Appendix B

DATA REVIEW NARRATIVES
1

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

Donna Tedder, ERG

Date: 9/1/2011

Subject: FGS Data Review Narrative for Total and Dissolved Mercury – Episode 6561

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 (CVAFS) analysis.

Table 1 summarizes the 37 samples (excluding laboratory filter blanks) FGS extracted 

and analyzed for total and dissolved mercury. 

Table 1. EPA Episode 6561 Total & Dissolved Mercury – Sample Identification

EPA 

Sample #

Lab Sample 

ID #

Sample 

Matrix Sample Description

Sampling 

Date

71791 1008018-01 Aqueous FGD Influent Day 1 8/2/2010

71791 1008018-02 Aqueous Dissolved FGD Influent, Day 1 8/2/2010

71792 1008031-13 Aqueous FGD Influent, Day 2 8/3/2010

71792 1008031-14 Aqueous Dissolved FGD Influent, Day 2 8/3/2010

71793 1008045-01 Aqueous FGD Influent, Day 3 8/4/2010

71793 1008045-02 Aqueous Dissolved FGD Influent, Day 3 8/4/2010

71794 1008062-01 Aqueous FGD Influent, Day 4 8/5/2010

71794 1008062-02 Aqueous Dissolved FGD Influent, Day 4 8/5/2010

71795 1008031-15 Aqueous FGD Bioreactor Influent, Day 1 8/3/2010

71795 1008031-16 Aqueous Dissolved FGD Bioreactor Influent, Day 2 8/3/2010

71796 1008045-03 Aqueous FGD Bioreactor Influent, Day 2 8/4/2010

71796 1008045-04 Aqueous Dissolved FGD Bioreactor Influent, Day 2 8/4/2010

71797 1008062-03 Aqueous FGD Bioreactor Influent, Day 3 8/5/2010

71797 1008062-04 Aqueous Dissolved FGD Bioreactor Influent, Day 3 8/5/2010

71798 1008072-03 Aqueous FGD Bioreactor Influent , Day 4 8/6/2010

71798 1008072-04 Aqueous Dissolved FGD Bioreactor Influent , Day 4 8/6/2010

71799 1008031-17 Aqueous FGD Bioreactor Effluent, Day 1 8/3/2010

71799 1008031-18 Aqueous Dissolved FGD Bioreactor Effluent, Day 1 8/3/2010

71800 1008045-05 Aqueous FGD Bioreactor Effluent, Day 2 8/4/2010
2

Table 1. EPA Episode 6561 Total & Dissolved Mercury – Sample Identification

EPA 

Sample #

Lab Sample 

ID #

Sample 

Matrix Sample Description

Sampling 

Date

71800 1008045-06 Aqueous Dissolved FGD Bioreactor Effluent, Day 2 8/4/2010

71801 1008062-05 Aqueous FGD Bioreactor Effluent, Day 3 8/5/2010

71801 1008062-06 Aqueous Dissolved FGD Bioreactor Effluent, Day 3 8/5/2010

71802 1008072-05 Aqueous FGD Bioreactor Effluent , Day 4 8/6/2010

71802 1008072-06 Aqueous Dissolved FGD Bioreactor Effluent , Day 4 8/6/2010

71803 1008062-07 Aqueous FGD Bioreactor Influent Duplicate 8/5/2010

71803 1008062-08 Aqueous Dissolved FGD Bioreactor Influent Duplicate 8/5/2010

71804 1008045-07 Aqueous FGD Bioreactor Effluent Duplicate, Day 2 8/4/2010

71804 1008045-08 Aqueous Dissolved FGD Bioreactor Effluent Duplicate, 

Day 2

8/4/2010

71805 1008018-03 Aqueous FGD Influent Field Blank, Day 1 8/2/2010

71806 1008018-06 Aqueous FGD Bioreactor Influent Field Blank, Day 1 8/2/2010

71807 1008031-19 Aqueous FGD Bioreactor Influent Field Blank, Day 2 8/3/2010

71808 1008045-15 Aqueous FGD Bioreactor Influent Field Blank, Day 3 8/4/2010

71809 1008062-13 Aqueous FGD Bioreactor Influent Field Blank, Day 4 8/5/2010

71810 1008018-09 Aqueous FGD Bioreactor Effluent Field Blank, Day 1 8/2/2010

71811 1008031-12 Aqueous FGD Bioreactor Effluent Field Blank, Day 2 8/3/2010

71812 1008045-16 Aqueous FGD Bioreactor Effluent Field Blank, Day 3 8/4/2010

71813 1008062-14 Aqueous FGD Bioreactor Effluent Field Blank, Day 4 8/5/2010

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.
3

BLANKS

All the preparation blanks or laboratory reagent blanks (LRBs) and the continuing 

calibration blanks (CCBs) met method-suggested criteria. Preparation Blanks F009001-

BLK2 and F009002-BLK4 had mercury levels of 0.10 and 0.27 ng/L, respectively, which 

are greater than the MDL, but less than the reporting limit. These blank results were 

appropriately fagged with a “J” qualifier.

DUPLICATES

Field duplicates, Sample 71804, were collected on Sample 71800. The 71800/71804

total mercury relative percent difference (RPD) was 10.4% and the dissolved mercury 

RPD was 1.8%. The method-suggested RPD criterion between field duplicates is 20%.

Laboratory duplicates were performed in this episode on samples 71795, 71796 and

71801. 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 (MS/MSD)

Matrix spikes (MS) and matrix spike duplicates (MSD) were performed on samples 

71796 and 71801 for the total mercury analyses. MS and MSDs were performed on 

samples 71791, 71795, 71801 & 71798 for the dissolved mercury analyses. All 

MS/MSD recoveries were within method specifications of 71-125%. All RPDs met 

method-specified criteria.

DETECTION LIMITS

The laboratory MDL in the synthetic matrix was 0.239 ng/L. Results below this MDL 

were reported as not detected (ND).
1

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

Donna Tedder, ERG

Date: 9/1/2011

Subject: TestAmerica Data Review Narrative for Total and Dissolved Metals by 200.8 –

Episode 6561

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

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

for Sample Episode 6561. The samples were analyzed according to EPA Method 200.8.

Table 1 summarizes the samples TestAmerica extracted and analyzed for total and 

dissolved metals by EPA Method 200.8.

Table 1. EPA Episode 6561 Total & Dissolved Metals – Sample Identification

EPA 

Sample # EPA Sample Description

Lab Sample 

ID #

Sample 

Matrix

Sampling 

Date

Receipt 

Date

71791 FGD Influent, Day 1 280-5932-1 Aqueous 8/2/2010 8/3/2010

71792 FGD Influent, Day 2 280-5964-1 Aqueous 8/3/2010 8/4/2010

71793 FGD Influent, Day 3 280-6008-1 Aqueous 8/4/2010 8/5/2010

71794 FGD Influent, Day 4 280-6067-4 Aqueous 8/5/2010 8/6/2010

71795 FGD Bioreactor Influent, Day 1 280-5964-2 Aqueous 8/3/2010 8/4/2010

71796 FGD Bioreactor Influent, Day 2 280-6008-2 Aqueous 8/4/2010 8/5/2010

71797 FGD Bioreactor Influent, Day 3 280-6067-1 Aqueous 8/5/2010 8/6/2010

71798 FGD Bioreactor Influent, Day 4 280-6117-1 Aqueous 8/6/2010 8/7/2010

71799 FGD Bioreactor Effluent, Day 1 280-5964-3 Aqueous 8/3/2010 8/4/2010

71800 FGD Bioreactor Effluent, Day 2 280-6008-3 Aqueous 8/4/2010 8/5/2010

71801 FGD Bioreactor Effluent, Day 3 280-6067-2 Aqueous 8/5/2010 8/6/2010

71802 FGD Bioreactor Effluent, Day 4 280-6117-2 Aqueous 8/6/2010 8/7/2010

71803 FGD Bioreactor Influent -

Duplicate, Day 3

280-6067-3 Aqueous 8/5/2010 8/6/2010

71804 FGD Bioreactor Effluent -

Duplicate, Day 2

280-6008-4 Aqueous 8/4/2010 8/5/2010

71805 FGD Influent Field Blank, Day 

1

280-5932-2 Aqueous 8/2/2010 8/3/2010

71806 FGD Bioreactor Influent Field 

Blank, Day 1

280-5964-4 Aqueous 8/3/2010 8/4/2010
2

Table 1. EPA Episode 6561 Total & Dissolved Metals – Sample Identification

EPA 

Sample # EPA Sample Description

Lab Sample 

ID #

Sample 

Matrix

Sampling 

Date

Receipt 

Date

71810 FGD Bioreactor Effluent Field 

Blank, Day 1

280-5964-5 Aqueous 8/3/2010 8/4/2010

SUMMARY

The samples were prepared for total and dissolved metals analysis according to 

TestAmerica’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.

There were no findings from the data review that required additional qualifiers (excluding 

those identified by the laboratory) in this dataset.

INTERNAL STANDARDIZATION

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

INITIAL CALIBRATION

TestAmerica 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.

BLANKS

All the method blanks were less than the reporting limit (RL). No additional qualifiers 

were required for method blanks.

All instrument blanks (initial calibration blank (ICB) and continuing calibration blank 

(CCB)) were less than the RL; however, antimony was above the instrument detection 

limit (IDL) in one ICB and was flagged with the “J” qualifier.

REPORTING LIMIT VERIFICATION STANDARD (CRI)

All CRI samples passed TestAmerica’s 50–150% recovery limits.
3

LABORATORY CONTROL SAMPLES (LCS)

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

SYNTHETIC FGD INTERFERENCE CHECK SOLUTION

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

The serial dilution performed for the total and dissolved sample 71799 FGD Bioreactor 

Effluent, Day 1 (280-5964-3) met TestAmerica’s criteria of ±10% difference.

FIELD DUPLICATES

The relative percent difference (RPD) of the field duplicates 71800/71804 and 

71797/71803 were less than 20% for all values greater than the reporting limit. None of 

the total or dissolved analytes in parent sample 71800 and field duplicate sample 71804

were above the RL so the RPD could not be accurately determined. The RPD for all total 

and dissolved analytes above the reporting limit in parent sample 71797 and field 

duplicate sample 71803 were less than TestAmerica’s ±20% requirement. 

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

Matrix spikes (MS) and matrix spike duplicates (MSD) were performed on samples 

71799, 71801 and 71798. Many spike recoveries were outside the method control limits 

of 70–130% when sample concentrations exceeded the spike concentration by a factor of 

four or more, which have been flagged with a “4” qualifier indicating concentrations in 

the parent samples were greater than four times the spike amounts. Otherwise, all 

MS/MSD spike recoveries were within the method control limits of 70-130%. In 

addition, the RPD for all MS/MSD passed the method-specified criteria of 20 percent.

POST DIGESITON SPIKES

The post digestion spike performed on sample 71799 FGD Bioreactor Effluent, Day 1 

(280-5964-3) for total and dissolved analytes passed TestAmerica’s 85–115% control 

limits.
4

DETECTION LIMITS

The laboratory performed an MDL study in the synthetic FGD wastewater matrix, instead 

of reagent water.
1

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

Donna Tedder, ERG

Date: 9/1/2011

Subject: TestAmerica Data Review Narrative for Total and Dissolved Metals by 200.7 –

Episode 6561

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

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

tin, titanium, and zinc) for Sample Episode 6561. The samples were analyzed according 

to EPA Method 200.7.

Table 1 summarizes the samples TestAmerica extracted and analyzed for total and 

dissolved metals by EPA Method 200.7.

Table 1. EPA Episode 6561 Total & Dissolved Metals – Sample Identification

EPA 

Sample # EPA Sample Description

Lab Sample 

ID #

Sample 

Matrix

Sampling 

Date

Receipt 

Date

71791 FGD Influent, Day 1 280-5932-1 Aqueous 8/2/2010 8/3/2010

71792 FGD Influent, Day 2 280-5964-1 Aqueous 8/3/2010 8/4/2010

71793 FGD Influent, Day 3 280-6008-1 Aqueous 8/4/2010 8/5/2010

71794 FGD Influent, Day 4 280-6067-4 Aqueous 8/5/2010 8/6/2010

71795 FGD Bioreactor Influent, Day 1 280-5964-2 Aqueous 8/3/2010 8/4/2010

71796 FGD Bioreactor Influent, Day 2 280-6008-2 Aqueous 8/4/2010 8/5/2010

71797 FGD Bioreactor Influent, Day 3 280-6067-1 Aqueous 8/5/2010 8/6/2010

71798 FGD Bioreactor Influent, Day 4 280-6117-1 Aqueous 8/6/2010 8/7/2010

71799 FGD Bioreactor Effluent, Day 1 280-5964-3 Aqueous 8/3/2010 8/4/2010

71800 FGD Bioreactor Effluent, Day 2 280-6008-3 Aqueous 8/4/2010 8/5/2010

71801 FGD Bioreactor Effluent, Day 3 280-6067-2 Aqueous 8/5/2010 8/6/2010

71802 FGD Bioreactor Effluent, Day 4 280-6117-2 Aqueous 8/6/2010 8/7/2010

71803 FGD Bioreactor Influent -

Duplicate, Day 3

280-6067-3 Aqueous 8/5/2010 8/6/2010

71804 FGD Bioreactor Effluent -

Duplicate, Day 2

280-6008-4 Aqueous 8/4/2010 8/5/2010

71805 FGD Influent Field Blank, Day 1 280-5932-2 Aqueous 8/2/2010 8/3/2010
2

Table 1. EPA Episode 6561 Total & Dissolved Metals – Sample Identification

EPA 

Sample # EPA Sample Description

Lab Sample 

ID #

Sample 

Matrix

Sampling 

Date

Receipt 

Date

71806 FGD Bioreactor Influent Field 

Blank, Day 1

280-5964-4 Aqueous 8/3/2010 8/4/2010

71810 FGD Bioreactor Effluent Field 

Blank, Day 1

280-5964-5 Aqueous 8/3/2010 8/4/2010

SUMMARY

The samples were prepared for total and dissolved metals analysis according to 

TestAmerica’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

TestAmerica 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 (RL); however, some elements

had levels greater than the method detection limit (MDL) and were flagged with the “J” 

qualifier.

All instrument blanks (initial calibration blank (ICB) and continuing calibration blank

(CCB)) were less than the RL; however, some elements had levels greater than the MDL

and were flagged with the “J” qualifier.
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 

recoveries met the method-specified criteria.

SERIAL DILUTION

Serial dilutions were performed for each batch of total and dissolved samples. All serial 

dilution percent differences were less than 10% as required by TestAmerica’s SOP.

REPORTING LIMIT VERIFICATION STANDARD (CRI)

All CRI samples passed TestAmerica’s control limits of 50–150%.

FIELD DUPLICATES

The relative percent difference (RPD) of the field duplicates 71800/71804 and 

71797/71803 were less than 20% for all total and dissolved values greater than the RL.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

Matrix spikes (MS) and matrix spike duplicates (MSD) were performed on the total and 

dissolved samples of 71798, 71799 and 71801. Many spike recoveries were outside the 

method control limits of 70-130% when sample concentrations exceeded the spike 

concentrations by a factor of four or more, which have been flagged with a “4” qualifier 

indicating concentrations in the parent samples were greater than four times the spike 

amounts. Otherwise, all MS/MSD spike recoveries were within the 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% requirement.

POST DIGESTION SPIKE

The post digestion spike performed on sample 71799 FGD Bioreactor Effluent, Day1 

passed TestAmerica’s control limits of 85-115% recovery for all total and dissolved 

analytes except total sodium and dissolved manganese. The post digestion spike 

performed on sample 71798 FGD Bioreactor Influent, Day 4 passed TestAmerica’s 

control limits of 85-115% recovery for all total and dissolved analytes except total 

sodium. 
4

DETECTION LIMITS

The laboratory performed an MDL study in the synthetic FGD wastewater matrix, instead 

of reagent water.
1

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 

6561

Frontier Global Sciences (FGS) generated analytical data for dissolved hexavalent 

chromium for Sample Episode 6561. 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 6561 Dissolved Hexavalent Chromium – Sample Identification

EPA 

Sample 

#

Sample 

Matrix Sample Description

Sampling 

Date Analysis Date

71791 Aqueous FGD Influent Day 1 8/2/10 8/9/10

71792 Aqueous FGD Influent Day 2 8/3/10 8/9/10

71793 Aqueous FGD Influent Day 3 8/4/10 8/9/10

71794 Aqueous FGD Influent Day 4 8/5/10 8/30/10

71795 Aqueous FGD Bioreactor Influent Day 1 8/3/10 8/9/10

71796 Aqueous FGD Bioreactor Influent Day 2 8/4/10 8/9/10

71797 Aqueous FGD Bioreactor Influent Day 3 8/5/10 8/30/10

71798 Aqueous FGD Bioreactor Influent Day 4 8/6/10 8/30/10

71799 Aqueous FGD Bioreactor Effluent Day 1 8/3/10 8/9/10

71800 Aqueous FGD Bioreactor Effluent Day 2 8/4/10 8/30/10

71801 Aqueous FGD Bioreactor Effluent Day 3 8/5/10 8/30/10

71802 Aqueous FGD Bioreactor Effluent Day 4 8/6/10 8/30/10

71803 Aqueous FGD Bioreactor Influent Dup Day 3 8/5/10 8/30/10

71804 Aqueous FGD Bioreactor Effluent Dup Day 2 8/4/10 8/30/10

71805 Aqueous FGD Influent Field Blank Day 1 8/2/10 8/9/10

71806 Aqueous FGD Bioreactor Influent Field Blank Day 1 8/3/10 8/9/10

71810 Aqueous FGD Bioreactor Effluent Field Blank Day 1 8/3/10 8/9/10
2

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 (71791, 71792, 71793, 71794, 71795, 71796, 71797, 71798, and 71803)

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 109%.

BLANK

All of the preparation blanks/laboratory reagent blanks (LRBs) and the continuing 

calibration blanks (CCBs) met method-specified requirements. 
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 102% and 102%. A second set of LFB/LFBD, for the later analysis date,

had recoveries of 100% and 99.3%. 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 71803 was a duplicate of 

sample 71797. These samples were nondetects (NDs), indicating the analyte was not 

detected at or above the method detection limit. Sample 71804 was a duplicate of sample 

71800. 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 71791 and 71801. All MS/MSD recoveries were within 75%-125%, 

with RPDs of 1.47% and 4.44%, respectively.
1

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 6561

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry 

analyses for Sample Episode 6561. 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 6561 Classical Analytes – Sample Identification

EPA

Sample #

Sample

Matrix Sample Description

Sampling

Date

71791 Water FGD Influent, Day 1 8/2/10

71792 Water FGD Influent, Day 2 8/3/10

71793 Water FGD Influent, Day 3 8/4/10

71794 Water FGD Influent, Day 4 8/5/10

71795 Water FGD Bioreactor Influent, Day 1 8/3/10

71796 Water FGD Bioreactor Influent, Day 2 8/4/10

71797 Water FGD Bioreactor Influent, Day 3 8/5/10

71798 Water FGD Bioreactor Influent, Day 4 8/6/10

71799 Water FGD Bioreactor Effluent, Day 1 8/3/10

71800 Water FGD Bioreactor Effluent, Day 2 8/4/10

71801 Water FGD Bioreactor Effluent, Day 3 8/5/10
2

Table 1. EPA Episode 6561 Classical Analytes – Sample Identification

EPA

Sample #

Sample

Matrix Sample Description

Sampling

Date

71802 Water FGD Bioreactor Effluent, Day 4 8/6/10

71803 Water FGD Bioreactor Influent - Duplicate 8/5/10

71804 Water FGD Bioreactor Effluent - Duplicate 8/4/10

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 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. Two MS samples 

were run on samples 71798 (FGD bioreactor influent) and 71801 (FGD bioreactor 

effluent) for each analyte to check for matrix interferences in these matrices. 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 percent recoveries for the MS and MSD analysis for sample 71799 (FGD bioreactor 

effluent) were 112% and 116%, respectively, which are above the laboratory and method 

control limits of 90-110%. Sample 71799 was qualified as a maximum value. The LFB 

associated with this sample met the method criteria.
3

BOD5

Even though TestAmerica ran five dilutions on sample 71801, no dilutions had a 

dissolved oxygen (DO) depletion greater than 2.0 mg/L. Therefore, BOD5 was reported 

as not detected for this sample.

All glucose-glutamic acid standards and laboratory duplicates were analyzed 

appropriately and met the criteria specified in SM 5210B. BOD was not detected above 

the RL in any method blank; however, for batch 25403, the results for the three 

water/unseeded blanks were 0.24 mg/L, 0.21 mg/L, and 0.21 mg/L. All of these results 

were greater than the method control criteria of 0.20 mg/L. Because of these detections in 

the water/unseeded blanks, samples 71791, 71792, 71795, and 71799 were qualified with 

a “B” meaning the analyte was found in the sample and the blank. 

Chloride and Sulfate

The MS/MSD results of samples 71798 and 71801 for sulfate 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/MSD results will be qualified as estimated values.

COD

The percent recovery of the LFB associated with batch 25742 was 88.9%, which was less 

than the method control criteria of 90-110%, but did meet the historical laboratory criteria 

of 80-115%. The LFBD percent recovery (96.7%) did meet the method criteria. Because 

the laboratory originally had analyzed the percent recovery against the historical criteria, 

this LFB failure was not noted until after the hold time had expired, so the samples were 

not reanalyzed. The laboratory qualified these samples with a “*” indicating that the 

LFB or LFBD was not within the control limits. Samples 71792, 71795, and 71799 were 

already qualified by the laboratory with a “J” meaning the sample result was an estimated

value because it was less than the RL, so no further action was taken.

Samples 71795 and 71801 were diluted by 10 fold because of matrix interferences 

determined by the chloride prescreening. The diluted results were below the lowest

calibration standard; however, these samples were already qualified by the laboratory 

with a “J” meaning the sample result was an estimated value because it was less than the 

RL, so no further action was taken.

The RPD between sample 71797 and its field duplicate 71803 was 26.5% and the RPD 

between sample 71800 and its field duplicate 71804 was 35.8%. 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 EPA method 410.4.
4

The percent recoveries for the MS/MSD analysis for sample 71798 (FGD bioreactor 

influent) and for the MS analysis for sample 71801 (FGD bioreactor 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 71798 were 75% and 77%, respectively, and the 

percent recoveries for the MS and MSD analyses for sample 71801 were 89% and 96%,

respectively. The LFB associated with these samples met the method criteria. Sample 

71798 was qualified as a minimum value. Results for samples with a similar matrix (i.e., 

FGD bioreactor influent) could also be biased low. Sample 71801 was already qualified 

by the laboratory with a “J” meaning the sample result was an estimated value because it 

was less than the RL; therefore, this sample was not additionally qualified as a minimum 

value.

Cyanide 

Cyanide was detected at 0.00240 mg/L in the method blank associated with samples 

71794, 71797, 71798, 71801, 71802, and 71803. Although this concentration is greater 

than the MDL (0.0020 mg/L), it is lower than the RL (0.010 mg/L). Because the blank 

result was less than the RL, no samples were qualified based on the LRB result.

The RPD between sample 71800 and its field duplicate 71804 was 21.1%. 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.

All samples were diluted prior to distillation by a factor of 10 due to matrix interferences.

The laboratory stated that the samples foamed during preparation and in order to protect 

the instruments, the samples needed to be diluted. The results of the diluted sample for 

71795, 71796, and 71804 were below the lowest calibration standard used by the 

laboratory (0.01 mg/L). However, these samples were already qualified by the laboratory 

with a “J” meaning the sample result was an estimated value because it was less than the 

RL, so no further action was taken.

Nitrate/Nitrite

The result for sample 71799 was below the lowest calibration standard. However, this 

sample was already qualified by the laboratory with a “J” meaning the sample result was 

an estimated value because it was less than the RL, so no further action was taken.

The percent recovery for the MS analysis for sample 71798 (FGD bioreactor influent) 

was below the control limits of 90-110% required by the method and below the 

laboratory control limits of 72-113%. The percent recoveries of the MS and MSD 

samples were 70% and 102%, respectively. TestAmerica qualified both the MS and MSD 

results for sample 71798 with an “E” meaning that the results exceeded the calibration 

range. The MSD sample result was above the highest calibration standard and even 

though the MS sample result was within the calibration range, it was expected to be 

above the highest calibration standard. If the MSD result is reported, it will be qualified 

as an estimated value because the result was above the highest calibration standard.
5

The MS percent recovery for sample 71799 (FGD bioreactor effluent) was not within the 

method control limits, but was within the laboratory control limits. The percent 

recoveries of the MS and MSD samples were 112% and 107%, respectively. Sample 

71799 was already qualified by the laboratory with a “J” meaning the sample result was 

an estimated value because it was less than the RL, so there was no need to further 

qualify the result as a maximum value. 

Phosphorus 

The results for Samples 71792, 71793, and 71798 were less than the lowest calibration 

standard (0.025 mg/L). However, these samples were already qualified by the laboratory

with a “J” meaning the sample result was an estimated value because it was less than the 

RL, so no further action was taken.

The percent recoveries for the MS and MSD analyses for samples 71798 and 71801 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 for MS and MSD 

analyses on sample 71798 were both 73% and the percent recoveries for MS and MSD 

analyses on sample 71801 were both 74%. The results may be biased low for samples 

with similar matrixes (i.e., FGD bioreactor influent and FGD bioreactor effluent) because 

of matrix interferences. Sample 71801 was qualified as a minimum value because the MS 

percent recovery was below the method specified criteria. Sample 71798 was already 

qualified by the laboratory with a “J” meaning the sample result was an estimated value 

because it was less than the RL, so there was no need to further qualify the result as a 

minimum value. 

The RPD between sample 71797 and its field duplicate 71803 for phosphorus was 25.8%. 

The results for these samples were greater than the MDL, but less than the RL. These low 

concentrations might be the reason for the high RPD. 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 365.1.

TDS

Constant weight was not achieved after 3 drying cycles for samples 71791, 71795, 71796, 

71797, 71798, 71799, 71800, 71801, 71802, 71803, and 71804. For samples 71791, 

71795, 71796, 71797, 71798, 71799, 71800, 71801, and 71803 the weight increased from 

the first weighing to the second weighing. 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.

At least one laboratory duplicate was analyzed per batch. The RPDs for all laboratory 

duplicates analyzed were less than 10% as required by SM 2540C. 
6

TKN

The percent recoveries for the MS and MSD analyses for sample 71798 (Bioreactor

influent) did not meet the method control limits of 90%-110% or the laboratory criteria of 

54%-131%. The MS and MSD percent recoveries were 202% and 206%, respectively. 

The LFB associated with this sample met the method criteria. These percent recoveries 

suggest that results could be biased high for samples with a similar matrix (i.e., bioreactor 

influent). Sample 71798 was qualified as a maximum value.

TSS 

At least one laboratory duplicate was analyzed per batch. The RPDs for laboratory 

duplicates for samples 71791, 71792, 71794, and 71798 were less than 10% as required 

by Method SM2540D. However, the RPD for sample 71801 was 15%. The results for 

sample 71801 and its laboratory duplicate were both qualified by the laboratory with a 

“J” meaning the sample result was an estimated value because it was less than the RL, so 

sample 71801 was not additionally qualified. 

The RPD between sample 71797 and its field duplicate 71803 was 28.6%. The RPD 

between sample 71800 and its field duplicate 71804 was also 28.6%. The results for these 

four samples were less than the reporting limit. These low concentrations could have 

caused the high RPDs. 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

71799 Ammonia Maximum Value MS % recovery 

above methodspecified criteria

13 mg/L

71791 BOD B Unseeded water 

blank > methodspecified criteria

40 mg/L

71792 BOD B Unseeded water 

blank > methodspecified criteria

9.7 mg/L

71795 BOD B Unseeded water 

blank > methodspecified criteria

7.4 mg/L

71799 BOD B Unseeded water 

blank > methodspecified criteria

1.7 mg/L
7

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level Detected

71798 COD Minimum Value MS % recovery 

below methodspecified criteria

84 mg/L

71798 Nitrate/Nitrite Minimum Value MS % recovery 

below methodspecified criteria

13 mg/L

71801 Total 

Phosphorus

Minimum Value MS % recovery 

below methodspecified criteria

0.19 mg/L

71798 TKN Maximum Value MS % recovery 

above methodspecified criteria

3.2 mg/L