses (compliance programs and procedures). All Results are less than the laboratory reporting limits. All laboratory QA/QC requirements are acceptable. Yes No Technical Validation Review Checklist: Yes No Yes No Report Sections Included: Job Summary Report Sub-contracted Laboratory Results Sample Identification Customer Specific Data Sheets, Reports, & Documentation Technical Validation of Data Package Customer Database Entries Analytical Laboratory Certificate of Analysis Analytical Laboratory QC Report Chain of Custody Reviewed By:Peggy Kendall Date:7/1/2015 Electronic Data Deliverable (EDD) Sent Separately Page 3 of 36 Certificate of Laboratory Analysis This report shall not be reproduced, except in full. Order # J15060247 2015017803 Collection Date: 04-Jun-15 11:37 AM Site: AW-5D Matrix: GW_WW Analyte Analysis Date/TimeMethodUnits Qualifiers RDLResult Sample #: AnalystDF Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND Page 4 of 36 Certificate of Laboratory Analysis This report shall not be reproduced, except in full. Order # J15060247 2015017804 Collection Date: 04-Jun-15 1:47 PM Site: SMW-6C Matrix: GW_WW Analyte Analysis Date/TimeMethodUnits Qualifiers RDLResult Sample #: AnalystDF Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND Page 5 of 36 Certificate of Laboratory Analysis This report shall not be reproduced, except in full. Order # J15060247 2015017805 Collection Date: 04-Jun-15 3:06 PM Site: SMW-3C Matrix: GW_WW Analyte Analysis Date/TimeMethodUnits Qualifiers RDLResult Sample #: AnalystDF Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND Page 6 of 36 Certificate of Laboratory Analysis This report shall not be reproduced, except in full. Order # J15060247 2015017806 Collection Date: 04-Jun-15 4:05 PM Site: SMW-3B Matrix: GW_WW Analyte Analysis Date/TimeMethodUnits Qualifiers RDLResult Sample #: AnalystDF Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND Page 7 of 36 Certificate of Laboratory Analysis This report shall not be reproduced, except in full. Order # J15060247 2015017807 Collection Date: 04-Jun-15 3:55 PM Site: ABMW-1S Matrix: GW_WW Analyte Analysis Date/TimeMethodUnits Qualifiers RDLResult Sample #: AnalystDF Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND Page 8 of 36 Certificate of Laboratory Analysis This report shall not be reproduced, except in full. Order # J15060247 2015017808 Collection Date: 04-Jun-15 11:26 AM Site: ABMW-2S Matrix: GW_WW Analyte Analysis Date/TimeMethodUnits Qualifiers RDLResult Sample #: AnalystDF Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND Page 9 of 36 Certificate of Laboratory Analysis This report shall not be reproduced, except in full. Order # J15060247 2015017809 Collection Date: 04-Jun-15 10:33 AM Site: ABMW-2D Matrix: GW_WW Analyte Analysis Date/TimeMethodUnits Qualifiers RDLResult Sample #: AnalystDF Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND Page 10 of 36 Certificate of Laboratory Analysis This report shall not be reproduced, except in full. Order # J15060247 2015017810 Collection Date: 04-Jun-15 12:19 PM Site: AW-9D Matrix: GW_WW Analyte Analysis Date/TimeMethodUnits Qualifiers RDLResult Sample #: AnalystDF Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND Page 11 of 36 Certificate of Laboratory Analysis This report shall not be reproduced, except in full. Order # J15060247 2015017811 Collection Date: 04-Jun-15 1:02 PM Site: AW-9C Matrix: GW_WW Analyte Analysis Date/TimeMethodUnits Qualifiers RDLResult Sample #: AnalystDF Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND Page 12 of 36 Certificate of Laboratory Analysis This report shall not be reproduced, except in full. Order # J15060247 2015017812 Collection Date: 04-Jun-15 2:02 PM Site: AW-9B Matrix: GW_WW Analyte Analysis Date/TimeMethodUnits Qualifiers RDLResult Sample #: AnalystDF Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Vendor Method V_BRAND Page 13 of 36 3958 6th Ave NW • Seattle, WA 98107 • T: 206-632-6206 • F: 206-632-6017 • www.brooksrand.com • brl@brooksrand.com June 30, 2015 Peggy Kendall Duke Energy Analytical Laboratory Mail Code MGO3A2 (Building 7405) 13339 Hagers Ferry Rd. Huntersville, NC 28078 980-875-5848 Project: Duke Energy/Sutton (LIMS# J15060247) Mr. Perkins, Attached is the report associated with ten (10) aqueous samples submitted for hexavalent chromium, selenium speciation, arsenic speciation, iron speciation, and manganese speciation analyses on June 4, 2015. The samples were received in a sealed cooler at temperature of -0.2°C on June 5, 2015. Hexavalent chromium analysis was performed by ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS). Selenium speciation and arsenic speciation analyses were performed via ion chromatography inductively coupled plasma collision reaction cell mass spectrometry (IC-ICP-CRC-MS). All samples requesting iron speciation analysis were analyzed by spectrophotometry. Mn(II) analysis was performed via IC-ICP-CRC-MS. Mn(IV) analysis were performed via digestion and subsequent analysis by inductively coupled plasma triple quadrupole mass spectrometry (ICP-QQQ-MS). Any issues associated with the analyses are addressed in the following report. If you have any questions, please feel free to contact me at your convenience. Sincerely, Jeremy Maute Project Manager Brooks Rand Labs, LLC Page 14 of 36 Brooks Rand Labs, LLC Report prepared for: Peggy Kendall Duke Energy Analytical Laboratory Mail Code MGO3A2 (Building 7405) 13339 Hagers Ferry Rd. Huntersville, NC 28078 Project: Duke Energy/Sutton (LIMS# J15060247) June 30, 2015 1. Sample Reception Ten (10) aqueous samples were submitted for hexavalent chromium, selenium speciation, arsenic speciation, iron speciation, and manganese speciation analyses on June 4, 2015. All samples were received in acceptable condition on June 5, 2015 in a sealed container at -0.2°C. All samples were received in a laminar flow clean hood, void of trace metals contamination and ultra-violet radiation, and were designated discrete sample identifiers. Sample fractions requesting hexavalent chromium, selenium speciation, arsenic speciation, and iron speciation analyses were field filtered by the client. Two containers were submitted for each client sample requesting manganese speciation, one field filtered fraction and one unfiltered fraction. An aliquot of each sample submitted for hexavalent chromium analysis was filtered into a clean polypropylene tube. All hexavalent chromium sample fractions were stored in a secure refrigerator maintained at a temperature of 4oC, until the analyses could be performed. An aliquot of each sample requiring selenium speciation evaluation was decanted into a polypropylene centrifuge tube and each filtrate was stored in a secure, monitored cryofreezer (maintained at a temperature of -80°C) until selenium speciation analysis could be performed. The original bottles were then stored in a secure, monitored refrigerator (maintained at a temperature of ≤6oC). An aliquot of each sample submitted for arsenic speciation analysis was decanted into a polypropylene centrifuge tube; all fractions were then stored in a secure, monitored refrigerator (maintained at a temperature of ≤6oC) until the analyses could be performed. The sample fractions requesting iron speciation analysis were stored in a secure, monitored refrigerator (maintained at a temperature of ≤6oC) until the analyses could be performed. An aliquot of each filtered sample submitted for manganese speciation analysis was decanted into a polypropylene centrifuge tube for Mn(II) analysis. These fractions were stored in a Page 15 of 36 secure, monitored refrigerator (maintained at a temperature of ≤6oC) until the analyses could be performed. Subsequently, the original bottles (filtered and unfiltered fractions) intended for Mn speciation were preserved to pH < 2 with concentrated HNO3 and then stored in a secure polyethylene container, known to be free from trace metals contamination, until the digestion could be performed. 2. Sample Preparation All sample preparation is performed in laminar flow clean hoods known to be free from trace metals contamination. All applied water for dilutions and sample preservatives are monitored for contamination to account for any biases associated with the sample results. Hexavalent Chromium Analysis by IC-ICP-DRC-MS Prior to analysis, an aliquot of each sample was filtered with a syringe filter (0.45µm) and injected directly into a sealed autosampler vial. No further sample preparation was performed as any chemical alteration of a sample may shift the equilibrium of the system, resulting in changes in speciation ratios. Selenium Speciation Analysis by IC-ICP-CRC-MS Prior to analysis, an aliquot of each sample was filtered with a syringe filter (0.45µm) and injected directly into a sealed autosampler vial. No further sample preparation was performed as any chemical alteration of a sample may shift the equilibrium of the system, resulting in changes in speciation ratios. Arsenic Speciation Analysis by IC-ICP-CRC-MS An aliquot of each sample was filtered directly into a sealed autosampler vial. No further sample preparation was performed as a buffered EDTA solution was provided by Brooks Rand Labs for field-preservation of the submitted samples. Iron Speciation Analysis by Spectrophotometry No sample preparation was required as a de- gassed HCL solution was provided by Brooks Rand Labs for field-preservation of the submitted samples. Manganese Mn(II) Analysis by IC-ICP-CRC-MS An aliquot of each sample was filtered (0.45µm) directly into an autosampler vial for Mn(II) analysis. No additional sample preparation was performed as any chemical alteration of the samples may shift the equilibrium of the system resulting in changes in speciation ratios. Manganese Mn(IV) Analysis by ICP-QQQ-MS Each filtered and unfiltered sample submitted for Mn speciation analysis was preserved with 1% HNO3 (v/v) upon sample receipt. Each sample fraction was then further digested on a hotblock apparatus with aliquots of 50% HNO3 (v/v) and 50% HCl (v/v), in accordance with the digestion procedure specified in EPA Method 200.8. All resulting sample digests were analyzed for total manganese via inductively coupled plasma triple quadrupole mass spectrometry (ICP-QQQ-MS). Page 16 of 36 3. Sample Analysis All sample analysis is preceded by a minimum of a five-point calibration curve spanning the entire concentration range of interest. Calibration curves are performed at the beginning of each analytical day. All calibration curves, associated with each species of interest, are standardized by linear regression resulting in a response factor. All sample results are instrument blank corrected to account for any operational biases associated with the analytical platform. Prior to sample analysis, all calibration curves are verified using second source standards which are identified as initial calibration verification standards (ICV). Ongoing instrument performance is identified by the analysis of continuing calibration verification standards (CCV) and continuing calibration blanks (CCB) at a minimum interval of every ten analytical runs. Hexavalent Chromium Analysis by IC-ICP-DRC-MS Each sample for hexavalent chromium analysis was analyzed by ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS) on June 6, 2015. An aliquot of each sample is injected onto an anion exchange column and mobilized by a basic (pH > 7) gradient. The eluting chromium species are then introduced into a radio frequency (RF) plasma where energy-transfer processes cause desolvation, atomization, and ionization. The ions are extracted from the plasma through a differentially-pumped vacuum interface and travel through a pressurized chamber (DRC) containing a reaction gas which preferentially reacts with interfering ions of the same target mass to charge ratios (m/z). A solid-state detector detects ions transmitted through the mass analyzer and the resulting current is processed by a data handling system. Retention times for each eluting species are compared to known standards for species identification. Selenium Speciation Analysis by IC-ICP-CRC-MS Each sample for selenium speciation analysis was analyzed by ion chromatography inductively coupled plasma collision reaction cell mass spectrometry (IC-ICP-CRC-MS) on June 5, 2015. An aliquot of each sample is injected onto an anion exchange column and mobilized by a basic (pH > 7) gradient. The eluting selenium species are then introduced into a radio frequency (RF) plasma where energy-transfer processes cause desolvation, atomization, and ionization. The ions are extracted from the plasma through a differentially-pumped vacuum interface and travel through a pressurized chamber (CRC) containing a reaction gas which preferentially reacts with interfering ions of the same target mass to charge ratios (m/z). A solid-state detector detects ions transmitted through the mass analyzer and the resulting current is processed by a data handling system. Retention times for each eluting species are compared to known standards for species identification. Page 17 of 36 Arsenic Speciation Analysis by IC-ICP-CRC-MS All samples submitted for As speciation quantitation were analyzed by via ion chromatography inductively coupled plasma collision reaction cell mass spectrometry (IC-ICP-CRC-MS) on June 22-23, 2015. Aliquots of each sample are injected onto an anion exchange column and eluted isocratically. The eluting arsenic species are then introduced into a radio frequency (RF) plasma where energy-transfer processes cause desolvation, atomization, and ionization. The ions are extracted from the plasma through a differentially-pumped vacuum interface and travel through a pressurized chamber (CRC) containing a specific collision gas. Polyatomic interferences, due to their inherently larger size, collide more frequently with the collision gas and therefore may be separated from the analyte of interest via kinetic energy discrimination (KED). A solid-state detector detects ions transmitted through the mass analyzer on the basis of their mass-to- charge ratio (m/z), and the resulting current is processed by a data handling system. Retention times for each eluting species are compared to known standards for species identification. Iron Speciation Analysis by Spectrophotometry All sample fractions submitted for iron speciation were analyzed on June 5, 2015. The samples were analyzed for iron speciation in accordance with the scientifically accepted method outlined by: Stookey, L.L., (1970). “Ferrozine - A new spectrophotometric reagent for iron”, Anal.Chem., 42:779-81. Manganese Mn(II) Analysis by IC-ICP-CRC-MS All samples for Mn(II) analysis were analyzed by ion chromatography inductively coupled plasma collision reaction cell mass spectrometry (IC-ICP-CRC-MS) on June 5, 2015. Aliquots of each sample are injected onto an anion exchange column and mobilized by an acidic (pH < 7) gradient. An ion pairing agent provides a dynamic ion exchange mechanism for the cationic manganese species on the chromatographic column. The differences in the affinity of manganese species towards the ion pair agent and the column results in separation. The eluting selenium species are then introduced into a radio frequency (RF) plasma where energy-transfer processes cause desolvation, atomization, and ionization. The ions are extracted from the plasma through a differentially-pumped vacuum interface and travel through a pressurized chamber (CRC) containing a reaction gas which preferentially reacts with interfering ions of the same target mass to charge ratios (m/z). A solid-state detector detects ions transmitted through the mass analyzer and the resulting current is processed by a data handling system. Retention times for each eluting species are compared to known standards for species identification. Manganese Mn(IV) Analysis by ICP-QQQ-MS All samples submitted for Mn speciation quantitation were analyzed by inductively coupled plasma triple quadrupole mass spectrometry (ICP-QQQ-MS) on June 17, 2015. Aliquots of each sample digest are introduced into a radio frequency (RF) plasma where energy-transfer processes cause Page 18 of 36 desolvation, atomization, and ionization. The ions are extracted from the plasma through a differentially-pumped vacuum interface and travel through an initial quadrupole (Q1), which filters the target masses prior to their entrance into a second chamber. The second chamber contains specific reactive gasses or collision gasses that preferentially react either with interfering ions of the same target mass to charge ratios (m/z) or with the target analyte, producing an entirely different mass to charge ratio (m/z) which can then be differentiated from the initial interferences. The ions then exit the collision/reaction cell into and additional quadrupole (Q2). A solid-state detector detects ions transmitted through the mass analyzer, on the basis of their mass-to-charge ratio (m/z), and the resulting current is processed by a data handling system. 4. Analytical Issues No significant analytical issues were encountered. All quality control parameters associated with the samples were within acceptance limits. For Fe(II) analysis the client sample, identified as ABMW-2S, was analyzed as the quality control sample. The matrix spike (MS) spike recovery for Fe(II) was below the lower control limit of 75%, at 71.8%. The native Fe(II) concentration in the parent sample was greater than the spiking level. Acceptable spike recoveries are often not realized when the ambient level analyte concentration is greater than the spiking level. No qualification of data was necessary. Mn(IV) is quantified by analyzing the water samples for total Mn and dissolved Mn. Mn(IV) is operationally defined as the difference between the filtered and unfiltered total Mn concentrations, since it is thermodynamically favored to be in the form of a precipitate. The estimated method detection limit (eMDL) for hexavalent chromium is generated from replicate analyses of the lowest standard in the calibration curve. The eMDL values for selenite, selenate, and selenocyanate are generated from replicate analyses of the lowest standard in the calibration curve. Not all selenium species are present in preparation blanks; therefore, eMDL calculations based on preparation blanks are artificially biased low. The eMDL values for methylseleninic acid and selenomethionine are calculated from the average eMDL of selenite, selenate, and selenocyanate. The calibration does not contain methylseleninic acid or selenomethionine due to impurities in these standards which would bias the results for other selenium species. The eMDL values for arsenite, arsenate, and dimethylarsinic acid are generated using the standard deviation of replicate analyses of the lowest standard in the calibration curve. The eMDL for monomethylarsonic acid is calculated from the average eMDL of the three arsenic species contained in the calibration (i.e., arsenite, arsenate, and dimethylarsinic acid); the Page 19 of 36 calibration and CCVs do not contain monomethylarsonic acid due to impurities in this standard which would bias the results for other arsenic species. The eMDL values for iron speciation have been generated from replicate analyses of the lowest standard in the calibration curve. The eMDL for Mn(II) has been generated from replicate analyses of the lowest standard in the calibration curve. The eMDL values for Mn(IV) been calculated using the standard deviation of the method blanks prepared and analyzed concurrently with the submitted samples. If you have any questions or concerns regarding this report, please feel free to contact me. Sincerely, Jeremy Maute Project Manager Brooks Rand Labs, LLC Page 20 of 36 Sample Results (1) Sample ID Cr(VI)Se(IV)Se(VI)SeCN MeSe(IV)SeMe Unknown Se Species (n) AW-5D 0.023 ND (< 0.080)ND (< 0.065)ND (< 0.098)ND (< 0.081)ND (< 0.081)0 (0) SMW-6C 0.012 ND (< 0.080)ND (< 0.065)ND (< 0.098)ND (< 0.081)ND (< 0.081)0 (0) SMW-3C 0.012 ND (< 0.080)ND (< 0.065)ND (< 0.098)ND (< 0.081)ND (< 0.081)0 (0) SMW-3B 0.019 ND (< 0.080)ND (< 0.065)ND (< 0.098)ND (< 0.081)ND (< 0.081)0 (0) ABMW-1S 0.025 0.211 ND (< 0.065)0.251 ND (< 0.081)ND (< 0.081)0.160 (1) ABMW-2S 0.026 ND (< 0.080)ND (< 0.065)ND (< 0.098)ND (< 0.081)ND (< 0.081)0 (0) ABMW-2D 0.022 ND (< 0.080)ND (< 0.065)ND (< 0.098)ND (< 0.081)ND (< 0.081)0 (0) AW-9D 0.033 ND (< 0.080)ND (< 0.065)ND (< 0.098)ND (< 0.081)ND (< 0.081)0 (0) AW-9C 0.046 ND (< 0.080)0.190 ND (< 0.098)ND (< 0.081)ND (< 0.081)0 (0) AW-9B 0.038 ND (< 0.080)ND (< 0.065)ND (< 0.098)ND (< 0.081)ND (< 0.081)0 (0) All results reflect the applied dilution and are reported in µg/L ND = Not detected at the applied dilution SeCN = Selenocyanate MeSe(IV) = Methylseleninic acid SeMe = Selenomethionine Unknown Se Species = Total concentration of all unknown Se species observed by IC-ICP-MS n = number of unknown Se species observed Report Generated by: Jeremy Maute Brooks Rand Labs, LLC Speciation Results for Duke Energy Project Name: Duke Energy/Sutton Contact: Peggy Kendall Date: June 30, 2015 LIMS# J15060247 Page 21 of 36 Sample Results (2) Sample ID As(III)As(V)MMAs DMAs Unknown As Species AW-5D 0.293 0.204 0.150 0.078 ND (< 0.035) SMW-6C ND (< 0.062)ND (< 0.028)ND (< 0.035)ND (< 0.015)ND (< 0.035) SMW-3C 0.176 ND (< 0.028)ND (< 0.035)ND (< 0.015)ND (< 0.035) SMW-3B ND (< 0.062)ND (< 0.028)ND (< 0.035)ND (< 0.015)ND (< 0.035) ABMW-1S 157 2.40 ND (< 0.035)ND (< 0.015)ND (< 0.035) ABMW-2S 41.5 6.40 0.150 ND (< 0.015)ND (< 0.035) ABMW-2D 119 7.71 ND (< 0.035)ND (< 0.015)ND (< 0.035) AW-9D 0.326 ND (< 0.028)ND (< 0.035)ND (< 0.015)ND (< 0.035) AW-9C ND (< 0.062)ND (< 0.028)ND (< 0.035)ND (< 0.015)ND (< 0.035) AW-9B ND (< 0.062)ND (< 0.028)ND (< 0.035)ND (< 0.015)ND (< 0.035) All results reflect the applied dilution and are reported in µg/L ND = Not detected at the applied dilution MMAs = monomethylarsonic acid DMAs = dimethylarsinic acid Unknown As Species = Total concentration of all unknown As species observed by IC-ICP-MS Brooks Rand Labs, LLC Speciation Results for Duke Energy Project Name: Duke Energy/Sutton Contact: Peggy Kendall LIMS# J15060247 Date: June 30, 2015 Report Generated by: Jeremy Maute Page 22 of 36 Sample Results (3) Sample ID Fe(III)Fe(III)*Mn (II)Mn(IV)** AW-5D 29.2 ND (< 21)34.3 0.771 SMW-6C 1280 ND (< 8.4)254 ND (< 0.048) SMW-3C 1270 80 591 ND (< 0.048) SMW-3B 492 848 91.1 0.699 ABMW-1S 97.4 24.3 84.2 ND (< 0.048) ABMW-2S 25100 2400 825 38.1 ABMW-2D 940 230 146 ND (< 0.048) AW-9D 43.8 34.1 37.0 ND (< 0.048) AW-9C 9.7 ND (< 8.4)284 9.11 AW-9B 39.0 24.3 15.0 0.135 All results reflect the applied dilution and are reported in µg/L ND = Not detected at the applied dilution *Fe(III) defined as the difference between total recoverable Fe and Fe(II) **Mn(IV) operationally defined as the difference between total and dissolved Mn Brooks Rand Labs, LLC Speciation Results for Duke Energy Project Name: Duke Energy/Sutton Contact: Peggy Kendall LIMS# J15060247 Date: June 30, 2015 Report Generated by: Jeremy Maute Page 23 of 36 Quality Control Summary - Preparation Blank Summary (1) Analyte (µg/L)PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL*eMDL 5x RL 5x eMDL 50x RL 50x Cr(VI)0.033 0.017 0.013 0.013 0.019 0.010 0.001 0.007 0.050 -- Se(IV)0.000 0.000 0.000 0.000 0.000 0.000 0.002 --0.080 0.50 Se(VI)0.000 0.000 0.000 0.000 0.000 0.000 0.001 --0.065 0.50 SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.002 --0.098 0.46 MeSe(IV)0.000 0.000 0.000 0.000 0.000 0.000 0.002 --0.081 0.49 SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.002 --0.081 0.49 eMDL = Estimated Method Detection Limit; RL = Reporting Limit *Please see narrative regarding eMDL calculations Quality Control Summary - Preparation Blank Summary (2) Analyte (µg/L)PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL*eMDL 10x RL 10x As(III)0.000 0.000 0.000 0.000 0.000 0.000 0.006 0.062 0.20 As(V)0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.028 0.20 MMAs 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.035 0.20 DMAs 0.000 0.000 0.000 0.000 0.000 0.000 0.001 0.015 0.21 eMDL = Estimated Method Detection Limit; RL = Reporting Limit *Please see narrative regarding eMDL calculations Brooks Rand Labs, LLC Speciation Results for Duke Energy Project Name: Duke Energy/Sutton Contact: Peggy Kendall LIMS# J15060247 Date: June 30, 2015 Report Generated by: Jeremy Maute Page 24 of 36 Quality Control Summary - Preparation Blank Summary (3) Analyte (µg/L)PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL*eMDL 2x RL 2x eMDL 5x RL 5x Fe(II)-4.9 -2.4 -4.9 -2.4 -3.7 1.4 4.2 8.4 40 21 100 Total Fe 2.4 0.0 0.0 0.0 0.6 1.2 4.2 8.4 40 21 100 eMDL = Estimated Method Detection Limit; RL = Reporting Limit *Please see narrative regarding eMDL calculations Quality Control Summary - Preparation Blank Summary (3) Analyte (µg/L)eMDL*eMDL 100x RL 100x Fe(II)4.2 420 2000 Total Fe 4.2 420 2000 eMDL = Estimated Method Detection Limit; RL = Reporting Limit *Please see narrative regarding eMDL calculations Quality Control Summary - Preparation Blank Summary (3) Analyte (µg/L)PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL*eMDL 10x RL 10x eMDL 25x RL 25x Mn (II)-0.48 -0.62 -0.69 0.45 -0.59 0.53 0.086 0.86 5.0 -- Total Mn -0.161 -0.166 -0.176 -0.180 -0.168 0.009 0.001 --0.027 1.0 Diss Mn -0.085 -0.076 -0.103 -0.111 -0.088 0.016 0.002 --0.048 1.0 eMDL = Estimated Method Detection Limit; RL = Reporting Limit *Please see narrative regarding eMDL calculations Speciation Results for Duke Energy Brooks Rand Labs, LLC Project Name: Duke Energy/Sutton Contact: Peggy Kendall LIMS# J15060247 Date: June 30, 2015 Report Generated by: Jeremy Maute Page 25 of 36 Quality Control Summary - Certified Reference Materials (1) Analyte (µg/L)CRM True Value Result Recovery Cr(VI)LCS 2.002 1.781 89.0 Se(IV)LCS 10.00 10.03 100.3 Se(VI)LCS 10.00 10.32 103.2 SeCN LCS 8.92 8.821 98.9 MeSe(IV)LCS 6.47 6.709 103.7 SeMe LCS 9.32 9.547 102.4 Quality Control Summary - Certified Reference Materials (2) Analyte (µg/L)CRM True Value Result Recovery As(III)LCS 5.000 4.559 91.2 As(V)LCS 5.000 4.659 93.2 MMAs LCS 5.073 5.655 111.5 DMAs LCS 3.625 3.554 98.0 Report Generated by: Jeremy Maute Brooks Rand Labs, LLC Speciation Results for Duke Energy Project Name: Duke Energy/Sutton Contact: Peggy Kendall LIMS# J15060247 Date: June 30, 2015 Page 26 of 36 Quality Control Summary - Certified Reference Materials (3) Analyte (µg/L)CRM True Value Result Recovery Fe(II)ICV 100.0 92.5 92.5 Total Fe TMDA-70 368 355.4 96.6 Mn (II)LCS 1.00 1.053 105.3 Total Mn TMDA-70.2 312 302.2 96.9 Diss Mn TMDA-70.2 312 285.9 91.6 Report Generated by: Jeremy Maute Brooks Rand Labs, LLC Speciation Results for Duke Energy Project Name: Duke Energy/Sutton Contact: Peggy Kendall LIMS# J15060247 Date: June 30, 2015 Page 27 of 36 Quality Control Summary - Matrix Duplicates (1) Analyte (µg/L)Sample ID Rep 1 Rep 2 Mean RPD Cr(VI)Batch QC 0.020 0.023 0.022 14.3 Se(IV)AW-9B ND (< 0.080)ND (< 0.080)NC NC Se(VI)AW-9B ND (< 0.065)ND (< 0.065)NC NC SeCN AW-9B ND (< 0.098)ND (< 0.098)NC NC MeSe(IV)AW-9B ND (< 0.081)ND (< 0.081)NC NC SeMe AW-9B ND (< 0.081)ND (< 0.081)NC NC ND = Not detected at the applied dilution NC = Value was not calculated due to one or more concentrations below the eMDL Quality Control Summary - Matrix Duplicates (2) Analyte (µg/L)Sample ID Rep 1 Rep 2 Mean RPD As(III)SMW-3C 0.176 0.189 0.183 6.9 As(V)SMW-3C ND (< 0.028)ND (< 0.028)NC NC MMAs SMW-3C ND (< 0.035)ND (< 0.035)NC NC DMAs SMW-3C ND (< 0.015)ND (< 0.015)NC NC ND = Not detected at the applied dilution NC = Value was not calculated due to one or more concentrations below the eMDL Report Generated by: Jeremy Maute Brooks Rand Labs, LLC Speciation Results for Duke Energy Project Name: Duke Energy/Sutton Contact: Peggy Kendall LIMS# J15060247 Date: June 30, 2015 Page 28 of 36 Quality Control Summary - Matrix Duplicates (3) Analyte (µg/L)Sample ID Rep 1 Rep 2 Mean RPD Fe(II)ABMW-2S 25080 24340 24710 3.0 Total Fe Batch QC 15820 16800 16310 6.0 Mn (II)AW-5D 34.27 34.99 34.63 2.1 Total Mn Batch QC 304.3 296.4 300.3 2.6 Diss Mn Batch QC 309.5 312.5 311.0 0.9 ND = Not detected at the applied dilution NC = Value was not calculated due to one or more concentrations below the eMDL Report Generated by: Jeremy Maute Brooks Rand Labs, LLC Speciation Results for Duke Energy Project Name: Duke Energy/Sutton Contact: Peggy Kendall LIMS# J15060247 Date: June 30, 2015 Page 29 of 36 Quality Control Summary - Matrix Spike/ Matrix Spike Duplicate (1) Analyte (µg/L)Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPD Cr(VI)Batch QC 5.000 4.660 92.8 5.000 4.606 91.7 1.2 Se(IV)AW-9B 251.0 252.8 100.7 251.0 247.5 98.6 2.1 Se(VI)AW-9B 250.0 249.0 99.6 250.0 243.7 97.5 2.1 SeCN AW-9B 228.8 221.5 96.8 228.8 220.5 96.4 0.4 Quality Control Summary - Matrix Spike/ Matrix Spike Duplicate (2) Analyte (µg/L)Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPD As(III)SMW-3C 20.00 18.47 91.4 20.00 19.24 95.3 4.1 As(V)SMW-3C 20.00 18.29 91.5 20.00 18.41 92.1 0.7 DMAs SMW-3C 20.98 18.94 90.3 20.98 19.27 91.8 1.7 Quality Control Summary - Matrix Spike/ Matrix Spike Duplicate (3) Analyte (µg/L)Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPD Fe(II)ABMW-2S 10000 31890 71.8*10000 33839 91.3 5.9 Total Fe Batch QC 10000 26536 102.3 10000 27023 107.1 1.8 Mn (II)AW-5D 50.00 83.77 98.3 50.00 83.60 97.9 0.2 Total Mn Batch QC 1000 1238 93.8 1000 1283 98.2 3.5 Diss Mn Batch QC 1000 1288 97.7 1000 1232 92.1 4.4 *Ambient analyte concentration greater than spiking level. See case narrative. Report Generated by: Jeremy Maute Brooks Rand Labs, LLC Speciation Results for Duke Energy Project Name: Duke Energy/Sutton Contact: Peggy Kendall LIMS# J15060247 Date: June 30, 2015 Page 30 of 36 Page 31 of 36 Page 32 of 36 Page 33 of 36 Page 34 of 36 Page 35 of 36 Page 36 of 36