13339 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: J13020369

Project Name: WWTS - Biweekly (2)

Lab Contact: Jason C Perkins

Date: 3/26/2013

Customer Address: 3195 Pine Hall Rd

Customer Name(s): Bill Kennedy, Melonie Martin, Wayne Chapman, Travis Thornton

Mailcode: Belews Steam Station

Belews Creek, NC 28012

Phone: 980-875-5348

Report Authorized By:

(Signature)

Program Comments:

Please contact the Program Manager (Jason C Perkins) 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. 

Jason C Perkins

Page 1 of 16
Sample ID's & Descriptions:

Sample ID Plant/Station

Collection 

Date and Time Collected By Sample Description

2013004289 BELEWS 27-Feb-13 7:30 AM TO FGD Purge Eff 

2013004290 BELEWS 27-Feb-13 7:30 AM TO EQ TANK EFF. 

2013004291 BELEWS 27-Feb-13 7:30 AM TO BIOREACTOR 1 INF. 

2013004292 BELEWS 27-Feb-13 7:30 AM TO BIOREACTOR 2 INF. 

2013004293 BELEWS 27-Feb-13 7:30 AM TO BIOREACTOR 2 EFF. 

2013004294 BELEWS 27-Feb-13 7:30 AM TO FILTER BLANK 

2013004295 BELEWS 27-Feb-13 7:30 AM TO Trip Blank 

7 Total Samples

Page 2 of 16
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: DBA Account Date: 3/26/2013

Electronic Data Deliverable (EDD) Sent Separately

The following vendor labs are Pending Qualifi Applied Speciation

Page 3 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13020369

2013004289

Collection Date: 27-Feb-13 7:30 AM

Site: FGD Purge Eff 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 110 mg/L 5 50 EPA 300.0 03/15/2013 21:36 BGN9034

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 282 ug/L 5 100 EPA 245.1 03/07/2013 14:17 AGIBBS

DISSOLVED METALS BY ICP

Manganese (Mn) 9.35 mg/L 0.05 10 EPA 200.7 03/18/2013 15:15 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 205 mg/L 0.5 10 EPA 200.7 03/12/2013 11:22 MHH7131

Manganese (Mn) 10.9 mg/L 0.05 10 EPA 200.7 03/12/2013 11:22 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 410 ug/L 10 10 EPA 200.8 03/20/2013 12:51 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 350 ug/L 10 10 EPA 200.8 03/08/2013 15:16 KRICHAR

Chromium (Cr) 300 ug/L 10 10 EPA 200.8 03/08/2013 15:16 KRICHAR

Copper (Cu) 171 ug/L 10 10 EPA 200.8 03/08/2013 15:16 KRICHAR

Nickel (Ni) 252 ug/L 10 10 EPA 200.8 03/08/2013 15:16 KRICHAR

Selenium (Se) 4630 ug/L 10 10 EPA 200.8 03/08/2013 15:16 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 03/08/2013 15:16 KRICHAR

Zinc (Zn) 305 ug/L 10 10 EPA 200.8 03/08/2013 15:16 KRICHAR

SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC)

Vendor Parameter Complete Vendor Method V_AS&C

TOTAL DISSOLVED SOLIDS

TDS 19000 mg/L 200 1 SM2540C 03/05/2013 15:35 SWILLI3

2013004290

Collection Date: 27-Feb-13 7:30 AM

Site: EQ TANK EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) 169 ug/L 2.5 50 EPA 245.1 03/07/2013 14:19 AGIBBS

DISSOLVED METALS BY ICP

Manganese (Mn) 9.02 mg/L 0.05 10 EPA 200.7 03/18/2013 15:19 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 212 mg/L 0.5 10 EPA 200.7 03/12/2013 11:26 MHH7131

Manganese (Mn) 9.85 mg/L 0.05 10 EPA 200.7 03/12/2013 11:26 MHH7131

Page 4 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13020369

2013004290

Collection Date: 27-Feb-13 7:30 AM

Site: EQ TANK EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

DISSOLVED METALS BY ICP-MS

Selenium (Se) 247 ug/L 10 10 EPA 200.8 03/20/2013 12:54 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) 242 ug/L 10 10 EPA 200.8 03/08/2013 15:20 KRICHAR

Chromium (Cr) 216 ug/L 10 10 EPA 200.8 03/08/2013 15:20 KRICHAR

Copper (Cu) 127 ug/L 10 10 EPA 200.8 03/08/2013 15:20 KRICHAR

Nickel (Ni) 202 ug/L 10 10 EPA 200.8 03/08/2013 15:20 KRICHAR

Selenium (Se) 3310 ug/L 10 10 EPA 200.8 03/08/2013 15:20 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 03/08/2013 15:20 KRICHAR

Zinc (Zn) 227 ug/L 10 10 EPA 200.8 03/08/2013 15:20 KRICHAR

2013004291

Collection Date: 27-Feb-13 7:30 AM

Site: BIOREACTOR 1 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

DISSOLVED METALS BY ICP

Manganese (Mn) 3.44 mg/L 0.05 10 EPA 200.7 03/18/2013 15:23 MHH7131

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 210 mg/L 0.5 10 EPA 200.7 03/12/2013 11:30 MHH7131

Manganese (Mn) 4.97 mg/L 0.05 10 EPA 200.7 03/12/2013 11:30 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) 95.3 ug/L 10 10 EPA 200.8 03/20/2013 12:57 DJSULL1

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 03/08/2013 15:23 KRICHAR

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 03/08/2013 15:23 KRICHAR

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 03/08/2013 15:23 KRICHAR

Nickel (Ni) 40.4 ug/L 10 10 EPA 200.8 03/08/2013 15:23 KRICHAR

Selenium (Se) 114 ug/L 10 10 EPA 200.8 03/08/2013 15:23 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 03/08/2013 15:23 KRICHAR

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 03/08/2013 15:23 KRICHAR

SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC)

Vendor Parameter Complete Vendor Method V_AS&C

Page 5 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13020369

2013004292

Collection Date: 27-Feb-13 7:30 AM

Site: BIOREACTOR 2 INF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 217 mg/L 0.5 10 EPA 200.7 03/12/2013 11:34 MHH7131

Manganese (Mn) 4.97 mg/L 0.05 10 EPA 200.7 03/12/2013 11:34 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 10 ug/L 10 10 EPA 200.8 03/08/2013 15:27 KRICHAR

Chromium (Cr) < 10 ug/L 10 10 EPA 200.8 03/08/2013 15:27 KRICHAR

Copper (Cu) < 10 ug/L 10 10 EPA 200.8 03/08/2013 15:27 KRICHAR

Nickel (Ni) 12.9 ug/L 10 10 EPA 200.8 03/08/2013 15:27 KRICHAR

Selenium (Se) 12.0 ug/L 10 10 EPA 200.8 03/08/2013 15:27 KRICHAR

Silver (Ag) < 10 ug/L 10 10 EPA 200.8 03/08/2013 15:27 KRICHAR

Zinc (Zn) < 10 ug/L 10 10 EPA 200.8 03/08/2013 15:27 KRICHAR

2013004293

Collection Date: 27-Feb-13 7:30 AM

Site: BIOREACTOR 2 EFF. 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

INORGANIC IONS BY IC

Bromide 120 mg/L 5 50 EPA 300.0 03/15/2013 21:55 BGN9034

MERCURY (COLD VAPOR) IN WATER

Mercury (Hg) < 1 ug/L 1 20 EPA 245.1 03/07/2013 14:21 AGIBBS

TOTAL RECOVERABLE METALS BY ICP

Boron (B) 236 mg/L 0.5 10 EPA 200.7 03/12/2013 11:38 MHH7131

Manganese (Mn) 5.01 mg/L 0.05 10 EPA 200.7 03/12/2013 11:38 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 5 ug/L 5 5 EPA 200.8 03/08/2013 15:30 KRICHAR

Chromium (Cr) < 5 ug/L 5 5 EPA 200.8 03/08/2013 15:30 KRICHAR

Copper (Cu) < 5 ug/L 5 5 EPA 200.8 03/08/2013 15:30 KRICHAR

Nickel (Ni) < 5 ug/L 5 5 EPA 200.8 03/08/2013 15:30 KRICHAR

Selenium (Se) < 5 ug/L 5 5 EPA 200.8 03/08/2013 15:30 KRICHAR

Silver (Ag) < 5 ug/L 5 5 EPA 200.8 03/08/2013 15:30 KRICHAR

Zinc (Zn) < 5 ug/L 5 5 EPA 200.8 03/08/2013 15:30 KRICHAR

SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC)

Vendor Parameter Complete Vendor Method V_AS&C

Page 6 of 16
Certificate of Laboratory Analysis

This report shall not be reproduced, except in full.

Order # J13020369

2013004294

Collection Date: 27-Feb-13 7:30 AM

Site: FILTER BLANK 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

DISSOLVED METALS BY ICP

Manganese (Mn) 0.023 mg/L 0.005 1 EPA 200.7 03/18/2013 15:07 MHH7131

DISSOLVED METALS BY ICP-MS

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 03/20/2013 12:44 DJSULL1

2013004295

Collection Date: 27-Feb-13 7:30 AM

Site: Trip Blank 

Matrix: OTHER

Analyte Result Units Qualifiers RDL Method Analysis Date/Time

Sample #:

DF Analyst

TOTAL RECOVERABLE METALS BY ICP

Boron (B) < 0.05 mg/L 0.05 1 EPA 200.7 03/12/2013 11:18 MHH7131

Manganese (Mn) < 0.005 mg/L 0.005 1 EPA 200.7 03/12/2013 11:18 MHH7131

TOTAL RECOVERABLE METALS BY ICP-MS

Arsenic (As) < 1 ug/L 1 1 EPA 200.8 03/08/2013 15:13 KRICHAR

Chromium (Cr) < 1 ug/L 1 1 EPA 200.8 03/08/2013 15:13 KRICHAR

Copper (Cu) < 1 ug/L 1 1 EPA 200.8 03/08/2013 15:13 KRICHAR

Nickel (Ni) < 1 ug/L 1 1 EPA 200.8 03/08/2013 15:13 KRICHAR

Selenium (Se) < 1 ug/L 1 1 EPA 200.8 03/08/2013 15:13 KRICHAR

Silver (Ag) < 1 ug/L 1 1 EPA 200.8 03/08/2013 15:13 KRICHAR

Zinc (Zn) < 2 ug/L 2 1 EPA 200.8 03/08/2013 15:13 KRICHAR

SELENIUM SPECIATION - (Analysis Performed by Applied Speciation and Consulting, LLC)

Vendor Parameter Complete Vendor Method V_AS&C

Page 7 of 16
 

March 8, 2013 

Jay Perkins 

Duke Energy Analytical Laboratory 

Mail Code MGO3A2 (Building 7405) 

13339 Hagers Ferry Rd. 

Huntersville, NC 28078 

(704) 875-5245 

Project: Belews - FGD WWTS Bi-Monthly Sampling) (LIMS #J13020369) 

Dear Mr. Perkins, 

Attached is the report associated with four (4) aqueous samples submitted for selenium 

speciation on February 28, 2013. The samples were received in a sealed cooler at 1.7°C on 

March 1, 2013. Selenium speciation analysis was performed via ion chromatography inductively 

coupled plasma collision reaction cell mass spectrometry (IC-ICP-CRC-MS). Any issues 

associated with the analysis are addressed in the following report. 

If you have any questions, please feel free to contact me at your convenience. 

 Sincerely, 

 

 Russell Gerads 

Vice President 

Applied Speciation and Consulting, LLC 

 

 

Page 8 of 16
Applied Speciation and Consulting, LLC 

Report prepared for: 

Jay Perkins 

Duke Energy Analytical Laboratory 

Mail Code MGO3A2 (Building 7405) 

13339 Hagers Ferry Rd. 

Huntersville, NC 28078 

Project: Belews - FGD WWTS Bi-Monthly Sampling) (LIMS #J13020369) 

March 8, 2013 

1. Sample Reception 

Four (4) aqueous samples in 125mL HDPE bottles (provided by Applied Speciation and 

Consulting) were submitted for selenium speciation analysis on February 28, 2013. The 

samples were received on March 1, 2013 in a sealed container at 1.7°C.

The samples were received in a laminar flow clean hood, void of trace metals contamination 

and ultra-violet radiation, and were designated discrete sample identifiers. An aliquot of 

each sample was filtered (0.45μm) and each filtrate was stored in a secure, monitored 

cryofreezer (maintained at a temperature of -80oC) until selenium speciation analysis could 

be performed via ion chromatography inductively coupled plasma collision reaction cell 

mass spectrometry (IC-ICP-CRC-MS). 

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. 

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 an 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. 

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 

Page 9 of 16
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. 

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 March 7, 2013. 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. 

4. Analytical Issues 

The overall analyses went well and no significant analytical issues were encountered. All 

quality control parameters associated with the samples were within acceptance limits. 

The estimated method detection limits (eMDLs) 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 for methylseleninic acid and selenomethionine is 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. 

Page 10 of 16
If you have any questions or concerns regarding this report, please feel free to contact me. 

Sincerely, 

Russell Gerads 

Vice President 

Applied Speciation and Consulting, LLC 

Page 11 of 16
Sample Results

Sample ID Se(IV) Se(VI) SeCN MeSe(IV) SeMe

Unknown Se 

Species (n)

FGD Purge Eff 330 79.1 ND (<2.6) 8.2 ND (<4.1) 0.0 (0)

BioReactor 1 Inf 24.5 62.8 ND (<0.65) 5.5 ND (<1.0) 10.4 (1)

BioReactor 2 Eff ND (<1.7) ND (<0.73) ND (<0.65) ND (<1.0) ND (<1.0) 0.0 (0)

Metals Trip Blk 0.162 0.043 ND (<0.026) ND (<0.041) ND (<0.041) 0.0 (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

Report Generated by: Russell Gerads

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins

Date: March 8, 2013

LIMS #J13020369

Page 12 of 16
Quality Control Summary - Preparation Blank Summary

Analyte (μg/L) PBW1 PBW2 PBW3 PBW4 Mean StdDev eMDL* eMDL 10x eMDL 250x eMDL 1000x

Se(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.007 0.068 1.7 6.8

Se(VI) 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.029 0.73 2.9

SeCN 0.000 0.000 0.000 0.000 0.000 0.000 0.003 0.026 0.65 2.6

MeSe(IV) 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.041 1.0 4.1

SeMe 0.000 0.000 0.000 0.000 0.000 0.000 0.004 0.041 1.0 4.1

eMDL = Estimated Method Detection Limit

*Please see narrative regarding eMDL calculations

Quality Control Summary - Certified Reference Materials

Analyte (μg/L) CRM True Value Result Recovery

Se(IV) LCS 4.79 4.89 102.2

Se(VI) LCS 4.74 4.59 96.9

SeCN LCS 4.46 4.40 98.6

MeSe(IV) LCS 3.24 3.05 94.3

SeMe LCS 4.66 4.48 96.0

Selenium Speciation Results for Duke Energy

Project Name: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins

LIMS #J13020369

Date: March 8, 2013

Report Generated by: Russell Gerads

Applied Speciation and Consulting, LLC

Page 13 of 16
Quality Control Summary - Matrix Duplicates

Analyte (μg/L) Sample ID Rep 1 Rep 2 Mean RPD

Se(IV) Batch QC ND (<6.8) ND (<6.8) NC NC

Se(VI) Batch QC ND (<2.9) ND (<2.9) NC NC

SeCN Batch QC ND (<2.6) ND (<2.6) NC NC

MeSe(IV) Batch QC ND (<4.1) ND (<4.1) NC NC

SeMe Batch QC ND (<4.1) ND (<4.1) 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 Spike/ Matrix Spike Duplicate

Analyte (μg/L) Sample ID Spike Conc MS Result Recovery Spike Conc MSD Result Recovery RPD

Se(IV) Batch QC 5560 5658 101.8 5560 5534 99.5 2.2

Se(VI) Batch QC 5045 5009 99.3 5045 4890 96.9 2.4

SeCN Batch QC 4575 4462 97.5 4575 4451 97.3 0.3

Report Generated by: Russell Gerads

Applied Speciation and Consulting, LLC

Selenium Speciation Results for Duke Energy

Project Name: Belews - FGD WWTS Bi-Monthly Sampling)

Contact: Jay Perkins

LIMS #J13020369

Date: March 8, 2013

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