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 Total 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 

1
Table 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 Influent - Duplicate 8/26/2010 

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

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

71854 1008223-20 Aqueous Dissolved FGD SBR Effluent 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 that required additional qualifiers in this 

dataset. 

SAMPLE RECEIPT, HANDLING, 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 CALIBRATION VERIFICATIONS 

All initial and continuing calibration verifications (ICVs, CCVs) met method-specified 

criteria. 

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3

BLANKS 

All instrument and preparation blanks met method-specified criteria. Preparation Blanks 

F009230-BLK1, F009230-BLK2, F009252-BLK5, F009277-BLK1, F009277-BLK3, 

F009277-BLK4 and F009277-BLK5 had mercury levels greater than or equal to the 

MDL but less than the reporting limit and these 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 percent difference (RPD) was 17.4% for total 

mercury and 26.3% for dissolved mercury. 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 method-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 matrix 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 RPDs 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 for Total and Dissolved Metals by 200.8 – 

Episode 6562

Test America generated analytical data for total and dissolved metals (antimony, arsenic, 

cadmium, chromium, copper, lead, nickel, selenium, silver, thallium, and vanadium).The 

samples were analyzed according to EPA Method 200.8. 

Table 1 summarizes the samples Test America 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 

1
Table 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 Desulfurization Wastewaters,” dated October 6, 

2010, based on EPA Method 200.8, by ICP/MS analysis. 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 with poor recoveries. The poor recoveries 

are probably due to high sulfates in this episode’s samples that could form 

insoluble silver sulfide and/or silver sulfate. 

INTERNAL STANDARDIZATION 

All internal standards used by TestAmerica were within the method criteria. 

INITIAL CALIBRATION 

Test America performed the initial calibrations on each analysis 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 blank and four calibration standards. 

INITIAL AND CONTINUING CALIBRATION VERIFICATION (ICV/CCV) 

The initial calibration verifications (ICV) and continuing calibration 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. 

2
REPORTING LIMIT VERIFICATION STANDARD (CRI) 

All CRI samples passed Test America’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 interference 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 present 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 America’s requirement of ±10% difference. 

FIELD DUPLICATES 

The relative percent difference (RPD) of the field 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 within the 70–130% method control limits. The 

RPD for all MS/MSD passed the method-specified criteria of 20 percent, 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 sample 71851 FGD SBR Effluent, Day 3 (280-

6791-3) for total and dissolved analytes passed TestAmerica’s 85–115% control limits 

with the exception of silver. The poor recoveries of silver are probably due to high 

3
4

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 for Total and Dissolved Metals by 200.7 – 

Episode 6562

Test America generated analytical data for total and dissolved metals (aluminum, boron, 

barium, beryllium, calcium, cobalt, iron, magnesium, manganese, molybdenum, sodium, 

tin, titanium, and zinc). The samples were analyzed according to EPA Method 200.7. 

Table 1 summarizes the samples Test America 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 

1
Table 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, HANDLING, 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% criterion 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 calibrations on each analysis day. The initial 

calibration for the ICP analysis consisted of a blank and one calibration standard. 

INITIAL AND CONTINUING CALIBRATION VERIFICATIONS 

The initial calibration verifications (ICV) and continuing calibration 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; 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 were flagged with the “J” qualifier. 

2
3

LABORATORY CONTROL SAMPLES (LCS) 

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

INTERFERENCE CHECK SOLUTIONS 

Interference checks were performed 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 America’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 matrix spike duplicates (MSD) were performed on the total and 

dissolved samples of 71848 and 71851. Some elements with high concentrations 

frequently failed the EPA 200.7 Method spike recovery control limits of 70–130% but 

were flagged with a “4” qualifier indicating that the concentration in the parent sample 

was greater than 4 times the spike and could not be reliably calculated. No MS/MSD 

spike recoveries failed the EPA 200.7 Method control limits of 70–130%, except those 

already qualified with a “4” as mentioned above, and therefore no additional data 

qualifiers were needed. In addition, all RPDs of the MS/MSDs were within 

TestAmerica’s ± 20% requirements. 

SERIAL DILUTION (SRD) 

Serial dilutions were performed for each batch of total and dissolved 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 spike 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 analytical data for dissolved hexavalent 

chromium for Sample Episode 6562. FGS analyzed the samples according to a modified 

EPA Method 218.6 for dissolved hexavalent chromium by Liquid Chromatography – 

Inductively Coupled Plasma Mass 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 Bioreactor Influent Day 1 8/3/10 8/9/10

71846 Aqueous FGD Bioreactor Influent Day 2 8/4/10 8/9/10

71847 Aqueous FGD Bioreactor Influent Day 3 8/5/10 8/30/10

71848 Aqueous FGD Bioreactor Influent Day 4 8/6/10 8/30/10

71849 Aqueous FGD Bioreactor Effluent Day 1 8/3/10 8/9/10

71850 Aqueous FGD Bioreactor Effluent Day 2 8/4/10 8/30/10

71851 Aqueous FGD Bioreactor Effluent Day 3 8/5/10 8/30/10

71852 Aqueous FGD Bioreactor Effluent Day 4 8/6/10 8/30/10

71853 Aqueous FGD Bioreactor Influent Dup Day 3 8/5/10 8/30/10

71854 Aqueous FGD Bioreactor Effluent 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 Bioreactor Influent Field Blank Day 1 8/3/10 8/9/10

71860 Aqueous FGD Bioreactor Effluent Field Blank Day 1 8/3/10 8/9/10

1
SUMMARY 

The samples 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 for the hexavalent chromium 

data in this episode. 

SAMPLE RECEIPT, HANDLING, AND STORAGE ISSUES 

There were no sample receipt issues in this data package. 

INITIAL PRECISION AND ACCURACY/RECOVERY 

The initial precision and recovery (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 blank and eight calibration standards with a 

correlation factor ≥ 0.995 as required by the method. 

A secondary source initial calibration verification (ICV) was 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 method-specified requirements. 

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3

OTHER CHECKS 

The laboratory control sample/duplicate (LCS/LCSD) or laboratory fortified 

blank/duplicate (LFB/LFBD) passed 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 second 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 duplicates performed in this episode 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 nondetects (NDs), indicating the analyte was 

not detected at or above the method detection 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) were performed using a secondary source 

spike on samples 71844, 71848, and 71851. All MS/MSD 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 for 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 (BOD5) 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 Analytes – 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 Effluent, Day 1 8/24/10 

71850 Water FGD SBR Effluent, Day 2 8/25/10 

71851 Water FGD SBR Effluent, Day 3 8/26/10 

1 
Table 1. EPA Episode 6562 Classical Analytes – Sample Identification 

EPA 

Sample # 

Sample 

Matrix 

Sampling 

Sample Description Date 

71852 Water FGD SBR Effluent, Day 4 8/27/10 

71853 Water FGD SBR Influent - Duplicate 8/26/10 

71854 Water FGD SBR Effluent - Duplicate 8/25/10 

SUMMARY 

All samples were analyzed within the holding time specified in 40 CFR 136 Table II. All 

samples were preserved appropriately. 

 

Two field duplicate samples were collected and 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 standard used to create the curve, the sample was 

diluted and reanalyzed. All sample results were between the lowest and highest standards 

unless otherwise noted below. Additionally, unless 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 secondary source standard 

used to verify calibration, was always within the control limits specified 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 criteria 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) and 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 using a higher dilution factor. If reported, the 

MS and MSD results will be qualified as estimated values. The result for sample 71841 

2 
was within the calibration range, so this sample was not qualified. The LFB associated 

with this sample met the method criteria. 

BOD5 

The data reviewer identified no issues. All glucose-glutamic acid standards, water blanks, 

and laboratory duplicates were analyzed appropriately 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 did not reanalyze the samples with a higher 

dilution factor because the percent recoveries 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 sample 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 was not qualified because there are no specific 

control limits for field duplicates specified in EPA method 410.4. 

The percent recoveries for the MS and 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 recoveries 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 similar matrix (FGD SBR influent and 

FGD SBR effluent) could be biased low. Samples 71848 and 71851 were qualified as 

minimum values. The LFB percent recoveries associated 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 LRB associated with samples 71844, 71847, 71848, 

71851, 71852, and 71853. These blank results were greater than the MDL (0.0020 mg/L), 

3 
but 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 calibration 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 further 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 recoveries of both the 

MS and MSD samples were outside of the laboratory control criteria of 90-110%. 

However, because there are no criteria for MS/MSD analyses specified in SM 4500 CNE 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 within the control limits specified by EPA method 353.2, the 

laboratory did not reanalyze the samples using a higher dilution factor. 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 sample was not qualified. The LFB associated 

with this sample met the method criteria. 

Phosphorus 

The percent recoveries for the MS/MSD analysis 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%. The percent recoveries of the 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). TestAmerica 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 

4 
was not qualified because there are no 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 increased 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 contains high concentrations 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 control limits, sample 71844 was qualified as an 

estimated value. 

TDS was detected above the MDL (4.7 mg/L), but below the 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 associated with sample 71841 was not within the 

method control limits of 90-110%, but was within the laboratory control limits of 77-

115%. The percent recoveries 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 analyses on sample 71851. The percent recoveries 

for the MS and MSD samples were 114% and 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 laboratory 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 laboratory 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. 

5 
6 

TSS 

One laboratory duplicate was analyzed per batch. 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 laboratory duplicate of sample 71854 was 18%. 

Because the laboratory duplicate RPD was greater 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 duplicate 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 % recovery 

below methodspecified criteria 

130 mg/L 

71851 COD Minimum Value MS % recovery 

below methodspecified criteria 

140 mg/L 

71841 Cyanide Estimated Value pH upon receipt < 

10 S.U. 

1.2 mg/L 

71844 TDS Estimated Value Lab duplicate 

RPD > methodspecified criteria 

11,000 mg/L 

71841 TKN Minimum Value LFB % recovery 

below methodspecified criteria 

130 mg/L 

71854 TSS Estimated Value Lab duplicate 

RPD > methodspecified criteria 

12 mg/L