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: Donna Tedder, ERG

Laura Aviles-Alvarez, ERG

Date: 9/1/2011

Subject: FGS Data Review Narrative for Total and Dissolved Mercury – Episode 6563

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 23 samples (excluding laboratory filter blanks) FGS extracted 

and analyzed for total and dissolved mercury.

Table 1. EPA Episode 6563 Total & Dissolved Mercury – Sample Identification

EPA 

Sample #

Lab Sample 

ID #

Sample 

Matrix Sample Description

Sampling 

Date

71891 1009100-03 Aqueous FGD Influent Day 1 9/13/2010

71891 1009100-04 Aqueous Dissolved FGD Influent, Day 1 9/13/2010

71892 1009111-08 Aqueous FGD Influent, Day 2 9/14/2010

71892 1009111-09 Aqueous Dissolved FGD Influent, Day 2 9/14/2010

71893 1009128-04 Aqueous FGD Influent, Day 3 9/15/2010

71893 1009128-05 Aqueous Dissolved FGD Influent, Day 3 9/15/2010

71894 1009134-03 Aqueous FGD Influent, Day 4 9/16/2010

71894 1009134-04 Aqueous Dissolved FGD Influent, Day 4 9/16/2010

71895 1009111-10 Aqueous FGD Effluent Day 1 9/14/2010

71895 1009111-11 Aqueous Dissolved FGD Effluent, Day 1 9/14/2010

71896 1009128-06 Aqueous FGD Effluent, Day 2 9/15/2010

71896 1009128-07 Aqueous Dissolved FGD Effluent, Day 2 9/15/2010

71897 1009134-05 Aqueous FGD Effluent, Day 3 9/16/2010

71897 1009134-06 Aqueous Dissolved FGD Effluent, Day 3 9/16/2010

71898 1009141-02 Aqueous FGD Effluent, Day 4 9/17/2010

71898 1009141-03 Aqueous Dissolved FGD Effluent, Day 4 9/17/2010

71899 1009128-08 Aqueous FGD Effluent Duplicate, Day 2 9/15/2010

71899 1009128-09 Aqueous Dissolved FGD Effluent Duplicate, Day 2 9/15/2010

71900 1009100-05 Aqueous FGD Influent Field Blank, Day 1 9/13/2010
2

Table 1. EPA Episode 6563 Total & Dissolved Mercury – Sample Identification

EPA 

Sample #

Lab Sample 

ID #

Sample 

Matrix Sample Description

Sampling 

Date

71901 1009100-08 Aqueous FGD Effluent Field Blank, Day 1 9/13/2010

71902 1009111-12 Aqueous FGD Effluent Field Blank, Day 2 9/14/2010

71903 1009128-12 Aqueous FGD Effluent Field Blank, Day 3 9/15/2010

71904 1009134-07 Aqueous FGD Effluent Field Blank, Day 4 9/16/2010

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.

BLANKS

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

calibration blanks (CCBs) met method-specified criteria. Preparation Blanks F010073-

BLK5, F010073-BLK6, F010122-BLK6, F010122–BLK7, and F010123-BLK5 had 

mercury levels of 0.45, 0.29, 0.16, 0.13, and 0.09 ng/L, respectively. These blank results

were greater than the MDL (0.08 ng/L), but less than the RL (0.50 ng/L). Because all of 

the blank results were less than the RL, no samples were qualified based on these 

preparation blank results.

DUPLICATES

A field duplicate, Sample 71899, was collected on the Sample 71896. The total mercury 

relative percent difference (RPD) was 4.65% and the dissolved mercury RPD was 

12.46%. The method-suggested RPD criteria between field duplicates is 20%.
3

Laboratory duplicates were performed in this episode on samples 71891 and 71896. All 

RPDs were less than 20% (the method-suggested RPD criterion between field duplicates; 

the method does not require the analysis of laboratory duplicates).

LABORATORY CONTROL SAMPLES

All laboratory control samples were within Frontier’s control limits of 80-120% recovery

and 24% RPD, except F010073-BS3 (blank spike (BS)), which had a recovery of 121% 

recovery. Because this recovery does meet the ongoing precision and recovery (OPR)

criteria, and because the other BS samples and all initial and continuing calibration 

verification samples in this batch met method criteria, there was no need to qualify any 

data based on this BS failure.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES (MS/MSD)

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

71891, 71896, and 71897 for the total mercury analyses. MS and MSDs were performed 

on sample 71897 for the dissolved mercury analyses. All aqueous 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

Date: 9/1/2011

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

Episode 6563

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

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

Sample Episode 6563. 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 6563 Total & Dissolved Metals – Sample Identification

EPA 

Sample 

#

EPA Sample Description Lab Sample 

ID #

Sample 

Matrix

Sampling 

Date

Receipt 

Date

71891 FGD Influent, Day 1 280-7312-1 Aqueous 9/13/2010 9/14/2010

71891 FGD Influent, Day 1 – Solid 280-7312-3 Solid 9/13/2010 9/14/2010

71891 FGD Influent, Day 1 - Filtrate 280-7312-4 Aqueous 9/13/2010 9/14/2010

71892 FGD Influent, Day 2 280-7362-1 Aqueous 9/14/2010 9/15/2010

71892 FGD Influent, Day 2 – Solid 280-7362-4 Solid 9/14/2010 9/15/2010

71892 FGD Influent, Day 2 – Filtrate 280-7362-5 Aqueous 9/14/2010 9/15/2010

71893 FGD Influent, Day 3 280-7401-1 Aqueous 9/15/2010 9/16/2010

71893 FGD Influent, Day 3 – Solid 280-7401-4 Solid 9/15/2010 9/16/2010

71893 FGD Influent, Day 3 – Filtrate 280-7401-5 Aqueous 9/15/2010 9/16/2010

71894 FGD Influent, Day 4 280-7482-1 Aqueous 9/16/2010 9/17/2010

71894 FGD Influent, Day 4 – Solid 280-7482-3 Solid 9/16/2010 9/17/2010

71894 FGD Influent, Day 4 - Filtrate 280-7482-4 Aqueous 9/16/2010 9/17/2010

71895 FGD Effluent, Day 1 280-7362-2 Aqueous 9/14/2010 9/15/2010

71896 FGD Effluent, Day 2 280-7401-2 Aqueous 9/15/2010 9/16/2010

71897 FGD Effluent, Day 3 280-7482-2 Aqueous 9/16/2010 9/17/2010

71898 FGD Effluent, Day 4 280-7536-1 Aqueous 9/17/2010 9/18/2010

71899 FGD Effluent, Day 2 -

Duplicate

280-7401-3 Aqueous 9/15/2010 9/16/2010
2

Table 1. EPA Episode 6563 Total & Dissolved Metals – Sample Identification

EPA 

Sample 

#

EPA Sample Description Lab Sample 

ID #

Sample 

Matrix

Sampling 

Date

Receipt 

Date

71900 FGD Influent Field Blank, 

Day 1

280-7312-2 Aqueous 9/13/2010 9/14/2010

71901 FGD Effluent Field Blank, 

Day 1

280-7362-3 Aqueous 9/14/2010 9/15/2010

SUMMARY

The samples were prepared for total and dissolved metals analysis according 

TestAmerica’s “FGD ICP/MS SOP: Inductively Coupled Plasma Mass Spectrometry for 

Trace Element 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.

• The serial dilution analysis for thallium in the solid phase of sample 71891 did not 

meet TestAmerica’s requirement of ±10% difference.

• The serial dilution analysis for total nickel in the filtrate phase of sample 71891 

did not meet TestAmerica’s requirement of ±10% difference.

• All matrix spike (MS)/matrix spike duplicates (MSD) for total and dissolved 

silver failed the 70–130% control limits, except for dissolved silver in the MS for 

sample 71897.

• All the MS/MSD RPDs for silver failed TestAmerica’s SOP control limits of 

±20%. 

• The MS/MSD RPD for total selenium for sample 71898 failed TestAmerica’s 

SOP control limits of ±20%.

• The post digestion spikes (PDS) for selenium in the solid phase for sample 71891 

failed the method criteria of 85–115%.

• The PDS for silver failed the method criteria of 85-115% for several samples.

INTERNAL STANDARDIZATION

All internal standards used by TestAmerica were within the method criteria. 
3

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; however, some elements were 

above the MDL and flagged with a “J” qualifier. No additional qualifiers were required 

for method blanks.

All instrument blanks (ICB and CCB) were less than the reporting limit; however, some 

elements were above the MDL and flagged with a “J” qualifier. No additional qualifiers 

were required for instrument blanks.

REPORTING LIMIT VERIFICATION STANDARD (CRI)

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

LABORATORY CONTROL SAMPLES (LCS)

All LCS samples passed the method limits of 85–115%, with the exception of selenium 

in the solid sample LCS 280-34676/2-A at 84%; however, TestAmerica had a control 

limit set at 78–108%. No data was qualified based on this LCS.

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 (SRD)

The serial dilution performed for solid sample 71891 FGD Influent, Day 1 - Solid (280-

7312-3) failed Test America’s requirement of ±10% difference for thallium and was 

flagged “W”. The serial dilution performed for sample 71891 FGD Influent, Day 1 -
4

Filtrate (280-7312-4) failed Test America’s requirement of ±10% difference for nickel 

and was flagged “W”. All other elements passed Test America’s requirement of ±10% 

difference in the serial dilutions and required no further qualifiers.

FIELD DUPLICATES

The relative percent difference (RPD) of the field duplicates (71896/71899) were less

than ±20% for all values equal to or greater than the reporting limit.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

MS and MSD were performed on Samples 71897 and 71898. 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 “4”. All 

MS/MSDs for total and dissolved silver failed the 70–130% method control limits with 

the exception of the dissolved silver in sample 71897 FGD Effluent, Day 3 MS. All the 

MS/MSD RPDs for silver failed TestAmerica’s SOP control limits of ±20%. The poor 

recoveries and RPD of silver are probably due to high sulfates in this episode’s samples 

that could form insoluble silver sulfide and/or silver sulfate. All other RPD results were 

less than the method required 20% with the exception of selenium for MSD sample 

71898 FGD Effluent, Day 4 (280-7536-1 MSD), which was 25%.

POST DIGESITON SPIKES

The PDS performed on solid sample 71891 FGD Influent, Day 1 - Solid (280-7312-3

PDS) failed Test America’s 75–125% control limits for selenium, which was flagged 

“W”. Silver failed Test America’s 85-115% control limits for the following samples: 

• Total silver for 71891 FGD Influent, Day 1 – Filtrate (280-7312-4 PDS);

• Total silver for 71897 FGD Effluent, Day 3 (280-7482-2 PDS);

• Dissolved silver for 71897 FGD Effluent, Day 3 (280-7482-2 PDS); and

• Dissolved silver for 71898 FGD Effluent, Day 4 (280-7536-1 PDS).

Each of these samples were flagged “W”. The poor recoveries of silver are probably due 

to high sulfates in this episode’s samples that could form insoluble silver sulfide and/or 

silver sulfate. Sample 71897 FGD Effluent, Day 3 (280-7482-2 PDS) also failed Test 

America’s 85-115% control limits for total selenium, and dissolved vanadium which 

were both flagged “W”. No additional qualifiers were required for PDS samples.

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

Date: 9/1/2011

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

Episode 6563

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) for Sample Episode 6563. 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 6563 Total & Dissolved Metals – Sample Identification

EPA 

Sample # EPA Sample Description

Lab Sample 

ID #

Sample 

Matrix

Sampling 

Date

Receipt 

Date

71891 FGD Influent, Day 1 280-7312-1 Aqueous 9/13/2010 9/14/2010

71891 FGD Influent, Day 1 - Solids 280-7312-3 Solid 9/13/2010 9/14/2010

71891 FGD Influent, Day 1 - Filtrate 280-7312-4 Aqueous 9/13/2010 9/14/2010

71892 FGD Influent, Day 2 280-7362-1 Aqueous 9/14/2010 9/15/2010

71892 FGD Influent, Day 2 – Solids 280-7362-4 Solid 9/14/2010 9/15/2010

71892 FGD Influent, Day 2 – Filtrate 280-7362-5 Aqueous 9/14/2010 9/15/2010

71893 FGD Influent, Day 3 280-7401-1 Aqueous 9/15/2010 9/16/2010

71893 FGD Influent, Day 3 – Solids 280-7401-4 Solid 9/15/2010 9/16/2010

71893 FGD Influent, Day 3 – Filtrate 280-7401-5 Aqueous 9/15/2010 9/16/2010

71894 FGD Influent, Day 4 280-7482-1 Aqueous 9/16/2010 9/17/2010

71894 FGD Influent, Day 4 – Solids 280-7482-3 Solid 9/16/2010 9/17/2010

71894 FGD Influent, Day 4 - Filtrate 280-7482-4 Aqueous 9/16/2010 9/17/2010

71895 FGD Effluent, Day 1 280-7362-2 Aqueous 9/14/2010 9/15/2010

71896 FGD Effluent, Day 2 280-7401-2 Aqueous 9/15/2010 9/16/2010

71897 FGD Effluent, Day 3 280-7482-2 Aqueous 9/16/2010 9/17/2010

71898 FGD Effluent, Day 4 280-7536-1 Aqueous 9/17/2010 9/18/2010

71899 FGD Effluent, Day 2 - Duplicate 280-7401-3 Aqueous 9/15/2010 9/16/2010
2

Table 1. EPA Episode 6563 Total & Dissolved Metals – Sample Identification

EPA 

Sample # EPA Sample Description

Lab Sample 

ID #

Sample 

Matrix

Sampling 

Date

Receipt 

Date

71900 FGD Influent Field Blank, Day 1 280-7312-2 Aqueous 9/13/2010 9/14/2010

71901 FGD Effluent Field Blank, Day 1 280-7362-3 Aqueous 9/14/2010 9/15/2010

SUMMARY

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

TestAmerica’s SOP for ECP Analysis for Trace Metals by Method 200.7. Any significant 

findings are summarized below. No additional qualifiers were required.

The post digestion spikes (PDS) for total barium, total calcium, and total zinc in the 

filtrate phase for sample 71891 failed the method criteria of 85–115%.

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; 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.
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 duplicate (71899) 

to parent sample (71896) 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 71897 and 71898. 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 PDS samples performed passed the method criteria of 85–115%, 

with the exception of barium, calcium and zinc in the filtrate for sample 71891 FGD 

Influent, Day 1 (280-7312-4 PDS).

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

Laura Aviles-Alvarez, ERG

Date: 9/1/2011

Subject: FGS Data Review Narrative for Dissolved Hexavalent Chromium – Episode 

6563

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

chromium for Sample Episode 6563. 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 6563 Dissolved Hexavalent Chromium–Sample Identification

EPA 

Sample 

#

Sample 

Matrix Sample Description

Sampling 

Date Analysis Date

71891 Aqueous FGD Influent Day 1 9/13/10 10/11/10

71892 Aqueous FGD Influent Day 2 9/14/10 10/11/10

71893 Aqueous FGD Influent Day 3 9/15/10 10/12/10

71894 Aqueous FGD Influent Day 4 9/16/10 10/12/10

71895 Aqueous FGD Effluent Day 1 9/14/10 10/12/10

71896 Aqueous FGD Effluent Day 2 9/15/10 10/12/10

71897 Aqueous FGD Effluent Day 3 9/16/10 10/12/10

71898 Aqueous FGD Effluent Day 4 9/17/10 10/12/10

71899 Aqueous FGD Effluent Dup Day 2 9/15/10 10/12/10

71900 Aqueous FGD Influent Field Blank Day 1 9/13/10 10/11/10

71901 Aqueous FGD Effluent Field Blank Day 1 9/14/10 10/11/10

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.
2

Several samples (71891, 71892, 71893, 71894, 71895, 71896, 71897, 71898, and 71899)

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 within the ± 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 94.9 to 95.5%.

BLANK

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

calibration blanks (CCBs) met method-specified requirements. 

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 101% and 102%. The method suggested that a second source quality 
3

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). 

One field duplicate was collected and analyzed. Sample 71899 was a duplicate of 

effluent sample 71896. These samples were nondetects (NDs), indicating the analyte was 

not detected at or above the method detection limit.

MATRIX SPIKE AND MATIX SPIKE DUPLICATES

The MS and matrix spike duplicate (MSD) were performed using a secondary source 

spike on samples 71891 and 71897. All MS/MSD recoveries with within 75%-125%, 

with RPDs of 2.63% and 1.88%, 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 6563

TestAmerica Denver Laboratory generated analytical data for classical wet chemistry 

analyses for Sample Episode 6563. 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.

The TSS concentration of the influent samples was greater than one percent, so as 

requested, the laboratory separated the solid and liquid portions of the samples and 

analyzed both portions separately for the following analytes: 

• Ammonia, 

• Chloride,

• Cyanide, 

• Nitrate/Nitrite, 

• Phosphorus, 

• Sulfate, and

• TKN.

Table 1 summarizes the nine field samples analyzed by TestAmerica and particularly 

highlights how the laboratory split and analyzed the influent samples.
2

Table 1. EPA Episode 6563 Classical Analytes – Sample Identification

EPA

Sample #

Sample Description Sampling

Date

Sample

Matrix

Portion of 

Sample

Analytes 

71891 FGD Influent, Day 1 9/13/10

Water Entire 

Fraction

BOD5, COD, TDS, and 

TSS

Water Filtrate

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Sulfate, Phosphorus, and 

TKN

Solids Solids

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Sulfate, Phosphorus, and

TKN

71892 FGD Influent, Day 2 9/14/10

Water Entire 

Fraction

BOD5, COD, TDS, and 

TSS

Water Filtrate

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Sulfate, Phosphorus, and 

TKN

Solids Solids

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Sulfate, Phosphorus, and 

TKN

71893 FGD Influent, Day 3 9/15/10

Water Entire 

Fraction

BOD5, COD, TDS, and 

TSS

Water Filtrate

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Sulfate, Phosphorus, and 

TKN

Solids Solids

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Sulfate, Phosphorus, and 

TKN

71894 FGD Influent, Day 4 9/16/10

Water Entire 

Fraction

BOD5, COD, TDS, and 

TSS

Water Filtrate

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Sulfate, Phosphorus, and 

TKN

Solids Solids

Ammonia, Chloride, 

Cyanide, Nitrate/Nitrite, 

Sulfate, Phosphorus, and 

TKN

71895 FGD Effluent, Day 1 9/14/10 Water Entire 

Fraction All analytes
3

Table 1. EPA Episode 6563 Classical Analytes – Sample Identification

EPA

Sample #

Sample Description Sampling

Date

Sample

Matrix

Portion of 

Sample

Analytes 

71896 FGD Effluent, Day 2 9/15/10 Water Entire 

Fraction All analytes

71897 FGD Effluent, Day 3 9/16/10 Water Entire 

Fraction All analytes

71898 FGD Effluent, Day 4 9/17/10 Water Entire 

Fraction All analytes

71899 FGD Effluent -

Duplicate 9/15/10 Water Entire Fraction All analytes

SUMMARY

Unless otherwise noted below, all samples were analyzed within the holding time

specified in 40 CFR 136 Table II. 

TestAmerica could not use a preserved sample volume for phase separation. Therefore, 

they combined two of the unpreserved 250 mL metal sample volumes and phase 

separated this volume. After phase separation, TestAmerica preserved the samples 

accordingly. Because of this process, ammonia, nitrate/nitrite, TKN, phosphorus, and 

cyanide influent samples were not preserved immediately following sample collection as 

required by the method. 

One field duplicate sample was 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, 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 noted 

below.
4

If required by the method, a matrix spike (MS) sample was analyzed on sample 71897

(FGD 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

As stated above, filtrate and solid aliquots of samples 71891 - 71894 were not preserved 

immediately after sample collection. Instead, TestAmerica preserved the sample after 

phase separation. Because these samples were not preserved immediately following 

sample collection, they were qualified as estimated values.

The data reviewer identified no other issues. All QC samples met the criteria specified in 

EPA Method 350.1.

BOD5

All glucose-glutamic acid standards and water blanks were analyzed appropriately and 

met the criteria specified in SM 5210B.

The RPD between sample 71897 and its laboratory duplicate was 23%, which is above 

both the method and laboratory criteria of 20%. Sample 71897 was qualified as an 

estimated value.

Three of the four batches had seed correction factors lower than 0.6 mg/L. The seed 

correction factors were 0.5373 mg/L, 0.552 mg/L, 0.6147 mg/L, and 0.576 mg/L for 

batches 31398, 31731, 31878, and 32012, respectively. TestAmerica did not flag these 

samples with an “s” to indicate the seed correction blank (SCB) recovery was low. A low 

seed correction factor indicates that samples may be biased low. Thus, samples 71891, 

71892, 71893, 71895, 71896, 71898, and 71899 were qualified as minimum values and 

for consistency were also flagged with an “s.” Due to the short holding time, the samples 

could not be reanalyzed.

Chloride and Sulfate

The analyzed results for the MS and matrix spike duplicate (MSD) samples associated 

with sample 71897 for both chloride and sulfate were above the calibration range. 

TestAmerica did not rerun the samples with a greater dilution factor because the MS and 

MSD percent recoveries were within the method control criteria. If reported, the MS and 

MSD results will be qualified as estimated values. 
5

COD

The percent recoveries for the MS and MSD analyses for sample 71897 (FGD effluent) 

were below the control limits of 90-110% required by EPA Method 410.4. The percent 

recoveries for the MS and MSD analyses were 89% and 82%, respectively. The low 

percent recovery could indicate that results for samples with the same matrix (FGD 

effluent) could be biased low. Sample 71897 was flagged as a minimum value. The LFBs 

associated with all samples met the method criteria.

The RPD between sample 71896 and its field duplicate 71899 was 25.5%. 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.

Cyanide

As stated above, filtrate and solid aliquots of samples 71891 - 71894 were not preserved 

immediately after sample collection. Instead, TestAmerica preserved the sample after 

performing the phase separation. The solid aliquot results of samples 71891 - 71894 were 

already qualified by TestAmerica with a “J” meaning the results were estimated values 

because they were less than the RL, so no further qualification was necessary. Because 

the filtrate aliquots of samples 71891 - 71894 were not preserved immediately after 

sample collection, they were qualified as estimated values.

Both solid and filtrate volumes of samples 71891 - 71894 were analyzed 10, 9, 8, and 7 

days outside of the 14-day holding time. All of these samples were qualified by the lab 

with an “H,” meaning the samples were analyzed beyond the method-specified hold time. 

Because all of these samples were either qualified with a “J” meaning that the results 

were estimated values because they were less than the RL or they were qualified as 

estimated values because they were not preserved immediately after sample collection, no 

further qualification was necessary.

The analyzed results for sample 71896 and solid samples 71891 - 71894 were lower than 

the lowest calibration standard. Since all the samples were already qualified by 

TestAmerica with a “J” indicating that the results were estimated values because they 

were less than the RL, these samples did not need to be further qualified.

The RPD between sample 71896 and its field duplicate 71899 was 135%. The result for 

71896 was below the RL and flagged with a “J”, but the result for 71899 was above the 

RL. The low amount of cyanide present in these samples was likely the cause 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 SM 4500 CN- E.

Cyanide was detected in the laboratory reagent blank associated with sample 71895 at 

0.00415 mg/L, which was greater than the MDL, but less than the RL. Since the blank 

result was less than the RL, no samples were qualified.
6

Nitrate/Nitrite

As stated above, filtrate and solid aliquots of samples 71891 - 71894 were not preserved 

immediately after sample collection. Instead, TestAmerica preserved the sample after 

phase separation. The solid aliquot results of samples 71891 - 71894 were already 

qualified by TestAmerica with a “J” meaning the results were estimated values because 

they were less than the RL, so no further qualification was necessary. Because the filtrate 

aliquots of samples 71891 - 71894 were not preserved immediately after sample 

collection, they were qualified as estimated values.

The percent recoveries for the MS analysis for sample 71895 and the MS and MSD 

analyses for sample 71897 (FGD effluent) were below the control limits of 90-110% 

required by EPA Method 353.2 but within the laboratory control limits of 72-113%. The 

percent recoveries for the MS and MSD samples were 89% and 92% respectively for 

sample 71895 and were both 84% for sample 71897. The MS and MSD results for 

sample 71897 were above the calibration curve, but not reanalyzed using a higher 

dilution factor. Because the MS and MSD results for sample 71897 at 12.7 mg/L were 

more than ±10% greater than the highest calibration level (10.0 mg/L), the MS and MSD 

recoveries were considered unreliable. Because it was not possible to tell whether the low 

percent recovery was caused by matrix interferences or the MS and MSD results being 

above the calibration curve, sample 71897 was not qualified. Sample 71895 was qualified 

as a minimum value. The LFBs associated with all samples met the method criteria.

Phosphorus 

As stated above, filtrate and solid aliquots of samples 71891 - 71894 were not preserved 

immediately after sample collection. Instead, TestAmerica preserved the sample after 

phase separation. The filtrate aliquot results of samples 71891 and 71894 were already 

qualified by TestAmerica with a “J” meaning the results were estimated values because 

they were less than the RL, so no further qualification was necessary. Phosphorus was not 

detected in the filtrate aliquots of samples 71892 and 71893, so these samples also did not 

need to be qualified. Because the solid aliquots of samples 71891 - 71894 were not 

preserved immediately after sample collection, they were qualified as estimated values.

Results for the filtrate volumes of samples 71891 and 71894 were below the lowest 

calibration standard. These samples were already qualified with a “J” meaning the results 

were estimated values because they were less than the RL, so no further qualification was 

necessary.
7

TDS

Samples 71891 - 71894 were analyzed 14, 13, 12, and 11 days, respectively, past the 7-

day hold time due to laboratory error. TestAmerica only qualified these samples with an 

“H”, so they were additionally qualified as estimated values.

All 14 samples analyzed for TDS did not achieve a constant weight after three drying 

cycles. The weight increased from the first weighing to the second weighing for samples 

71895, 71896, 71898, and 71899. SM 2540C warns that samples that 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, so this was likely the cause for the inconsistent weight calculations. The samples 

were not qualified, but results may be biased high. 

The RPD between sample 71897 and its laboratory duplicate was less than 10% as

required by SM 2540C. The RPD between sample 71891 and its laboratory duplicate was 

11%. Because the RPD was greater than the method control limits, sample 71891 was

qualified as an estimated value. 

TDS was detected at 8.0 mg/L, which is above the MDL (4.7 mg/L), but below the RL

(10 mg/L), in the LRB associated with sample 71895. Because the blank result was less 

than the RL, no samples needed to be qualified based on the LRB result. 

TKN

As stated above, filtrate and solid aliquots of samples 71891 - 71894 were not preserved 

immediately after sample collection. Instead, TestAmerica preserved the sample after 

phase separation. Because these samples were not preserved immediately after sample 

collection, they were qualified as estimated values.

TKN was detected in the LRB associated with filtrate samples 71891 - 71894 at 0.133

mg/L and also detected in the LRB associated with samples 71895 - 71897 and 71899 at 

0.219 mg/L. The blank results were greater than the MDL (0.077 mg/L), but less than the 

RL (1.0 mg/L). Because the blank results were less than the RL, no samples were 

qualified based on the LRB results.

The LFB and LFBD percent recoveries associated with filtrate samples 71891 - 71894 

were not within the method criteria of 90-110%, but were within the laboratory criteria of 

77-115%. The percent recoveries of the LFB and LFBD were 84% and 86%, 

respectively. Filtrate samples 71891 - 71894 were already qualified as estimated values 

because the samples were not preserved immediately after sample collection, so there 

was no need to further qualify these samples as minimum values.

The percent recoveries for the MS and MSD analyses for sample 71897 (FGD effluent) 

did not meet the control limits (90-110%) specified in EPA Method 351.2 and did not 

meet the laboratory criteria of 54-131%. The MS and MSD percent recoveries were 
8

137% and 175%. TestAmerica flagged the MS/MSD samples with a “4” because the 

sample result was more than 4 times the spike amount indicating the control limits are not 

reliable. Thus, sample 71897 was not additionally qualified because of the high MS/MSD 

percent recoveries. The LFB associated with sample 71897 met the method criteria.

TSS 

The laboratory duplicate RPDs for samples 71891, 71893, and 71895 were less than 10% 

as required by SM 2540D. However, the RPD for sample 71897 and its laboratory 

duplicate was 12%. Because this RPD was above the method criteria, sample 71897 was

qualified as an estimated value.

The RPD between sample 71896 and its field duplicate 71899 was 138%. 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 SM 2540D.

Constant weight was not achieved after three drying cycles for sample 71899. SM 2540D 

warns that samples that 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, so this was likely the cause for the 

inconsistent weight calculations. The sample was not qualified, but results may be biased 

high.
9

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level 

Detected

71891 

(filtrate)

Ammonia Estimate Value Sample not preserved 

immediately following 

collection.

13 mg/L

71892 

(filtrate)

Ammonia Estimate Value Sample not preserved 

immediately following 

collection.

14 mg/L

71893 

(filtrate)

Ammonia Estimate Value Sample not preserved 

immediately following 

collection.

13 mg/L

71894 

(filtrate)

Ammonia Estimate Value Sample not preserved 

immediately following 

collection.

12 mg/L

71891 

(solids)

Ammonia Estimate Value Sample not preserved 

immediately following 

collection.

34 mg/Kg

71892 

(solids)

Ammonia Estimate Value Sample not preserved 

immediately following 

collection.

29 mg/Kg

71893 

(solids)

Ammonia Estimate Value Sample not preserved 

immediately following 

collection.

32 mg/Kg

71894 

(solids)

Ammonia Estimate Value Sample not preserved 

immediately following 

collection.

32 mg/Kg

71891 BOD Minimum Value, 

s

SCB Recovery Low 10 mg/L

71892 BOD Minimum Value,

s

SCB Recovery Low 9.5 mg/L

71893 BOD Minimum Value,

s

SCB Recovery Low 13 mg/L

71895 BOD Minimum Value,

s

SCB Recovery Low 8.5 mg/L

71896 BOD Minimum Value,

s

SCB Recovery Low 7.1 mg/L

71897 BOD Estimated Value Lab duplicate RPD > 

method-specified 

criteria

6.8 mg/L

71898 BOD Minimum Value,

s

SCB Recovery Low 3.5 mg/L

71899 BOD Minimum Value,

s

SCB Recovery Low 6.9 mg/L
10

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level 

Detected

71897 COD Minimum Value MS % recovery < 

method-specified 

criteria

380 mg/L

71891 

(filtrate)

Cyanide H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 10 

days past hold time

0.36 mg/L

71892 

(filtrate)

Cyanide H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 9 

days past hold time

0.20 mg/L

71893 

(filtrate)

Cyanide H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 8 

days past hold time

0.29 mg/L

71894 

(filtrate)

Cyanide H, Estimated 

Value

Sample not preserved 

immediately following 

collection. Analyzed 7 

days past hold time

0.31 mg/L

71891 

(filtrate)

Nitrate/Nitrite Estimated Value Sample not preserved 

immediately following 

collection.

12 mg/L

71892 

(filtrate)

Nitrate/Nitrite Estimated Value Sample not preserved 

immediately following 

collection.

14 mg/L

71893 

(filtrate)

Nitrate/Nitrite Estimated Value Sample not preserved 

immediately following 

collection.

14 mg/L

71894 

(filtrate)

Nitrate/Nitrite Estimated Value Sample not preserved 

immediately following 

collection.

12 mg/L

71895 Nitrate/Nitrite Minimum Value MS % recovery < 

method-specified 

criteria

9.7 mg/L

71891 

(solids)

Phosphorus Estimated Value Sample not preserved 

immediately following 

collection.

33 mg/Kg

71892 

(solids)

Phosphorus Estimated Value Sample not preserved 

immediately following 

collection.

380 mg/Kg
11

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level 

Detected

71893 

(solids)

Phosphorus Estimated Value Sample not preserved 

immediately following 

collection.

34 mg/Kg

71894 

(solids)

Phosphorus Estimated Value Sample not preserved 

immediately following 

collection.

6.5 mg/Kg

71891 TDS H, Estimated 

Value

Analyzed 14 days past 

hold time, Lab duplicate 

RPD > methodspecified criteria

35,000 

mg/L

71892 TDS H, Estimated 

Value

Analyzed 13 days past 

hold time

35,000 

mg/L

71893 TDS H, Estimated 

Value

Analyzed 12 days past 

hold time

37,000 

mg/L

71894 TDS H, Estimated 

Value

Analyzed 11 days past 

hold time

35,000 

mg/L

71897 TSS Estimated Value Lab duplicate RPD > 

method-specified 

criteria

7.2 mg/L

71891 

(filtrate)

TKN Estimated Value Sample not preserved 

immediately following 

collection. LFB % 

recovery < methodspecified criteria

29 mg/L

71892 

(filtrate)

TKN Estimated Value Sample not preserved 

immediately following 

collection. LFB % 

recovery < methodspecified criteria

32 mg/L

71893 

(filtrate)

TKN Estimated Value Sample not preserved 

immediately following 

collection. LFB % 

recovery < methodspecified criteria

31 mg/L

71894 

(filtrate)

TKN Estimated Value Sample not preserved 

immediately following 

collection. LFB % 

recovery < methodspecified criteria

26 mg/L

71891 

(solids)

TKN Estimated Value Sample not preserved 

immediately following 

collection.

900 mg/Kg
12

Table 2. Data Review Summary Table

Sample Analyte Qualifier/Action Reason Level 

Detected

71892

(solids)

TKN Estimated Value Sample not preserved 

immediately following 

collection.

840 mg/Kg

71893

(solids)

TKN Estimated Value Sample not preserved 

immediately following 

collection.

710 mg/Kg

71894

(solids)

TKN Estimated Value Sample not preserved 

immediately following 

collection.

880 mg/Kg