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NC0003433_J15060672F_20150902
+ DUKE Analytical Laboratory Page 1of31 ENERGY Order Number: Project Name: Customer Name(s): Customer Address: Lab Contact: Report Authorized By: (Signature) Program Comments: 13339 Hagers Ferry Road Huntersville, NC 28078-7929 McGuire Nuclear Complex - MG03A2 Phone:980-875-5245 Fax:980-875-4349 Order Summary Report J15060672 CAPE FEAR - AB GW ASSESSMENT SPECIATION Tim Hunsucker, Chris Suttell, Kathy Webb, John Toepfer Peggy Kendall p eggY• kendalQlne: uke-energy.com Date: 201-5.08.03 Peggy Kendall 13:29:39-04'00' Please contact the Program Manager (Peggy Kendall) with any questions regarding this report. Data Flags & Calculations: 8/3/2015 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. Sample ID's & Descriptions: Collection Sample ID Plant/Station Date and Time Collected By Sample Description 2015020258 Cape Fear 17-Jun-15 1:05 PM Kyle Donovan CTMW-8 2015020259 Cape Fear 17-Jun-15 4:28 PM Kyle Donovan CMW-1 2015020260 Cape Fear 17-Jun-15 3:40 PM Kyle Donovan CMW-8 2015020261 Cape Fear 17-Jun-15 9:50 AM Kyle Donovan MW-9BR 2015020262 Cape Fear 17-Jun-15 9:42 AM Kyle Donovan MW-10 2015020263 Cape Fear 17-Jun-15 10:36 AM Kyle Donovan MW-9 6 Total Samples Page 2 of 31 Page 3 of 31 Technical Validation Review Checklist: COC and .pdf report are in agreement with sample totals Yes No and analyses (compliance programs and procedures). All Results are less than the laboratory reporting limits. ❑ Yes❑ No All laboratory QA/QC requirements are acceptable.❑ Yes ❑ No Report Sections Included: U Job Summary Report ❑ Sample Identification n Technical Validation of Data Package ❑ Analytical Laboratory Certificate of Analysis ❑ Analytical Laboratory QC Report Sub -contracted Laboratory Results ❑ Customer Specific Data Sheets, Reports, & Documentation ❑ Customer Database Entries 66 Chain of Custody [I/0] Electronic Data Deliverable (EDD) Sent Separately Reviewed By: Peggy Kendall Date: 8/3/2015 Certificate of Laboratory Analysis Page 4 of 31 This report shall not be reproduced, except in full. Order # J15060672 Site: CTMW-8 Collection Date: 17-Jun-15 1:05 PM Analyte Result Units Qualifiers RDL DF Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Sample #: 2015020258 Matrix: GW WW Method Analysis Date/Time Analyst Vendor Method V_BRAND Certificate of Laboratory Analysis Page 5 of 31 This report shall not be reproduced, except in full. Order # J15060672 Site: CMW-1 Collection Date: 17-Jun-15 4:28 PM Analyte Result Units Qualifiers RDL DF Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Sample #: 2015020259 Matrix: GW WW Method Analysis Date/Time Analyst Vendor Method V_BRAND Certificate of Laboratory Analysis Page 6 of 31 This report shall not be reproduced, except in full. Order # J15060672 Site: CMW-8 Collection Date: 17-Jun-15 3:40 PM Analyte Result Units Qualifiers RDL DF Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Sample #: 2015020260 Matrix: GW WW Method Analysis Date/Time Analyst Vendor Method V_BRAND Certificate of Laboratory Analysis Page 7 of 31 This report shall not be reproduced, except in full. Order # J15060672 Site: MW-9BR Collection Date: 17-Jun-15 9:50 AM Analyte Result Units Qualifiers RDL DF Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Sample #: 2015020261 Matrix: GW WW Method Analysis Date/Time Analyst Vendor Method V_BRAND Certificate of Laboratory Analysis Page 8 of 31 This report shall not be reproduced, except in full. Order # J15060672 Site: MW-10 Collection Date: 17-Jun-15 9:42 AM Analyte Result Units Qualifiers RDL DF Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Sample #: 2015020262 Matrix: GW WW Method Analysis Date/Time Analyst Vendor Method V_BRAND Certificate of Laboratory Analysis This report shall not be reproduced, except in full. Order # J15060672 Site: MW-9 Collection Date: 17-Jun-15 10:36 AM Analyte Result Units Qualifiers RDL DF Speciation of an Element - (Analysis Performed by Brooks Rand Labs LLC) Vendor Parameter Complete Sample #: 2015020263 Matrix: GW WW Page 9 of 31 Method Analysis Date/Time Analyst Vendor Method V_BRAND Page 10 of 31 BRO�©KS RAND LABS MEANINGFUL METALS DATA July 31, 2015 Peggy Kendall Duke Energy Analytical Laboratory Mail Code MGO3A2 (Building 7405) 13339 Hagers Ferry Rd. Huntersville, NC 28078 (704) 875-5245 Project: Duke Energy Progress Cape Fear (LIMS# J15060672) Ms. Kendall, Attached is the report associated with six (6) aqueous samples submitted for hexavalent chromium, selenium speciation, arsenic speciation, iron speciation, and manganese speciation analyses on June 17, 2015. The samples were received in a sealed cooler at 0.2°C on June 18, 2015. Hexavalent chromium analysis was performed by ion chromatography inductively coupled plasma dynamic reaction cell mass spectrometry (IC-ICP-DRC-MS). 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) and arsenic speciation analyses were 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 3958 6th Ave NW • Seattle, WA 98107 • T: 206-632-6206 • F: 206-632-6017 • www.brooksrand.com • brl@brooksrand.com Page 11 of 31 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 Progress Cape Fear (LIMS# J15060672) July 31, 2015 1. Sample Reception Six (6) aqueous samples were submitted for hexavalent chromium, selenium speciation, arsenic speciation, iron speciation, and manganese speciation analyses on June 17, 2015. All samples were received in acceptable condition on June 18, 2015 in a sealed container at 0.2°C. The client instructed Brooks Rand Labs to cancel selenium speciation analyses for all client samples in this sampling event. The chain of custody form reflects selenium speciation as a target analyte; however, no selenium speciation results were reported in accordance with the client's instructions. 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 4°C, until the analyses could be performed. An aliquot of each sample submitted for arsenic speciation analysis was filtered (0.45µm) into a polypropylene centrifuge tube; all filtrates and original bottles were then stored in a secure, monitored refrigerator (maintained at a temperature of <6°C) 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 <6°C) 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 12 of 31 secure, monitored refrigerator (maintained at a temperature of <6°C) 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. 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 Spectrophotometrx 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(17 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). I 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 Page 13 of 31 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 23, 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. Arsenic Speciation Analysis by IC-ICP-CRC-MS Each sample was analyzed for arsenic speciation via ion chromatography inductively coupled plasma collision reaction cell mass spectrometry (IC-ICP-CRC-MS) on June 27-28, 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 samples submitted for Fe speciation quantification were analyzed for Fe(II) on June 18, 2015. The samples were analyzed for total recoverable iron on July 14, 2015. Iron speciation analysis was completed in accordance with the scientifically accepted method outlined by: Page 14 of 31 Stookey, L.L., (1970). "Ferrozine - A new spectrophotometric reagent for iron", Anal.Chem., 42:779-81. Manganese Mn�I 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 30, 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(II 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 July 16, 2015. Aliquots of each sample digest are 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 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 With the exceptions noted below, all quality control parameters associated with the samples were within acceptance limits. Mn(II) results for the client samples, MW-10 and MW-9, were inconsistent with the associated dissolved manganese results, which should be sampled from the same containers. Two containers were submitted for each client sample requesting manganese speciation, one field filtered fraction and one unfiltered fraction. An aliquot of each filtered sample submitted for manganese speciation analysis is decanted into a polypropylene centrifuge tube Page 15 of 31 for Mn(II) analysis. The Mn(II) fractions for samples MW-10 and MW-9 appeared to be swapped; the Mn(II) fractions were analyzed for total manganese for confirmation. An analysis of the total metals results for several analytes was conducted and these results were directly compared to dissolved metals results. The component analysis revealed that these two Mn(II) fractions, MW-10 and MW-9, were mislabeled and were likely swapped at sample reception when the Mn(II) fractions were decanted into new vessels for subsequent Mn(II) analysis. Since Brooks Rand Labs is confident that the sample containers were mislabeled, Mn(II) results for the client samples MW-10 and MW-9 were corrected to account for the confirmed sample ID discrepancy. The raw instrument data indicates Mn(II) results of 556 µg/L (sample MW-10) and 13400 µg/L sample MW-9). Whereas in this report Mn(II) results of 13400 µg/L (sample MW-10) and 556 µg/L (sample MW-9) are used. For Mn(II) analysis the client sample, identified as CMW-8, was analyzed as the quality control sample. Mn(II) results were greater than the value of the associated high calibration standard. A linear range verification standard was analyzed at 2000 µg/L. The Mn(II) recovery for the linear range verification standard was acceptable, at 105.1 %, demonstrating that the linear range of the analytical platform extended to 2000 µg/L for Mn(II). All reported Mn(II) results were less than 2000 µg/L with the dilutions at the instrument factored in, and thus were within the linear range demonstrated by the linear range verification standard. No corrective actions were necessary and no qualification of data was necessary. The matrix spike duplicate sample (MSD) spike recovery for Mn(II) was below the lower control limit of 75%, at 62.1%. The native Mn(II) concentration in the quality control sample was significantly 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. Total and dissolved manganese results for the client samples, identified as CMW-8 and MW-10, were greater than the value of the associated high calibration standard. A linear range verification standard was analyzed at 2000 µg/L. The manganese recovery for the linear range verification standard was acceptable, at 100.0%, demonstrating that the linear range of the analytical platform extended to 2000 µg/L for manganese. Total and dissolved manganese results for CMW-8 and MW-10 were less than 2000 µg/L with the dilutions at the instrument factored in, and thus were within the linear range demonstrated by the linear range verification standard. No corrective actions were necessary and no qualification of data was necessary. The estimated method detection limit (eMDL) for hexavalent chromium is generated from replicate analyses of the lowest standard in the calibration curve. Page 16 of 31 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 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 Fe(II) and total recoverable Fe were set at 5 based on the sensitivity of the instrument. 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 17 of 31 Speciation Results for Duke Energy Project Name: Duke Energy Progress Cape Fear Contact: Peggy Kendall LIMS# J15060672 Date: July 31, 2015 Report Generated by: Jeremy Maute Brooks Rand Labs, LLC Sample Results (1 Sample ID Cr(VI) CTMW-8 ND (< 0.005) CMW-1 ND (< 0.005) CMW-8 ND (< 0.005) MW-9BR ND (< 0.005) MW-10 0.007 MW-9 0.014 All results reflect the applied dilution and are reported in pg/L ND = Not detected at the applied dilution Page 18 of 31 Speciation Results for Duke Energy Project Name: Duke Energy Progress Cape Fear Contact: Peggy Kendall LIMS# J15060672 Date: July 31, 2015 Report Generated by: Jeremy Maute Brooks Rand Labs, LLC Sample Results (2) Unknown As Sample ID As(III) As(V) MMAs DMAs Species CTMW-8 3.67 1.42 ND (<0.053) ND (<0.083) ND (<0.053) CMW-1 0.604 0.077 ND (<0.053) ND (<0.083) ND (<0.053) CMW-8 0.201 ND (<0.028) ND (<0.053) ND (<0.083) ND (<0.053) MW-9BR 0.070 ND (<0.028) ND (<0.053) ND (<0.083) ND (<0.053) MW-10 0.071 ND (<0.028) ND (<0.053) ND (<0.083) ND (<0.053) MW-9 0.102 0.055 ND (<0.053) ND (<0.083) ND (<0.053) All results reflect the applied dilution and are reported in Ng/L MMAs = monomethylarsonic acid DMAs = dimethylarsinic acid Unknown As Species = Total concentration of all unknown As species observed by IC-ICP-MS Page 19 of 31 Speciation Results for Duke Energy Project Name: Duke Energy Progress Cape Fear Contact: Peggy Kendall LIMS# J15060672 Date: July 31, 2015 Report Generated by: Jeremy Maute Brooks Rand Labs, LLC Sample Results (3 Sample ID Fe(II) Fe(III)* Mn (II) Mn(IV)** CTMW-8 7620 ND (<500) 1270 ND (<0.19) CMW-1 52600 ND (<500) 1170 ND (<0.19) CMW-8 34000 1000 12000 ND (<0.19) MW-9BR 431 ND (<5.0) 908 ND (<0.19) MW-10 771 ND (<5.0) 13400 ND (<0.19) MW-9 376 26.3 556 ND (<0.19) All results reflect the applied dilution and are reported in pg/L ND = Not detected at the applied dilution *Fe(III) operationally defined as the difference between total recoverable Fe and Fe(II) *Mn(IV) operationally defined as the difference between total and dissolved Mn Page 20 of 31 Speciation Results for Duke Energy Project Name: Duke Energy Progress Cape Fear Contact: Peggy Kendall LIMS# J15060672 Date: July 31, 2015 Report Generated by: Jeremy Maute Brooks Rand Labs, LLC Quality Control Summary - Preparation Blank Summary (1) Analyte (Ng/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 5x RL 5x Cr(VI) 0.004 0.000 0.001 -0.001 0.001 0.002 0.001 0.005 0.050 eMDL = Estimated Method Detection Limit; RL = Reporting Limit *Please see narrative regarding eMDL calculations Quality Control Summary - Preparation Blank Summary (2) Analyte (Ng/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 0.005 0.049 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 0.005 0.053 0.20 DMAs 0.000 0.000 0.000 0.000 0.000 0.000 0.008 0.083 0.21 eMDL = Estimated Method Detection Limit; RL = Reporting Limit *Please see narrative regarding eMDL calculations Page 21 of 31 Speciation Results for Duke Energy Project Name: Duke Energy Progress Cape Fear Contact: Peggy Kendall LIMS# J15060672 Date: July 31, 2015 Report Generated by: Jeremy Maute Brooks Rand Labs, LLC Quality Control Summary - Preparation Blank Summary (3) Analyte (lag/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL** eMDL 1x RL 1x eMDL 100x RL 100x Fe(I1) 0.0 0.0 0.0 0.0 0.0 0.0 5.0 5.0 20 500 2000 Total Fe 0.0 0.0 0.0 0.0 0.0 0.0 5.0 5.0 20 500 2000 eMDL = Estimated Method Detection Limit; RL = Reporting Limit **Please see narrative regarding eMDL calculations Quality Control Summary - Preparation Blank Summary (3) Analyte (lag/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 100x RL 100x eMDL 25x RL 25x Mn (II) -0.29 -0.25 -0.28 -0.30 -0.27 0.02 0.026 2.6 50 - - Total Mn -0.63 -0.74 -0.74 -0.77 -0.70 0.06 0.008 - - 0.19 1.0 Diss Mn -0.774 -0.826 -0.824 -0.805 -0.808 0.024 0.003 - - 0.072 1.0 eMDL = Estimated Method Detection Limit; RL = Reporting Limit *Please see narrative regarding eMDL calculations Page 22 of 31 Speciation Results for Duke Energy Project Name: Duke Energy Progress Cape Fear Contact: Peggy Kendall LIMS# J15060672 Date: July 31, 2015 Report Generated by: Jeremy Maute Brooks Rand Labs, LLC Quality Control Summary - Certified Reference Materials (1 Analyte (lag/L) CRM True Value Result Recovery Cr(VI) LCS 2.002 1.967 98.2 Quality Control Summary - Certified Reference Materials (2) Analyte (lag/L) CRM True Value Result Recovery As(III) LCS 5.00 5.04 100.9 As(V) LCS 5.00 4.58 91.6 MMAs LCS 5.07 5.73 113.0 DMAs LCS 3.63 3.51 96.8 Quality Control Summary - Certified Reference Materials (3) Analyte (lag/L) CRM True Value Result Recovery Fe(II) ICV 500.0 514.3 102.9 Total Fe TMDA-70 369 402.5 109.1 Mn (II) LCS 10.00 10.26 102.6 Total Mn TMDA-70.2 312 310.2 99.4 Diss Mn TMDA-70.2 312 302.6 97.0 Page 23 of 31 Speciation Results for Duke Energy Project Name: Duke Energy Progress Cape Fear Contact: Peggy Kendall LIMS# J15060672 Date: July 31, 2015 Report Generated by: Jeremy Maute Brooks Rand Labs, LLC Quality Control Summary - Matrix Duplicates (1) Analyte (pg/L) Sample ID Rep 1 Rep 2 Mean RPD 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 (pg/L) Sample ID Rep 1 Rep 2 Mean RPD As(III) Batch QC 0.135 0.075 0.105 56.9* As(V) Batch QC ND (<0.028) ND (<0.028) NC NC MMAs Batch QC ND (<0.053) ND (<0.053) NC NC DMAs Batch QC ND (<0.083) ND (<0.083) NC NC ND = Not detected at the applied dilution NC = Value was not calculated due to one or more concentrations below the eMDL *Results associated with RPD outlier are less than the reporting limit. Page 24 of 31 Speciation Results for Duke Energy Project Name: Duke Energy Progress Cape Fear Contact: Peggy Kendall LIMS# J15060672 Date: July 31, 2015 Report Generated by: Jeremy Maute Brooks Rand Labs, LLC Qualitv Control Summary - Matrix Duplicates (3 Analyte (pg/L) Sample ID Rep 1 Rep 2 Mean RPD Fe(II) Batch QC 185.7 195.2 190.5 5.0 Total Fe Batch QC 177.4 177.4 177.4 0.0 Mn (II) CMW-8 12040 12200 12120 1.3 Total Mn MW-9 518.4 510.1 514.3 1.6 Diss Mn MW-9 615.0 600.7 607.8 2.4 ND = Not detected at the applied dilution NC = Value was not calculated due to one or more concentrations below the eMDL Page 25 of 31 Speciation Results for Duke Energy Project Name: Duke Energy Progress Cape Fear Contact: Peggy Kendall LIMS# J15060672 Date: July 31, 2015 Report Generated by: Jeremy Maute Brooks Rand Labs, LLC Qualitv Control Summary - Matrix Spike/Matrix Spike Duplicate 0 Analyte (lag/L) Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPD Cr(VI) MW-9 5.000 4.582 91.4 5.000 4.706 93.9 2.7 Qualitv Control Summary - Matrix Spike/Matrix Spike Duplicate (2) Analyte (lag/L) Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPD As(III) As(V) DMAs Batch QC Batch QC Batch QC 20.00 20.00 20.98 18.53 18.22 18.31 92.1 91.1 87.3 20.00 20.00 20.98 18.34 18.71 17.58 91.2 93.5 83.8 1.1 2.7 4.1 Quality Control Summary - Matrix Spike/Matrix Spike Duplicate (3) Analyte (lag/L) Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPD Fe(II) Total Fe Batch QC Batch QC 500.0 500.0 714.3 650.3 104.8 94.6 500.0 500.0 721.4 659.4 106.2 96.4 1.0 1.4 Mn (II) Total Mn Diss Mn CMW-8 MW-9 MW-9 500.0 1000 1000 12630 1503 1389 102.0* 98.9 78.1 500.0 1000 1000 12430 1584 1668 62.1* 106.9 106.0 0.8 5.2 18.3 *Ambient analyte concentration greater than spiking level. See case narrative 0 U y H N 0 0 6J co C O 0 00 C U ® m d N �°,- 0 0 -t ®` yNj •O � d cn O � •• Q U � O N y z 0u; °z CC o o o o c� o Uu Li 4. .. a 0 O 0 fA _ cry _ m d N = c c c Q Z N p p o 0 2 A Z Z Z 0 Z Z Z Z � Z o j rr6 rF a ( � tvr` c J' N` M f,,, rr• .vim � � � � 00 L� ti `®l ij N ai ii u > Q U � cz Q O C J Page aB of 31 0 W � T 00 N W Y c C O C v -0 M 00 c u y m m m m o o C u ® jD C N 0 y O g cto y N •O � d v cd w o Y u O .U, y 9 0 � C Fcd a d 00 O cpa cd N D d p q O c 0 °° Ct1 abo . cn o Q) O d C C QIV u-I2I2Icn IQIUI�I�I�I11) � 6J7 ; a�i v p a ~ m 5 U U il v, rlN � J u C Z a �o ob x���o _ c c c S 0 Z Z Z � w Z. � N tc w U a :)R- 1` P Qom-• w � 1 In Su -6 r c cl) .,q z- p CIO- �_nnCC��� c M 1 ,1 4 '1' 1 -Z 3�333� Page 17 of 31 r u & P ge28of3 ca C O O V w 3 w w w c0 ;c-� 7 ;(D ca y C •. c�1 r (d 0 00 0 V� x v v E a E a v v Q 3 E E E E O v v U (D U U ca ^� -C cc U d) Q 0V C CQw u0 N o A N •-J N I Q N ^ N 0) N G� (n fn (n (n (� U)fn CO U) X �^ C G ° u M Q rn C U aD LL C c (D U)Q U) U ti c c y U) O O v C� Q.-C �o c � E o o h i+ V o 3.a o z cd W CL V > ! V CL � Cf' t+ O 0 C 7 ZVa C o v � w cc'' c 3 x x CU U p L C) C)2 2 Q dl C c c Q Z c c c .S v p T. �'Z Z Z p � 2 Z Z i E m Q% (n r,6 ro � G V^ ca 1V 1 0 N J � C a C a o L U .6 R 9 �� ^ n n d C0- cm v Im 0 . in- T T z Z z to -0 N _0 0 18804 Northcreek Parkway Phone (425) 483-3300Fix t o ?) Bothell, WA 98011 Maute agrees to all terms an — ...........x.,..+.•� By submitting of samples the client If you are not familiar NacrK: in the quotation provided by the BRI, project manager• (.�+ `b "> `' ` 9 conditions associated with your Protect, please contact your Pets ' ; .:-%V Ile with the term and kddrm: '' 1'� t �° ' ? BRL re resentative as soon as ssible 42- 483-3300. s ^� Re uested Turn Aroma Tom- phadx Nurnbec � 7 - Method of le Deity Fssc Number. . t ` Con--;--,'rac Number: L arum +a le R don: Ij iC3 ® NO � � � ConE,rmadon of Same �eP Nsr+se Comments Nt> 1217608 Iniitisls Re nested sand Methods N Matrix Vohune Preservative AS S field filtered Bottle ID Date and 1"tme EDTA -1 f�' 't` ' 3 o�J.�� '7 9 field filtered ID Cr 1 NH40HMH4SO4 Fe S field fettered ssed HCl Mn S field filtered e None unflltered Ti 5s' U `17 Mn S C w ` c None Se S field Filtered None 7Y As S field filtered EDT - Cr VI field filtered C.. w - NH40HINH4SO4 Fe S field filtered a t assed HCI Mn S c field filtered ' A - 11 s None Mn S ec unfiltered -R Uy' - j r +1 LA./- [ ► ; None Se S field filtered None Cornrnwts: Dater ime:=_______— Relinquished by: (sign) I� DateRime: t 7emp: (print) � Comments: Received W (sign) Date/Time:_— (print) Temp: Relinquished by: (sign) Date/I ime:_ _--___-- (print) Received b : (sign) purposes. ►e bottle as a se rate line item`f t`veant�ea(Ww)' soil (SI,), sediment (;;D), tissue (l�), product p'), other (0) Pe Please account for each camp groundwater (GW), Air, Freshwater WW), seawater ($V�, fir - Matru: Rcv i.t (Apt �5) 0 C- .onV iy Name: :ontact Person: Wdttss: 'hone Number ` .4 7 as Number - Email Address: Proiect Narne: PO Numb — Sam le �1 w -y6R ,MW-9FSR Myr/ -j134 raw .q 5k 1X' 18804� ck Parkway Phone (40§�4M �f3W Bothell, WA 98011 Fix (425) 483-9818 BRL Pro ect nnan to all terms and conditions set forth By submitting of samples the client agrees by the BRL project manager. If you are not familiar _ - L/ • in the quotation provided please contact your the term and conditions associated ble 425 483f 3300ect, with BRL re resentative ass( as L-`sir �i uested'I'um Around Time: Method of SanVLc Delivc courier -rracking Number.13 11w Yes :e- rx_-- Confirmation of Sample Reception: � 1217608 I>utials Re uested tes and Methods Comments J Bottle ID Date d Time Matrix an Volume Preservative EDTA -1 i K As S field ftttered field filtered t N1i40HINH4SO4 C field filtered Fe S c HCI t Mn S field filtered None Mn S unflite, None field fettered (? , Y{ None Se S c Se As S field filtered CsW !i' EDTA -1 12 K c C, I field filtered t'y1:t.77 r' NH40H/NH4SO4 field filtered De assed HCI Fe S field filtered None Mn S unfiltered None field filtered i = Se S None Dateffirne: Relinquished by: (sign) Date/Time: - c.� (print) Received by: (sign) Date/Time:___.--- Relinquished by: (sign) (print) Dateffime: (print) Received b : (sign) Please account Eor each sample bottle as a seperatc line itetn for veti6ca(w t?'rrP SiCS sediment (St)), tissue (I S}, product (�, otl'u (0) •Matrix: Air, Freshwater OINAO, seawater W, groundwater ((;W ,wastewater ( ) 0.ZC_ Rev 1.1 (April 2005) Page 31 of 31 str'!?4 Nor-hcil i is P:. .w, v Phone 4103-3300 Com un Name: BRL Project Rianr. _Icrcmy Maute Contact Person: t-, By submitting of samples the client agrees to all terms and conditions set forth in the quotation provided%y the BRL project manager. If you are not familiar with the term and conditions associated with your project, please contact your BRL representative as soon as possible 425 483-3300. Address: I4' �+ 1= S , , �. r. . � �, Phone Number: `- - ?" 1 1'ax Nwnixr Requested `I'um Around Time: limail Address: Method of Sample Delivery: Protect Name: - s ,' < ¢ cs Courier Tra Number - Project Number: i `�' Confr*mation of Sample Reception: Y� 13 No _ PO Numf,er: 1217608 gam k ID,/ 4Ap,Jg 'Z Bottle ID Date and Time Maw* Volume Preservative Initials Requested Anal tes and Methods Comments '2 ED fA -1 -- -! As :spec field Atered NH401-1/1:114SO4 C (VV field filtered L Degassed HCI ! Fe Spec Mn Spec field filtered field filtered w t o _ None M " / L' ' None Mn Spec unfiltered -� I C None Se Sp2c field filtered - ,h I I,v > t a5' r, t EDTA - 1 As Spec field filtered t3 r NH40H/NH4SO4 Cr VI field filtered (A,' 7 Dagassed HCl Fe Spec feld filtered None Mn Sper- field filtered I None None Mn Spec Se Spec Ifield unfiltered filtered _ Relinquished by (sign) (print) . =-r)ovc. Date(Tinte:! s'//S Comments: Received by: (sign) _ _ (print) 6zJU Vwtal 6+6, Daterrime % t t t it e,0 Temp: 2- Comments: Relinquished by (sign) (print) Datelrime: Received by (sign) (print) DateJTime Temp: Please account for each sample bottle as a seperate line item for verification purposes. Matrix: Air, Preshwa►er (hl�, seawater (S%), groundwater ((.Vt7, wastewater (\XNV), soil (Sl.), sediment (SD;: tissue (I'S), product (13), other (0) Rev 1.1 ( April ZIM)