Appendix B

DATA REVIEW NARRATIVES

### MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD CC: Jezebele Alicea, Alternate Work Assignment Manager, EPA EAD Deb Bartram, ERG TJ Finseth, ERG From: Randy Mercurio, ERG Date: 9/1/2011 Subject: FGS Data Review Narrative for Tota l and Dissolved Mercury – Episode 6562

Frontier Global Sciences (FGS) generated analytical data for total and dissolved mercury. FGS analyzed the samples according to EPA Method 1631E for mercury by Cold Vapor Atomic Fluorescence Spectrometry (CVA-FS) analysis.

Table 1 summarizes the 37 samples (excluding laboratory filter blanks) FGS extracted and analyzed for total and dissolved mercury.

Table 1. EPA Episode 6562 Total & Dissolved Mercury – Sample Identification

EPA Sample # Lab Sample ID # Sample Matrix Sample Description Sampling Date

71841 1008203-01 Aqueous FGD Influent Day 1 8/23/2010

71841 1008203-02 Aqueous Dissolved FGD Influent, Day 1 8/23/2010

71842 1008207-06 Aqueous FGD Influent, Day 2 8/24/2010

71842 1008207-07 Aqueous Dissolved FGD Influent, Day 2 8/24/2010

71843 1008223-13 Aqueous FGD Influent, Day 3 8/25/2010

71843 1008223-14 Aqueous Dissolved FGD Influent, Day 3 8/25/2010

71844 1008240-09 Aqueous FGD Influent, Day 4 8/26/2010

71844 1008240-10 Aqueous Dissolved FGD Influent, Day 4 8/26/2010

71845 1008207-08 Aqueous FGD SBR Influent, Day 1 8/24/2010

71845 1008207-09 Aqueous Dissolved FGD SBR Influent, Day 1 8/24/2010

71846 1008223-15 Aqueous FGD SBR Influent, Day 2 8/25/2010

71846 1008223-16 Aqueous Dissolved FGD SBR Influent, Day 2 8/25/2010

71847 1008240-11 Aqueous FGD SBR Influent, Day 3 8/26/2010

71847 1008240-12 Aqueous Dissolved FGD SBR Influent, Day 3 8/26/2010

71848 1008250-03 Aqueous FGD SBR Influent , Day 4 8/27/2010

71848 1008250-04 Aqueous Dissolved FGD SBR Influent , Day 4 8/27/2010

71849 1008207-10 Aqueous FGD SBR Effluent, Day 1 8/24/2010

71849 1008207-11 Aqueous Dissolved FGD SBR Effluent, Day 1 8/24/2010

71850 1008223-17 Aqueous FGD SBR Effluent, Day 2 8/25/2010

71850 1008223-18 Aqueous Dissolved FGD SBR Effluent, Day 2 8/25/2010

1Table 1. EPA Episode 6562 Total & Dissolved Mercury – Sample Identification

EPA Lab Sample Sample Sampling Sample # ID # Matrix Sample Description Date

71851 1008240-13 Aqueous FGD SBR Effluent, Day 3 8/26/2010

71851 1008240-14 Aqueous Dissolved FGD SBR Effluent, Day 3 8/26/2010

71852 1008250-05 Aqueous FGD SBR Effluent , Day 4 8/27/2010

71852 1008250-06 Aqueous Dissolved FGD SBR Effluent , Day 4 8/27/2010

71853 1008240-15 Aqueous FGD SBR Infl uent - Duplicate 8/26/2010

71853 1008240-16 Aqueous Dissolved FGD SBR Influent - Duplicate 8/26/2010

71854 1008223-19 Aqueous FGD SBR Efflue nt Duplicate, Day 2 8/25/2010

71854 1008223-20 Aqueous Dissolved FGD SBR E ffluent Duplicate, Day 2 8/25/2010

71855 1008203-03 Aqueous FGD Influent Field Blank, Day 1 8/23/2010

71856 1008203-06 Aqueous FGD SBR Influent Field Blank, Day 1 8/23/2010

71857 1008207-12 Aqueous FGD SBR Influent Field Blank, Day 2 8/24/2010

71858 1008223-11 Aqueous FGD SBR Influent Field Blank, Day 3 8/25/2010

71859 1008240-07 Aqueous FGD SBR Influent Field Blank, Day 4 8/26/2010

71860 1008203-09 Aqueous FGD SBR Effluent Field Blank, Day 1 8/23/2010

71861 1008207-19 Aqueous FGD SBR Effluent Field Blank, Day 2 8/24/2010

71862 1008223-12 Aqueous FGD SBR Effluent Field Blank, Day 3 8/25/2010

71863 1008240-08 Aqueous FGD SBR Effluent Field Blank, Day 4 8/26/2010

SUMMARY

The samples were prepared according to EPA Method 1631E to be analyzed by CVAFS. There were no findings from the data review th at required additional qualifiers in this dataset.

SAMPLE RECEIPT, HANDLIN G, AND STORAGE ISSUES

There were no sample receipt issues in this data package.

INITIAL CALIBRATION

FGS performed the initial calibrations on each analysis day. The initial calibration for the CVAFS analysis consisted of a blank and five calibration standards with a correlation coefficient ≥ 0.995. All method specified criteria were met.

INITIAL AND CONTINUING CAL IBRATION VERIFICATIONS

All initial and continuing calibration verifi cations (ICVs, CCVs) met method-specified criteria.

23 BLANKS

All instrument and preparation blanks met meth od-specified criteria. Preparation Blanks F009230-BLK1, F009230-BLK2, F009252-BLK5, F009277-BLK1, F009277-BLK3, F009277-BLK4 and F009277-BLK5 had mercury le vels greater than or equal to the MDL but less than the reporting limit and thes e were appropriately flagged with the “J” qualifier. No additional qualifiers were required.

DUPLICATES

Field duplicates, samples 71854 and 71853, were collected on samples 71850 and 71847, respectively. The 71850/71854 relative percen t difference (RPD) was 17.4% for total mercury and 26.3% for dissolved merc ury. The 71847/71853 RPD was 3.8% for total mercury and 154% for dissolved mercury. The method-suggested RPD criteria between field duplicates is 20%.

Laboratory duplicates were performed in this episode on samples 71848, 71846, and 71847. All RPDs were less than 20% (the me thod-suggested RPD criterion between field duplicates; the method does not require the analysis of laboratory duplicates).

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

Matrix spikes (MS) and ma trix spike duplicates (MSD) were performed on samples 71846, 71844, 71847, 71851 and 71848 for the total mercury analyses. MS and MSDs were performed on samples 71851 and 71848 for the dissolved mercury analyses. All aqueous MS/MSD recoveries were within the method specifications of 71-125%, except for the dissolved mercury MSD for sample 71851, which had a recovery of 60.1%. Therefore, the dissolved mercury result for sample 71851 was flagged with the laboratory’s QM-07 qualifier. All RP Ds met method-specified criteria.

### MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD CC: Jezebele Alicea, Alternate Work Assignment Manager, EPA EAD Deb Bartram, ERG TJ Finseth, ERG From: Randy Mercurio, ERG Date: 9/1/2011 Subject: TestAmerica Data Review Narrative fo r Total and Dissolved Metals by 200.8 – Episode 6562

Test America generated analytical data for total and dissolved meta ls (antimony, arsenic, cadmium, chromium, copper, lead, nickel, sele nium, silver, thallium, and vanadium).The samples were analyzed according to EPA Method 200.8.

Table 1 summarizes the samples Test Ameri ca extracted and analyzed for total and dissolved metals by EPA Method 200.8.

Table 1. EPA Episode 6562 Total & Dissolved Metals – Sample Identification

EPA Sample # EPA Sample Description Lab Sample ID # Sample Matrix Sampling Date Receipt Date

71841 FGD Influent, Day 1 280-6658-1 Aqueous 8/23/2010 8/24/2010
71842 FGD Influent, Day 2 280-6685-1 Aqueous 8/24/2010 8/25/2010
71843 FGD Influent, Day 3 280-6742-1 Aqueous 8/25/2010 8/26/2010
71844 FGD Influent, Day 4 280-6791-1 Aqueous 8/26/2010 8/27/2010
71845 FGD SBR Influent, Day 1 280-6685-2 Aqueous 8/24/2010 8/25/2010
71846 FGD SBR Influent, Day 2 280-6742-2 Aqueous 8/25/2010 8/26/2010
71847 FGD SBR Influent, Day 3 280-6791-2 Aqueous 8/26/2010 8/27/2010
71848 FGD SBR Influent, Day 4 280-6827-1 Aqueous 8/27/2010 8/28/2010
71849 FGD SBR Effluent, Day 1 280-6685-3 Aqueous 8/24/2010 8/25/2010
71850 FGD SBR Effluent, Day 2 280-6742-3 Aqueous 8/25/2010 8/26/2010
71851 FGD SBR Effluent, Day 3 280-6791-3 Aqueous 8/26/2010 8/27/2010
71852 FGD SBR Effluent, Day 4 280-6827-2 Aqueous 8/27/2010 8/28/2010

71853 FGD SBR Influent - Duplicate, Day 3 280-6791-4 Aqueous 8/26/2010 8/27/2010

71854 FGD SBR Effluent - Duplicate, Day 2 280-6742-4 Aqueous 8/25/2010 8/26/2010

71855 FGD Influent Field Blank, Day 1 280-6658-2 Aqueous 8/23/2010 8/24/2010

71856 FGD SBR Influent Field Blank, Day 1 280-6685-4 Aqueous 8/24/2010 8/25/2010

1Table 1. EPA Episode 6562 Total & Dissolved Metals – Sample Identification

EPA Sample # EPA Sample Description Lab Sample ID # Sample Matrix Sampling Receipt Date Date

71860 FGD SBR Effluent Field Blank, Day 1 280-6685-5 Aqueous 8/24/2010 8/25/2010

SUMMARY

The samples were prepared for total and dissolved metals analysis according to Test America’s “FGD ICP/MS SOP: Inductively Coupled Plasma Mass Spectrometry for Trace Elements Analysis in Flue Gas Desulf urization Wastewaters,” dated October 6, 2010, based on EPA Method 200.8, by ICP/MS an alysis. Any significant findings are summarized below. No additional data qualifiers were required.

 All matrix spike (MS) and matrix spike duplicates (MSD) for total and dissolved silver failed the 70-130% control limits w ith poor recoveries. The poor recoveries are probably due to high sulfates in th is episode’s samples that could form insoluble silver sulfide and/or silver sulfate.

INTERNAL STANDARDIZATION

All internal standards used by TestAmeri ca were within the method criteria.

INITIAL CALIBRATION

Test America performed the in itial calibrations on each an alysis day or before each analysis if more than one analysis was performed in one day. The initial calibration for the ICP-MS analysis consisted of a bl ank and four calibration standards.

INITIAL AND CONTINUING CALIBRA TION VERIFICATION (ICV/CCV)

The initial calibration verifications (ICV) and continuing calibrati on verifications (CCV) performed by TestAmerica all had recoveries within the method criteria.

METHOD/INSTRUMENT BLANKS

All the method blanks were less than the reporting limit. No additional qualifiers were required for method blanks.

All instrument blanks (ICB and CCB) were less than the reporting limit.

2REPORTI NG LIMIT VERIFICATION STANDARD (CRI)

All CRI samples passed Test Am erica’s 50–150% recovery limits.

LABORATORY CONTROL SAMPLES (LCS)

All LCS samples passed the method limits of 85–115%.

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION (ICSA)

Based on TestAmerica’s SOP, all interfer ence check sample A (ICSA) results had analytes of interest with concentrations less than the RL or less than five times the RL when known inherent contaminants are presen t in the stock solution used to make the ICS.

All interference check sample B (ICSAB) synthetic spikes recovered within TestAmerica’s SOP criteria of 70–130% of the true value.

SERIAL DILUTION (SRD)

The serial dilution performed for the total and dissolved sample 71851 FGD SBR Effluent, Day 3 (280-6791-3) met Test Amer ica’s requirement of ±10% difference.

FIELD DUPLICATES

The relative percent diffe rence (RPD) of the fiel d duplicates (71850/71854 & 71847/71853) were less than ±20% for all values equal to or greater than the reporting limit.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

MS and MSDs were performed on the total and dissolved samples of 71848 and 71851. Many spikes that failed outside of the 70–130% method control limits were flagged with a “4” qualifier indicating concentrations in the parent samples were greater than 4 times the spike amounts. All MS/MSDs for total and dissolved silver failed the 70–130% control limits. The poor recoveries of Silver are probably due to high sulfates (1600–1800 mg/L) in this episode’s samples that could form insoluble silver sulfide and/or silver sulfate. Otherwise, all MS/MSDs were w ithin the 70–130% method control limits. The RPD for all MS/MSD passed the method-specified criteria of 20 percen t, except for total silver for sample 71748 MS/MSD analyses, which had an RPD of 96%.

POST DIGESITON SPIKES

The post digestion spike performed on sa mple 71851 FGD SBR Effluent, Day 3 (280- 6791-3) for total and dissolved analytes passed TestAmer ica’s 85–115% control limits with the exception of silver. The poor recove ries of silver are probably due to high

34 sulfates (1600–1800 mg/L) in this episode’s samples that could form insoluble silver sulfide and/or silver sulfate.

DETECTION LIMITS

The laboratory performed an MDL study in the synthetic FGD wastewater matrix, instead of reagent water.

### MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD CC: Jezebele Alicea, Alternate Work Assignment Manager, EPA EAD Deb Bartram, ERG TJ Finseth, ERG From: Randy Mercurio, ERG Date: 9/1/2011 Subject: TestAmerica Data Review Narrative fo r Total and Dissolved Metals by 200.7 – Episode 6562

Test America generated analytical data for total and dissolved me tals (aluminum, boron, barium, beryllium, calcium, cobalt, iron, ma gnesium, manganese, molybdenum, sodium, tin, titanium, and zinc). The samples we re analyzed according to EPA Method 200.7.

Table 1 summarizes the samples Test Ameri ca extracted and analyzed for total and dissolved metals by EPA Method 200.7.

Table 1. EPA Episode 6562 Total & Dissolved Metals – Sample Identification

EPA Sample # EPA Sample Description Lab Sample ID # Sample Matrix Sampling Date Receipt Date

71841 FGD Influent, Day 1 280-6658-1 Aqueous 8/23/2010 8/24/2010
71842 FGD Influent, Day 2 280-6685-1 Aqueous 8/24/2010 8/25/2010
71843 FGD Influent, Day 3 280-6742-1 Aqueous 8/25/2010 8/26/2010
71844 FGD Influent, Day 4 280-6791-1 Aqueous 8/26/2010 8/27/2010
71845 FGD SBR Influent, Day 1 280-6685-2 Aqueous 8/24/2010 8/25/2010
71846 FGD SBR Influent, Day 2 280-6742-2 Aqueous 8/25/2010 8/26/2010
71847 FGD SBR Influent, Day 3 280-6791-2 Aqueous 8/26/2010 8/27/2010
71848 FGD SBR Influent, Day 4 280-6827-1 Aqueous 8/27/2010 8/28/2010
71849 FGD SBR Effluent, Day 1 280-6685-3 Aqueous 8/24/2010 8/25/2010
71850 FGD SBR Effluent, Day 2 280-6742-3 Aqueous 8/25/2010 8/26/2010
71851 FGD SBR Effluent, Day 3 280-6791-3 Aqueous 8/26/2010 8/27/2010
71852 FGD SBR Effluent, Day 4 280-6827-2 Aqueous 8/27/2010 8/28/2010
71853 FGD SBR Influent - Duplicate, Day 3 280-6791-4 Aqueous 8/26/2010 8/27/2010

71854 FGD SBR Effluent - Duplicate, Day 2 280-6742-4 Aqueous 8/25/2010 8/26/2010

71855 FGD Influent Field Blank, Day 1 280-6658-2 Aqueous 8/23/2010 8/24/2010

1Table 1. EPA Episode 6562 Total & Dissolved Metals – Sample Identification

EPA Sample # EPA Sample Description Lab Sample ID # Sample Matrix Sampling Receipt Date Date

71856 FGD SBR Influent Field Blank, Day 1 280-6685-4 Aqueous 8/24/2010 8/25/2010

71860 FGD SBR Effluent Field Blank, Day 1 280-6685-5 Aqueous 8/24/2010 8/25/2010

SUMMARY

The samples were prepared for total and dissolved metals analysis according to Test America’s SOP for ICP Analysis for Trace Metals by Method 200.7.

There were no findings from the data review that required additional qualifiers (excluding those identified by the laboratory) in this dataset.

SAMPLE RECEIPT, HANDLIN G, AND STORAGE ISSUES

There were no sample receipt issues in this data package.

INTERNAL STANDARDIZATION

While the internal standard (ISTD) Yttrium was used for these analyses, no checks for the ISTD recoveries within the ±30% criter ion of the calibration blank as per Section 9.11 of the SOP were seen. All ISTD were within the control limits.

INITIAL CALIBRATION

Test America performed the initial calibra tions on each analysis day. The initial calibration for the ICP analysis consisted of a blank and one calibration standard.

INITIAL AND CONTINUING CAL IBRATION VERIFICATIONS

The initial calibration verifications (ICV) and continuing calibrati on verifications (CCV) performed by TestAmerica all had recoveries within the method criteria.

METHOD/INSTRUMENT BLANKS

All the method blanks were less than the re porting limit; however, some had levels above the MDL and were flagged with the “J” qualifier.

All instrument blanks (ICB and CCB) were less than the reporting limit; however, some elements were above the MDL and we re flagged with the “J” qualifier.

23 LABORATORY CONTROL SAMPLES (LCS)

All LCSs passed the method control limits of 85–115%.

INTERFERENCE CHECK SOLUTIONS

Interference checks were perfor med using the synthetic matrix as the check solution. All data quality objectives met TestAmerica’s SOP criteria.

REPORTING LIMIT VERIFICATION STANDARD (CRI)

All CRI samples passed Test Amer ica’s SOP control limits of 50–150%.

FIELD DUPLICATES

The total and dissolved relative percent differences (RPDs) of the field duplicates (71854 and 71853) to parent samples (71850 and 71847, respectively) were less than 20% for values greater than the reporting limit.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD)

Matrix spikes (MS) and matr ix spike duplicates (MSD) were performed on the total and dissolved samples of 71848 and 71851. Some el ements with high concentrations frequently failed the EPA 200.7 Method spik e recovery control limits of 70–130% but were flagged with a “4” qualifier indicating th at the concentration in the parent sample was greater than 4 times the spike and coul d not be reliably calculated. No MS/MSD spike recoveries failed the EPA 200.7 Me thod control limits of 70–130%, except those already qualified with a “4” as mentione d above, and therefor e no additional data qualifiers were needed. In addition, al l RPDs of the MS/MSDs were within TestAmerica’s ± 20% requirements.

SERIAL DILUTION (SRD)

Serial dilutions were performe d for each batch of total and di ssolved samples. All serial dilution percent differences were less than 10% as required by Test America’s SOP.

POST DIGESTION SPIKE

Both total and dissolved post digestion sp ike samples performed passed the method criteria of 85–115%.

DETECTION LIMITS

The laboratory performed an MDL study in the synthetic FGD wastewater matrix, instead of reagent water.

### MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD CC: Jezebele Alicea, Alternate Work Assignment Manager, EPA EAD Deb Bartram, ERG TJ Finseth, ERG From: Donna Tedder, ERG Date: 9/1/2011 Subject: FGS Data Review Narrative for Dissolved Hexavalent Chromium – Episode 6562

Frontier Global Sciences (FGS) generated an alytical data for dissolved hexavalent chromium for Sample Episode 6562. FGS anal yzed the samples according to a modified EPA Method 218.6 for dissolved hexavalent chromium by Liquid Chromatography – Inductively Coupled Plasma Ma ss Spectrometry (LC-ICP-MS).

Table 1 summarizes the samples FGS extracted and analyzed for dissolved hexavalent chromium.

Table 1. EPA Episode 6562 Dissolved Hexavalent Chromium – Sample Identification

EPA Sample # Sample Matrix Sample Description Sampling Date Analysis Date
71841 Aqueous FGD Influent Day 1 8/2/10 8/9/10
71842 Aqueous FGD Influent Day 2 8/3/10 8/9/10
71843 Aqueous FGD Influent Day 3 8/4/10 8/9/10
71844 Aqueous FGD Influent Day 4 8/5/10 8/30/10
71845 Aqueous FGD Bior eactor Influent Day 1 8/3/10 8/9/10
71846 Aqueous FGD Bior eactor Influent Day 2 8/4/10 8/9/10
71847 Aqueous FGD Bior eactor Influent Day 3 8/5/10 8/30/10
71848 Aqueous FGD Bior eactor Influent Day 4 8/6/10 8/30/10
71849 Aqueous FGD Bioreactor E ffluent Day 1 8/3/10 8/9/10
71850 Aqueous FGD Bioreactor E ffluent Day 2 8/4/10 8/30/10
71851 Aqueous FGD Bioreactor E ffluent Day 3 8/5/10 8/30/10
71852 Aqueous FGD Bioreactor E ffluent Day 4 8/6/10 8/30/10
71853 Aqueous FGD Bioreactor Infl uent Dup Day 3 8/5/10 8/30/10
71854 Aqueous FGD Bioreactor Effl uent Dup Day 2 8/4/10 8/30/10
71855 Aqueous FGD Influent Field Blank Day 1 8/2/10 8/9/10
71856 Aqueous FGD Bioreact or Influent Field Blank Day 1 8/3/10 8/9/10
71860 Aqueous FGD Bioreact or Effluent Field Blan k Day 1 8/3/10 8/9/10

1SUMMARY

The sam ples were prepared for dissolved hexavalent chromium analysis according to FGS-129.01 Standard Operating Procedure (SOP), a modified EPA Method 218.6. Several samples (71841, 71842, 71843, 71844, 71845, 71846, 71847, 71848, 71849, 71850, 71851, 71852, 71853, and 71854) were diluted prior to analysis due to the presence of high levels of nontarget chloride interferences.

There were no issues requiring additional data qualifiers fo r the hexavalent chromium data in this episode.

SAMPLE RECEIPT, HANDLIN G, AND STORAGE ISSUES

There were no sample receipt issues in this data package.

INITIAL PRECISION AND ACCURACY/RECOVERY

The initial precision and reco very (IPR) performed by FGS had recoveries within the method criteria.

ON-GOING PRECISION AND ACCURACY/RECOVERY

The analytical method did not require the analysis of an on-going precision and recovery (OPR).

INITIAL CALIBRATION

FGS performed the initial calibrations on each analysis day. The initial calibration for the LC-ICP-MS analysis consisted of a bl ank and eight calibration standards with a correlation factor ≥ 0.995 as required by the method.

A secondary source initial calib ration verification (ICV) wa s analyzed and passed ± 10% of true value required by the method.

CONTINUING CALIBRATION VERIFICATION

All CCVs met method-specified criteria, ± 10% of true value with recoveries ranging from 95 to 107%.

BLANK

All of the preparation blanks/laboratory reagent blanks (LRBs) and the continuing calibration blanks (CCBs) met met hod-specified requirements.

23 OTHER CHECKS

The laboratory control sample/duplicate (LCS/LCSD) or laboratory fortified blank/duplicate (LFB/LFBD) pa ssed method criteria of ± 10% of true value with recoveries of 97.9% and 102%. A second set of LFB/LFBD, for the later analysis date, had recoveries of 100% and 95.5%. The method suggested that a s econd source quality control sample (QCS) must be analyzed by the laboratory at least once a quarter. The second source ICV meets this recommendation.

DETECTION LIMITS

The laboratory method detection limit (MDL ) in the synthetic matrix was 0.392 ug/L. Results below this MDL were reported as not detected.

DUPLICATES

There were no laboratory duplicat es performed in this episod e other than a duplicate of the LCSD and a duplicate of the matrix spike (MS).

Two field duplicates were collected and analyzed. Sample 71854 was a duplicate of effluent sample 71850. These samples were non detects (NDs), indicating the analyte was not detected at or above the method detect ion limit. Sample 71853 was a duplicate of influent sample 71847. These samples were also NDs.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

The MS and matrix spike duplicate (MSD) we re performed using a secondary source spike on samples 71844, 71848, and 71851. All MS/M SD recoveries were within 75%- 125%, with RPDs of 0.461%, 0.274% , and 4.03%, respectively.

### MEMORANDUM

To: Ron Jordan, Work Assignment Manager, EPA EAD CC: Jezebele Alicea, Alternate Work Assignment Manager, EPA EAD Deb Bartram, ERG TJ Finseth, ERG From: Donna Tedder, ERG Date: 9/1/2011 Subject: TestAmerica Data Review Narrative fo r Classicals Analyses – Episode 6562

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry analyses for Sample Episode 6562. All samples were tested for the following analytes:

 Ammonia by EPA method 350.1,

 Biochemical Oxygen Demand – 5 day (BOD 5 ) by SM 5210B,

 Chloride and Sulfate by EPA method 300.0,

 Chemical Oxygen Demand (COD) by EPA method 410.4,

 Cyanide by SM 4500 CN - E,

 Nitrate/Nitrite by EPA method 353.2,

 Phosphorus by EPA method 365.1,

 Total Dissolved Solids (TDS) by SM 2540C,

 Total Kjeldahl Nitrogen (TKN) by EPA method 351.2, and

 Total Suspended Solids (TSS) by SM 2540D.

Table 1 summarizes the 14 samples that TestAmerica analyzed for the above analytes.

Table 1. EPA Episode 6562 Classical An alytes – Sample Identification

EPA Sample # Sample Matrix Sample Description Sampling Date 71841 Water FGD Influent, Day 1 8/23/10 71842 Water FGD Influent, Day 2 8/24/10 71843 Water FGD Influent, Day 3 8/25/10 71844 Water FGD Influent, Day 4 8/26/10 71845 Water FGD SBR Influent, Day 1 8/24/10 71846 Water FGD SBR Influent, Day 2 8/25/10 71847 Water FGD SBR Influent, Day 3 8/26/10 71848 Water FGD SBR Influent, Day 4 8/27/10 71849 Water FGD SBR Effl uent, Day 1 8/24/10 71850 Water FGD SBR Effl uent, Day 2 8/25/10 71851 Water FGD SBR Effl uent, Day 3 8/26/10

1Table 1. EPA Episode 6562 Classical An alytes – Sample Id entification

EPA Sample # Sample Matrix Sampling Sample Description Date 71852 Water FGD SBR Effl uent, Day 4 8/27/10 71853 Water FGD SBR Influent - Duplicate 8/26/10 71854 Water FGD SBR Efflue nt - Duplicate 8/25/10

SUMMARY

All samples were analyzed within the holdi ng time specified in 40 CFR 136 Table II. All samples were preserved appropriately.

Two field duplicate samples were collected a nd analyzed for each analyte. The relative percent difference (RPD) between the sample and its duplicate was less than 20% unless otherwise noted below.

If applicable, the appropriate number of standards was used to create a calibration curve. If sample results were above the highest standa rd used to create the curve, the sample was diluted and reanalyzed. All sample results we re between the lowest and highest standards unless otherwise noted below. Additionally, un less otherwise noted, all calibration blanks and calibration verification samples met the criteria specified in the method.

If required by the method, the quality control sample (QCS), a seconda ry source standard used to verify calibration, was always within the control limits speci fied by the method.

As described below, the analyte of interest was detected above the method detection limit (MDL) in some laboratory reagent blanks (LRB). However, the analyte of interest was never detected above the reporting limit (RL) in the LRBs. If required by the method, all laboratory fortified blanks (LFB) met the crit eria specified in the method unless specified below.

If required by the method, a matrix spike (MS) sample was analyzed on samples 71848 (FGD bioreactor influent) a nd 71851 (FGD bioreactor effluent ) for each analyte to check for matrix interferences. For some analytes , TestAmerica spiked more samples than required. All MS samples analyzed met the criteria specified in the method unless described below.

DATA NOTES/ISSUES

Ammonia

The MS and MSD results for sample 71841 were above the calibration range. Because the percent recoveries were within the control limits specified by EPA method 350.1, the laboratory did not reanalyze the samples usi ng a higher dilution fact or. If reported, the MS and MSD results will be qualified as estimated values. The result for sample 71841

2was within the calibra tion range, so this sa mple was not qualified. The LFB associated with this sample met the method criteria.

BOD 5
The data reviewer identified no issues. All gl ucose-glutamic acid standards, water blanks, and laboratory duplicates were analyzed approp riately and met the criteria specified in SM 5210B.

Chloride and Sulfate

The MS and MSD results for samples 71848 and 71851 for sulfate and chloride were above the calibration curve. TestAmerica di d not reanalyze the samples with a higher dilution factor because the percent recove ries were within EPA method 300.0 control limits. If reported, these MS and MSD results will be qualified as estimated values. The LFB associated with this sa mple met the method criteria.

COD

The RPD between sample 71847 and its field duplicate 71853 was 37.0%. Even though the RPD was greater than 20%, the sample wa s not qualified because there are no specific control limits for field duplicat es specified in EPA method 410.4.

The percent recoveries for the MS a nd MSD analyses for sample 71848 (FGD SBR influent) and 71851 (FGD SBR effluent) were below the control limits of 90-110% required by EPA method 410.4. The percent recove ries for the MS and MSD analyses for sample 71848 were 71% and 72%, respectively, and the percent recoveries for the MS and MSD analyses for sample 71851 were 75% and 76%, respectively. These low percent recoveries suggest that results for samples with a sim ilar matrix (FGD SBR influent and FGD SBR effluent) could be biased lo w. Samples 71848 and 71851 were qualified as minimum values. The LFB percent recoveries a ssociated with all samples met the method criteria.

Cyanide

Sample 71841 was preserved to a pH greater than 10 S.U. after sample collection, but when the laboratory received the sample, the pH was neutral. The laboratory added more NaOH to increase the pH to greater than 10 S.U. upon receipt. This sample was qualified as an estimated value.

Cyanide was detected at 0.00273 mg/L in the laboratory reagent blank (LRB) associated with samples 71841, 71842, 71845, and 71849 and also detected at 0.00274 mg/L in the LRB associated with samples 71843, 71846, 71850, and 71854. Additionally, cyanide was detected at 0.00586 mg/L in the LR B associated with samples 71844, 71847, 71848, 71851, 71852, and 71853. These blank results were greater than the MDL (0.0020 mg/L),

3but less than the RL (0.010 mg/L). Because all of the blank results were less than the RL, no samples were qualified based on these LRB results.

Results for the following samples were less than the lowest calib ration standard (0.01 mg/L): 71850, 71851, 71852, and 71854. Because all of these samples were already flagged by TestAmerica with a “J”, meaning the sample result was an estimated value because it was less than the RL, no fu rther qualification was necessary.

The percent recoveries for the MS and MSD analyses of sample 71851 were both 22%. The laboratory spiked the sample with 0.100 mg /L. The percent recove ries of both the MS and MSD samples were outside of th e laboratory control criteria of 90-110%. However, because there are no criteria fo r MS/MSD analyses specified in SM 4500 CN E and sample 71851 was already qualified with a “J” meaning the result was less than the RL, further qualification was unnecessary.

The RPD between sample 71847 and its field duplicate 71853 was 26.9%. Even though this RPD was greater than 20%, the samples were not qualified because there are no specific control limits for field duplicates specified in SM 4500 CN - E.

Nitrate/Nitrite

The MS and MSD results for 71841 were above the calibration curve. Because the percent recoveries were w ithin the control lim its specified by EPA method 353.2, the laboratory did not reanalyze the samples usi ng a higher dilution fact or. If reported, the MS and MSD results will be qualified as estimated values. The result for sample 71841 was within the calibration range, so this sa mple was not qualified. The LFB associated with this sample met the method criteria.

Phosphorus

The percent recoveries for the MS/MSD anal ysis of sample 71851 were not within the control limits of 90-110% specified in EPA Method 365.1, but were within the laboratory control limits of 71-128%. Th e percent recoveries of th e MS and MSD samples were 83% and 86%, respectively. Sample 71851 was qualified by the laboratory with a “J” meaning the result was less than the RL, so no further qualification was necessary. The LRB percent recovery met the method criteria.

Samples 71842, 71845, 71846, 71849, 71850, 71851, and 71854 were less than the lowest calibration standard (0.025 mg/L). Test America flagged these samples with a “J”, so further qualification was not necessary.

The RPD between sample 71847 and its field duplicate 71853 for phosphorus was 22.2%. The result for sample 71853 was greater than the MDL, but less than the RL and the result for sample 71847 was the RL itself. The low concentrations of these samples might be the reason for the high RPD. Even though the RPD was greater than 20%, the sample

4was not qualified because there are n o specific control limits for field duplicates specified in EPA Method 365.1.

TDS

Constant weight was not achieved after 3 drying cycles for samples 71843, 71844, 71845, 71846, 71847, 71848, 71849, 71850, 71851, 71852, 71853, and 71854 in analytical batch 29115. It should be noted that the weight increa sed from the first weighing to the second weighing for all samples. Method 2540C warns that samples which contain high levels of calcium, magnesium, chloride, and sulfate may be hygroscopic meaning they absorb moisture from the air. FGD wastewater contai ns high concentratio ns of all of these species. This was likely the cause for the inconsistent weight calculations. The samples were not qualified, but results may be biased high.

The RPDs for laboratory duplicates from samples 71842 and 71848 were less than 10% as required by SM 2540C; however, the RPD for sample 71844 was 14%. Because the RPD was greater than the method contro l limits, sample 71844 was qualified as an estimated value.

TDS was detected above the MDL (4.7 mg/L), but below th e RL (10 mg/L) at 7.0 mg/L in the method blank (MB) associated with sample 71841. Because the blank result was less than the RL, no samples were qualified.

TKN

The percent recovery for the LFB associat ed with sample 71841 was not within the method control limits of 90-110%, but was wi thin the laboratory control limits of 77- 115%. The percent recove ries for the LFB and LFBD were 89% and 90%, respectively. Because the percent recovery of the LFB was below the method criteria, sample 71841 was qualified as a minimum value.

TestAmerica performed MS and MSD analys es on sample 71851. The percent recoveries for the MS and MSD samples were 114% a nd 113%, respectively. The samples did not meet the method control limits of 90-110%, but did meet the laboratory control limits of 54-131%. The LFB associated with this batch was within the labora tory control limits. The sample concentration was greater than 4 times the spike amount in the MS and MSD samples, so TestAmerica stated that the percent recoveries and RPDs could not be reliably calculated. Sample 71851 was not qualified because it is not possible to determine if the MS/MSD failure was a result of matrix interferences or caused by low spiking level.

TKN was detected at 0.237 mg/L in the laborat ory reagent blank associated with samples 71842 - 71854. The blank result was greater than the MDL (0.077 mg/L), but less than the RL (1.0 mg/L). Because the blank result was less than the RL, it was not necessary to qualify any samples.

56 TSS

One laboratory duplicate was analyzed per ba tch. The RPDs for the laboratory duplicates of samples 71841, 71842, 71848, 71851, and 71852 were less than 10% as required by the method. However, the RPD for the labo ratory duplicate of sample 71854 was 18%. Because the laboratory duplicate RPD was gr eater than the method control criteria, sample 71854 was qualified as an estimated value.

The RPD between sample 71847 and its field duplicate 71853 was 80.9%. The RPD between sample 71850 and its field duplicat e 71854 was 28.6%. Even though these RPDs were greater than 20%, the samples were not qualified because there are no specific control limits for field duplicates specified in SM 2540D.

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level Detected 71848 COD Minimum Value MS % recoverybelow methodspecified criteria 130 mg/L

71851 COD Minimum Value MS % recoverybelow methodspecified criteria 140 mg/L

71841 Cyanide Estimated Value pH upon receipt < 10 S.U. 1.2 mg/L

71844 TDS Estimated Value Lab duplicateRPD > methodspecified criteria 11,000 mg/L

71841 TKN Minimum Value LFB % recoverybelow methodspecified criteria 130 mg/L

71854 TSS Estimated Value Lab duplicateRPD > methodspecified criteria 12 mg/L